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Title:
A PROCESS FOR PRODUCING MICROPARTICLES FOR USE AS MICROBEADS AND MICROPARTICLES PRODUCED ACCORDING TO THE PROCESS
Document Type and Number:
WIPO Patent Application WO/2021/074398
Kind Code:
A1
Abstract:
A process for producing microparticles from marine macro-algae for use as microbeads comprises desalting the marine macro-algae and drying the desalted marine macro-algae. The desalted and dried marine macro-algae is then subjected to a chopping process which chops the marine macro-algae into pieces of maximum dimension, approximately 5mm. The chopped pieces of the marine macro-algae are then subjected to a de-oiling process carried out by a solvent extraction process. The de-oiled pieces of the marine macro-algae are then subjected to a second drying process to reduce the solvent content thereof. The dried de-oiled pieces of the marine macro-algae are processed in a ball mill to produce the microparticles of size in the range 1 micron to 1,000 microns, depending on the use to which the microparticles are to be put. For personal care cleansing products, the microparticles are produced to be of size in the range of 100 microns to 600 microns. The microparticles may be bleached.

Inventors:
LEAHY JAMES JOSEPH (IE)
KEATING SUSAN CLAIRE (IE)
Application Number:
PCT/EP2020/079242
Publication Date:
April 22, 2021
Filing Date:
October 16, 2020
Export Citation:
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Assignee:
SEAGREEN BIO LTD (IE)
International Classes:
A61K8/02; A61K8/9706; A61K8/9711; A61K8/9717; A61K8/9722; A61Q11/00; A61Q19/10; C11D9/38
Domestic Patent References:
WO2017205586A12017-11-30
Foreign References:
US4023734A1977-05-17
Other References:
JUSTYNA KOZLOWSKA; WERONIKA PRUS; NATALIA STACHOWIAK: "Microparticles based on natural and synthetic polymers for cosmetic applications", INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES, vol. 129, 15 May 2019 (2019-05-15), pages 952 - 956, XP009525008
GEORGE DECKNER: "Finding Alternatives to Synthetic Exfoliating Beads", PROSPECTOR, 28 February 2014 (2014-02-28), XP002764466, Retrieved from the Internet [retrieved on 20210118]
NAOHIRO KATO: "Production of crude bioplastic-beads with microalgae: Proof-of-concept", BIORESOURCE TECHNOLOGY REPORTS, vol. 6, 1 June 2019 (2019-06-01), pages 81 - 84, XP055765933, ISSN: 2589-014X, DOI: 10.1016/j.biteb.2019.01.022
ANNA LENA KLEIN: "Algae-Based Bioplastics", 1 January 2019 (2019-01-01), XP055765982, Retrieved from the Internet [retrieved on 20210118], DOI: 10.7795/320.201906
BROWNE MACRUMP PNIVEN SJTEUTEN ELTONKIN AGALLOWAY TTHOMPSON RC: "Accumulations of microplastic on shorelines worldwide: sources and sinks", ENVIRONMENTAL SCIENCE AND TECHNOLOGY, vol. 45, 2011, pages 9175 - 9179
WRIGHT SLTHOMPSON RCGALLOWAY TS: "The physical impacts of microplastics on marine organisms", A REVIEW. ENVIRONMENTAL POLLUTION, vol. 178, 2013, pages 483 - 492, XP028543870, DOI: 10.1016/j.envpol.2013.02.031
FYTILI DZABANIOTOU A: "Utilization of sewage sludge in EU application of old and new methods - A review", RENEWABLE AND SUSTAINABLE ENERGY REVIEWS, vol. 12, 2008, pages 116 - 140, XP022289925, DOI: 10.1016/j.rser.2006.05.014
Attorney, Agent or Firm:
GORMAN, Francis, Fergus et al. (IE)
Download PDF:
Claims:
Claims

1. A process for producing microparticles for use as microbeads, the process comprising chopping marine macro-algae into pieces of an intermediate size, and mechanically processing the pieces of the intermediate size to produce the microparticles of size not exceeding 1,000 microns.

2. A process as claimed in Claim 1 in which the pieces of intermediate size, into which the marine macro-algae is chopped, are of maximum dimension not exceeding 20mm.

3. A process as claimed in Claim 1 or 2 in which the pieces of intermediate size, into which the marine macro-algae is chopped, are of maximum dimension lying in the range of 0.8mm to 20mm.

4. A process as claimed in any preceding claim in which the pieces of intermediate size, into which the marine macro-algae is chopped, are of maximum dimension not exceeding 15mm. 5. A process as claimed in any preceding claim in which the pieces of intermediate size, into which the marine macro-algae is chopped, are of maximum dimension not exceeding 10mm.

6. A process as claimed in any preceding claim in which the pieces of intermediate size, into which the marine macro-algae is chopped, are of maximum dimension not exceeding 5mm.

7. A process as claimed in any preceding claim in which the pieces of intermediate size, into which the marine macro-algae is chopped, are of maximum dimension lying in the range of 0.8mm to 5mm.

8. A process as claimed in any preceding claim in which the pieces of intermediate size, into which the marine macro-algae is chopped, are of maximum dimension lying in the range of 0.8mm to 3mm.

9. A process as claimed in any preceding claim in which the pieces of intermediate size, into which the marine macro-algae is chopped, are of maximum dimension lying in the range of 0.9mm to 2.5mm. 10. A process as claimed in any preceding claim in which the marine macro-algae is chopped in a mechanical chopper to produce the pieces of the marine macro-algae of the intermediate size.

11. A process as claimed in any preceding claim in which the marine macro-algae is chopped to produce the pieces thereof of the intermediate size in a chopping drum.

12. A process as claimed in any preceding claim in which the size of the microparticles lies in the range of 1 micron to 1 ,000 microns.

13. A process as claimed in any preceding claim in which the size of the microparticles lies in the range of 2.5 microns to 800 microns.

14. A process as claimed in any preceding claim in which the size of the microparticles lies in the range of 10 microns to 600 microns.

15. A process as claimed in any preceding claim in which the size of the microparticles is selected to suit the function to be fulfilled by the microparticles.

16. A process as claimed in any preceding claim in which the microparticles are configured for use in a personal care product, and the size of the microparticles lies in the range of 50 microns to 600 microns.

17. A process as claimed in any of Claims 1 to 15 in which the microparticles are configured for use in a personal care cleansing product for cleansing the face and other sensitive parts of a human subject, and the size of the microparticles lies in the range of 100 microns to 180 microns.

18. A process as claimed in any of Claims 1 to 15 in which the microparticles are configured for use in a personal care product for cleansing the hands and other less sensitive parts of the human body, and the size of the microparticles lies in the range of 100 microns to 350 microns.

19. A process as claimed in any of Claims 1 to 15 in which the microparticles are configured for use in a body scrub product for scrubbing the human body, and the size of the microparticles lies in the range of 300 microns to 600 microns.

20. A process as claimed in any of Claims 1 to 15 in which the microparticles are configured for use in a dentifrice, and the size of the microparticles lies in the range of 100 microns to 350 microns.

21. A process as claimed in any of Claims 1 to 15 in which the microparticles are configured for use in an exfoliant product, and the size of the microparticles lies in the range of 100 microns to 600 microns.

22. A process as claimed in any of Claims 1 to 15 in which the microparticles are configured for use in a cosmetic product, and the size of the microparticles is less than 100 microns.

23. A process as claimed in any of Claims 1 to 15 in which the microparticles are configured for use as a filler in a cosmetics product, and the size of the microparticles is less than 100 microns.

24. A process as claimed in any of Claims 1 to 15 in which the microparticles are configured for use as a filler in a cosmetics product, and the size of the microparticles is less than 50 microns.

25. A process as claimed in any preceding claim in which the microparticles are of spherical or partly spherical shape.

26. A process as claimed in any preceding claim in which each microparticle comprises a solid microparticle.

27. A process as claimed in any preceding claim in which each microparticle comprises a homogeneous microparticle.

28. A process as claimed in any preceding claim in which the pieces of the marine macro-algae of the intermediate size are mechanically processed in a milling process to produce the microparticles of size not exceeding 1,000 microns.

29. A process as claimed in Claim 28 in which the milling process to which the pieces of the marine macro-algae of the intermediate size are subjected to produce the microparticles of size not exceeding 1,000 microns is carried out in a ball mill.

30. A process as claimed in any preceding claim in which the marine macro-algae is desalted.

31. A process as claimed in Claim 30 in which the marine macro-algae is desalted to reduce the residual salt content in the marine macro-algae to a level not exceeding 7% by weight.

32. A process as claimed in Claim 30 or 31 in which the marine macro-algae is desalted to reduce the residual salt content in the marine macro-algae to a level not exceeding 5% by weight.

33. A process as claimed in any of Claims 30 to 32 in which the marine macro-algae is desalted to reduce the residual salt content in the marine macro-algae to a level not exceeding 3% by weight.

34. A process as claimed in any of Claims 30 to 33 in which the marine macro-algae is desalted to reduce the residual salt content in the marine macro-algae to a level not exceeding 2.5% by weight.

35. A process as claimed in any of Claims 30 to 34 in which the marine macro-algae is desalted to reduce the residual salt content in the marine macro-algae to a level not exceeding 2% by weight.

36. A process as claimed in any of Claims 30 to 35 in which the marine macro-algae is desalted by immersing and soaking the marine macro-algae in fresh water.

37. A process as claimed in any of Claims 30 to 36 in which the marine macro-algae is desalted prior to chopping thereof to form the pieces of the intermediate size.

38. A process as claimed in any of Claims 30 to 37 in which the desalted marine macro-algae is dried in a first drying process to a predefined moisture content of less than 10% by weight.

39. A process as claimed in Claim 38 in which the predefined moisture content to which the desalted marine macro-algae is dried in the first drying process is less than 5% by weight.

40. A process as claimed in Claim 38 or 39 in which the predefined moisture content to which the desalted marine macro-algae is dried in the first drying process is less than 3% by weight.

41. A process as claimed in any of Claims 38 to 40 in which the marine macro-algae is dried during the first drying process in dehumidified warm air.

42. A process as claimed in any of Claims 38 to 41 in which the desalted marine macro-algae is dried in the first drying process prior to chopping of the marine macro-algae into the pieces of the intermediate size. 43. A process as claimed in any preceding claim in which the marine macro-algae is de-oiled.

44. A process as claimed in Claim 43 in which the marine macro-algae is de-oiled to reduce the oil content thereof to below 0.5% by weight.

45. A process as claimed in Claim 43 or 44 in which the marine macro-algae is de-oiled to reduce the oil content thereof to below 0.3% by weight. 46. A process as claimed in any of Claims 43 to 45 in which the marine macro-algae is de-oiled to reduce the oil content thereof to not more than 0.1% by weight.

47. A process as claimed in any of Claims 43 to 46 in which the marine macro-algae is de-oiled by one of a solvent extraction process, a supercritical extraction process and a mechanical pressing process.

48. A process as claimed in any of Claims 43 to 47 in which the marine macro-algae is de-oiled in a solvent extraction process.

49. A process as claimed in any of Claims 43 to 48 in which the oil extracted from the de-oiling of the marine macro-algae is recovered and saved.

50. A process as claimed in any of Claims 43 to 49 in which the marine macro-algae is de-oiled after the marine macro-algae has been desalted. 51. A process as claimed in any of Claims 43 to 50 in which the marine macro-algae is de-oiled after the marine macro-algae has been chopped into the pieces thereof of the intermediate size.

52. A process as claimed in any of Claims 43 to 51 in which the marine macro-algae is de-oiled after the drying thereof in the first drying process.

53. A process as claimed in any of Claims 43 to 52 in which the marine macro-algae is de-oiled prior to the mechanical processing of the marine macro-algae to form the microparticles.

54. A process as claimed in any of Claims 43 to 53 in which the de-oiled marine macro-algae is dried in a second drying process.

55. A process as claimed in Claim 54 in which the de-oiled marine macro-algae is dried in the second drying process until any residual solvent therein resulting from the de-oiling of the marine macro-algae has been reduced to not more than 5% by weight.

56. A process as claimed in Claim 54 or 55 in which the de-oiled marine macro-algae is dried in the second drying process until the residual solvent therein resulting from the de-oiling of the marine macroalgae has been reduced to not more than 1% by weight.

57. A process as claimed in any of Claims 54 to 56 in which the de-oiled marine macro-algae is dried in the second drying process until the residual solvent therein resulting from the de-oiling of the marine macro-algae has been reduced to not more than 0.1% by weight.

58. A process as claimed in any of Claims 54 to 57 in which the de-oiled marine macro-algae is dried in the second drying process until the residual solvent therein resulting from the de-oiling of the marine macro-algae has been reduced to not more than 0.01% by weight.

59. A process as claimed in any of Claims 54 to 58 in which the drying of the de-oiled marine macroalgae in the second drying process is carried out under vacuum.

60. A process as claimed in any of Claims 54 to 59 in which the drying of the de-oiled marine macroalgae in the second drying process is carried out at a pressure not greater than 100 mbar absolute pressure.

61. A process as claimed in any of Claims 54 to 60 in which the drying of the de-oiled marine macroalgae in the second drying process is carried out at a pressure not greater than 40 mbar absolute pressure.

62. A process as claimed in any of Claims 54 to 61 in which the drying of the de-oiled marine macroalgae in the second drying process is carried out at a pressure not greater than 20 mbar absolute pressure.

63. A process as claimed in any of Claims 54 to 62 in which the de-oiled marine macro-algae is dried during the second drying process at a temperature not greater than 45°C.

64. A process as claimed in any of Claims 54 to 63 in which the de-oiled marine macro-algae is dried during the second drying process at a temperature not greater than 40°C.

65. A process as claimed in any of Claims 54 to 64 in which the de-oiled marine macro-algae is dried during the second drying process at a temperature not greater than 35°C.

66. A process as claimed in any of Claims 54 to 65 in which the de-oiled marine macro-algae is dried during the second drying process at a temperature of approximately 35°C.

67. A process as claimed in any of Claims 54 to 66 in which the drying of the de-oiled marine macroalgae in the second drying process is carried out in a convection oven.

68. A process as claimed in any of Claims 54 to 67 in which the drying of the de-oiled marine macroalgae in the second drying process is carried out prior to the mechanical processing of the marine macroalgae to form the microparticles.

69. A process as claimed in any preceding claim in which the marine macro-algae is bleached.

70. A process as claimed in Claim 69 in which the marine macro-algae is bleached after the marine macro-algae has been formed into the microparticles.

71. A process as claimed in Claim 69 or 70 in which the microparticles are bleached.

72. A process as claimed in any of Claims 69 to 71 in which the bleaching of the marine macro-algae is carried out with an oxidising agent.

73. A process as claimed in Claim 72 in which the oxidising agent comprises a mild oxidising agent.

74. A process as claimed in Claim 69 or 70 in which the oxidising agent comprises one or more of the following oxidising agents: hydrogen peroxide (H202); sodium percarbonate (Na2C0 .5H202); sodium perborate ( NaB03-nH20); Sodium Hypochlorite (NaOCI); Calcium Hypochlorite (Ca(OCI)2); Zinc Dust (Zn); Thiourea dioxide (CH4N2O2S); Sodium Dithionite(Na2S204).

75. A process as claimed in any preceding claim in which the marine macro-algae comprises a marine macro-algae selected from one or more of the following marine macro-algae: ascophyllum; fucus serratus; fucus vesiculosus; pelvetia canaliculate; cystoseira tamariscifolia; cystoseira nodicaulis; laminaria digitata; laminaria ochroleuca; porphyra dioica; cladophora rupestris; codium tomentosum; ulva intestinalis; ulva fenestrate; calliblepharis ciliate; ceramium virgatum; Chondrus crispus; furcellaria lumbricalis; palmaria palmata; and vertebrata lanosa.

76. A process as claimed in any preceding claim in which the marine macro-algae comprises ascophyllum.

77. Microparticles produced from marine macro-algae according to the process as claimed in any preceding claim.

78. Microparticles as claimed in Claim 77 in which the microparticles are of size lying in the range of 1 micron to 1,000 microns.

79. Microparticles as claimed in Claim 77 or 78 in which the microparticles are of size lying in the range of 2.5 microns to 800 microns.

80. Microparticles as claimed in any of Claims 77 to 79 in which the microparticles are of size lying in the range of 10 microns to 600 microns.

81. Microparticles as claimed in any of Claims 77 to 80 in which the microparticles are configured for use as microbeads in a personal care product, and the size of the microparticles lies in the range of 50 microns to 600 microns.

82. Microparticles as claimed in any of Claims 77 to 81 in which the microparticles are configured for use as microbeads in a personal care cleansing product for use on the face and on other sensitive parts of the human body, and the size of the microparticles lies in the range of 100 microns to 180 microns.

83. Microparticles as claimed in any of Claims 77 to 81 in which the microparticles are configured for use as microbeads in a personal care cleansing product for use on the hands and on other less sensitive parts of the human body, and the size of the microparticles lies in the range of 100 microns to 350 microns.

84. Microparticles as claimed in any of Claims 77 to 81 in which the microparticles are configured for use as microbeads in a personal care body scrub product, and the size of the microparticles lies in the range of 300 microns to 600 microns.

85. Microparticles as claimed in any of Claims 77 to 81 in which the microparticles are configured for use as microbeads in an exfoliant product, and the size of the microparticles lies in the range of 100 microns to 600 microns.

86. Microparticles as claimed in any of Claims 77 to 81 in which the microparticles are configured for use as microbeads in a dentifrice, and the size of the microparticles lies in the range of 100 microns to 350 microns.

87. Microparticles as claimed in any of Claims 77 to 81 in which the microparticles are configured for use as a microbead filler in a cosmetic product, and the size of the microparticles are less than 100 microns.

88. Microparticles as claimed in Claim 87 in which the size of the microparticles is less than 50 microns.

89. Microparticles as claimed in any of Claims 77 to 80 in which the microparticles are configured for use as microbeads in a household domestic cleansing product, and the microparticles are of size lying in the range of 100 microns to 500 microns.

90. Microparticles as claimed in any of Claims 77 to 80 in which the microparticles are configured for use as microbeads in an industrial cleansing product, and the microparticles are of size lying in the range of 100 microns to 900 microns.

91. A process for producing a personal care product comprising mixing the microparticles produced by the process as claimed in any of Claims 1 to 76 with a composition suitable for the personal care product. 92. A process as claimed in Claim 91 in which the personal care product comprises a cosmetics product, the process comprising mixing the microparticles with a composition suitable for the cosmetic product.

93. A process as claimed in Claim 91 in which the personal care product comprises an exfoliant product, the process comprising mixing the microparticles with a composition suitable for the exfoliant product. 94. A process as claimed in Claim 91 in which the personal care product comprises a cleansing product for use on the face and other sensitive parts of the human body, the process comprising mixing microparticles with a suitable cleansing composition.

95. A process as claimed in Claim 91 in which the personal care product comprises a cleansing product for use on the hands and on other less sensitive parts of the human body, the process comprising mixing the microparticles with a suitable cleansing composition.

96. A process as claimed in Claim 91 in which the personal care product comprises a body scrub product, the process comprising mixing the microparticles with a suitable body scrub composition.

97. A process as claimed in Claim 91 in which the personal care product comprises a dentifrice, the process comprises mixing the microparticles with a suitable dentifrice composition.

98. A process as claimed in Claim 91 in which the personal care product comprises a filler, the process comprises providing the microparticles as the filler, and mixing the microparticles with a suitable composition for producing the personal care product.

99. A process as claimed in any of Claims 91 to 98 in which the oil recovered and saved from the deoiling of the marine macro-algae is mixed with the microparticles and the composition.

100. A personal care product comprising the microparticles produced according to the process as claimed in any of Claims 1 to 76. 101. A personal care product as claimed in Claim 100 in which the personal care product comprises a cleansing product for use on the face and other sensitive parts of the human body.

102. A personal care product as claimed in Claim 100 in which the personal care product comprises a cleansing product for use on the hands and other less sensitive parts of the human body.

103. A personal care product as claimed in Claim 100 in which the personal care product comprises a body scrub. 104. A personal care product as claimed in Claim 100 in which the personal care product comprises an exfoliant product.

105. A personal care product as claimed in Claim 100 in which the personal care product comprises a dentifrice.

106. A personal care product as claimed in Claim 100 in which the personal care product comprises a cosmetic product, and the microparticles form a filler in the cosmetic product.

107. A household domestic cleansing product comprising the microparticles produced according to the process as claimed in any of Claims 1 to 76.

108. An industrial cleansing product comprising the microparticles produced according to the process as claimed in any of Claims 1 to 76.

Description:
“A process for producing microparticles for use as microbeads and microparticles produced according to the process”

The present invention relates to a process for producing microparticles for use as microbeads, and the invention also relates to the microparticles produced according to the process. The invention also relates to a process for producing a personal care product, and to personal care products.

Microbeads of plastics material are extensively used as an ingredient in personal care products and cosmetics products. Such microbeads fall within the scope of the more general term “microplastics”. The term “microplastics” means particles of plastic material in the solid phase of size up to 1 mm, which are water insoluble and are non-degradable. Microplastics are used in the formulation of a variety of products including but not limited to personal care and cosmetics products, such as toothpaste, shower gel, shampoo, eye shadow, deodorant, blush powders, makeup foundation, skin creams, hairspray, nail polish, liquid makeup, mascara, shaving cream, baby products, facial cleansers, bath products, skincare lotions, sunscreen and hair colouring. In some of these products the microplastics may be large enough to be visible to the naked eye (for example, 50 microns to 1,000 microns), while others are relatively fine particles (low micron range of 2.5 microns to 50 microns), or very fine particles (typically of size less than 2.5 microns). In many cosmetics, the microplastic may be of size smaller than 5 microns. Microplastics may be present in personal care products and cosmetics products at different percentages, ranging from a fraction of 1% to 10%, and in some cosmetic products may be higher, while in some domestic and industrial cleansing products may be considerably higher than 10%.

Depending on the polymer type, composition, size and shape, microplastic ingredients have been included in formulations with a number of functions including but not limited to: viscosity regulators; emulsifiers; exfoliants; film formers; opacifying agents; liquid absorbent binders; bulking agents, for example, fillers; and optical blurring agents, for example, to reduce appearance of facial lines. When used for these functions the microplastics are commonly referred to as microbeads. The term microbeads generally refers to solid particles of various shapes, for example, spherical, amorphic between 1 micron and 1 ,000 microns (UNEP, 2015 - Plastic in Cosmetics).

Manufactured microbeads of non-degradable plastics used in personal care products and cosmetics products, as well as in household and industrial cleanser products, ultimately end up in the waste water stream. Typically the filters in wastewater systems do not adequately remove microplastics smaller than 200 microns (EPA 2003), thus allowing many plastic microbeads from cosmetics and personal care products to pass through stormwater, sewage and septic systems and through rivers and streams into marine ecosystems (Browne MA, Crump P, Niven SJ, Teuten EL, Tonkin A, Galloway T, Thompson RC. 2011. Accumulations of microplastic on shorelines worldwide: sources and sinks. Environmental Science and Technology 45:9175-9179). Once microbeads of non-degradable plastics materials enter the marine environment, they travel freely as aggregates, floating or in suspension in the water column. In the aquatic environment such microbeads of plastics material are consumed by aquatic organisms, potentially entering the human food chain (Wright SL, Thompson RC, Galloway TS. 2013. The physical impacts of microplastics on marine organisms: A review. Environmental Pollution 178:483-492). Estimates of half- lives of microplastics run in the hundreds of years, longer than any persistent organic pollutant (United Nations Environment Programme 2015 - Plastic in Cosmetics).

Treated wastewater effluents are also know to contain microplastics (Browne MA, Crump P, Niven SJ, Teuten EL, Tonkin A, Galloway T, Thompson RC. 2011. Accumulations of microplastic on shorelines worldwide: sources and sinks. Environmental Science and Technology 45:9175-9179), including microbeads similar to those contained in some personal care and cosmetics products (Leslie HA, Moester M, de Dreuk M, Vethaak AD. 2012. Exploratory study of the emission of microplastics from wastewater treatment plants. H2014/15: 45-47). Besides effluents, sewage sludge is another important receptacle of microplastics and microbeads from personal care and cosmetics products. In some parts of the world sewage sludge containing microplastics and microbeads are eventually emitted to the environment via landfilling or application to agricultural lands as bio-solids (Fytili D, Zabaniotou A. 2008. Utilization of sewage sludge in EU application of old and new methods - A review. Renewable and Sustainable Energy Reviews 12: 116-140).

Accordingly, there are many channels through which microbeads can enter the food chain for subsequent ingestion by humans. The ingestion of micro-particles of plastics material is increasingly recognised as having a range of adverse health effects on humans.

There is therefore a need for microbeads, which are suitable for use as an ingredient in personal care and cosmetic products, as well as domestic and industrial cleanser products, and other products, which are biodegradable, and which preferably, are marine biodegradable.

The present invention is directed towards providing microparticles for use as microbeads, and to a process for producing the microparticles. The invention is also directed towards a process for producing personal care products, and to personal care products comprising the microparticles.

According to the invention there is provided a process for producing microparticles for use as microbeads, the process comprising chopping marine macro-algae into pieces of an intermediate size, and mechanically processing the pieces of the intermediate size to produce the microparticles of size not exceeding 1,000 microns.

In one embodiment of the invention the pieces of intermediate size, into which the marine macro-algae is chopped, are of maximum dimension not exceeding 20mm.

In another embodiment of the invention the pieces of intermediate size, into which the marine macro-algae is chopped, are of maximum dimension lying in the range of 0.8mm to 20mm, and preferably, are of maximum dimension not exceeding 15mm, and advantageously, are of maximum dimension not exceeding 10mm, and ideally, are of maximum dimension not exceeding 5mm.

Preferably, the pieces of intermediate size, into which the marine macro-algae is chopped, are of maximum dimension lying in the range of 0.8mm to 5mm, and advantageously, lying in the range of 0.8mm to 3mm, and ideally, lying in the range of 0.9mm to 2.5mm.

In one embodiment of the invention the marine macro-algae is chopped in a mechanical chopper to produce the pieces of the intermediate size, and preferably, the marine macro-algae is chopped to produce the pieces of the intermediate size in a chopping drum.

Preferably, the size of the microparticles lies in the range of 1 micron to 1,000 microns, and advantageously, lies in the range of 2.5 microns to 800 microns, and ideally, lies in the range of 10 microns to 600 microns.

In one embodiment of the invention the size of the microparticles is selected to suit the function to be fulfilled by the microparticles.

In another embodiment of the invention the microparticles are configured for use in a personal care product, and the size of the microparticles lies in the range of 50 microns to 600 microns. In another embodiment of the invention the microparticles are configured for use in a personal care cleansing product for cleansing the face and other sensitive parts of a human subject, and the size of the microparticles lies in the range of 100 microns to 180 microns.

In another embodiment of the invention the microparticles are configured for use in a personal care product for cleansing the hands and other less sensitive parts of the human body, and the size of the microparticles lies in the range of 100 microns to 350 microns. In another embodiment of the invention the microparticles are configured for use in a body scrub product for scrubbing the human body, and the size of the microparticles lies in the range of 300 microns to 600 microns.

In another embodiment of the invention the microparticles are configured for use in a dentifrice, and the size of the microparticles lies in the range of 100 microns to 350_microns.

In another embodiment of the invention the microparticles are configured for use in an exfoliant product, and the size of the microparticles lies in the range of 100 microns to 600 microns. In another embodiment of the invention the microparticles are configured for use in a cosmetic product, and the size of the microparticles is less than 100 microns.

In another embodiment of the invention the microparticles are configured for use as a filler in a cosmetics product, and the size of the microparticles is less than 100 microns. Preferably, the microparticles are configured for use as a filler in a cosmetics product, and the size of the microparticles is less than 50 microns.

In one embodiment of the invention the microparticles are of spherical or partly spherical shape. Preferably, each microparticle comprises a solid microparticle.

Advantageously, each microparticle comprises a homogeneous microparticle. In another embodiment of the invention the pieces of the marine macro-algae of the intermediate size are mechanically processed in a milling process to produce the microparticles of size not exceeding 1,000 microns.

Preferably, the milling process to which the pieces of the marine macro-algae of the intermediate size are subjected to produce the microparticles of size not exceeding 1 ,000 microns is carried out in either a ball mill or a hammer mill.

In one embodiment of the invention the marine macro-algae is desalted.

In another embodiment of the invention the marine macro-algae is desalted to reduce the residual salt content in the marine macro-algae to a level not exceeding 7% by weight. Preferably, the marine macroalgae is desalted to reduce the residual salt content in the marine macro-algae to a level not exceeding 5% by weight. Advantageously, the marine macro-algae is desalted to reduce the residual salt content in the marine macro-algae to a level not exceeding 3% by weight. More preferably, the marine macro-algae is desalted to reduce the residual salt content in the marine macro-algae to a level not exceeding 2.5% by weight. Ideally, the marine macro-algae is desalted to reduce the residual salt content in the marine macro-algae to a level not exceeding 2% by weight.

In one embodiment of the invention the marine macro-algae is desalted by immersing and soaking the marine macro-algae in fresh water.

Preferably, the marine macro-algae is desalted prior to chopping thereof to form the pieces of the intermediate size.

In another embodiment of the invention the desalted marine macro-algae is dried in a first drying process to a predefined moisture content of less than 10% by weight. Preferably, the predefined moisture content to which the desalted marine macro-algae is dried in the first drying process is less than 5% by weight. Advantageously, the predefined moisture content to which the desalted marine macro-algae is dried in the first drying process is less than 3% by weight.

In one embodiment of the invention the marine macro-algae is dried during the first drying process in dehumidified warm air. In another embodiment of the invention the desalted marine macro-algae is dried in the first drying process prior to chopping of the marine macro-algae into the pieces of the intermediate size. In one embodiment of the invention the marine macro-algae is de-oiled.

In another embodiment of the invention the marine macro-algae is de-oiled to reduce the oil content thereof to below 0.5% by weight. Preferably, the marine macro-algae is de-oiled to reduce the oil content thereof to below 0.3% by weight. Advantageously, the marine macro-algae is de-oiled to reduce the oil content thereof to not more than 0.1% by weight.

In one embodiment of the invention the marine macro-algae is de-oiled by one of a solvent extraction process, a supercritical extraction process and a mechanical pressing process. Preferably, the marine macro-algae is de-oiled in a solvent extraction process.

In one embodiment of the invention the oil extracted from the de-oiling of the marine macro-algae is recovered and saved.

In another embodiment of the invention the marine macro-algae is de-oiled after the marine macro-algae has been desalted. Preferably, the marine macro-algae is de-oiled after the marine macro-algae has been chopped into the pieces thereof of the intermediate size. Advantageously, the marine macro-algae is de-oiled after the drying thereof in the first drying process.

Advantageously, the marine macro-algae is de-oiled prior to the mechanical processing of the marine macro-algae to form the microparticles.

In another embodiment of the invention the de-oiled marine macro-algae is dried in a second drying process. Preferably, the de-oiled marine macro-algae is dried in the second drying process until any residual solvent therein resulting from the de-oiling of the marine macro-algae has been reduced to not more than 5% by weight. Advantageously, the de-oiled marine macro-algae is dried in the second drying process until the residual solvent therein resulting from the de-oiling of the marine macro-algae has been reduced to not more than 1% by weight. More preferably, the de-oiled marine macro-algae is dried in the second drying process until the residual solvent therein resulting from the de-oiling of the marine macro- algae has been reduced to not more than 0.1 % by weight, and ideally, until the residual solvent therein resulting from the de-oiling of the marine macro-algae has been reduced to not more than 0.01% by weight.

In one embodiment of the invention the drying ofthe de-oiled marine macro-algae in the second drying process is carried out under vacuum.

In another embodiment ofthe invention the drying ofthe de-oiled marine macro-algae in the second drying process is carried out at a pressure not greater than 100 mbar absolute pressure. Preferably, the drying ofthe de-oiled marine macro-algae in the second drying process is carried out at a pressure not greater than 40 mbar absolute pressure. Advantageously, the drying ofthe de-oiled marine macro-algae in the second drying process is carried out at a pressure not greater than 20 mbar absolute pressure.

In another embodiment ofthe invention the de-oiled marine macro-algae is dried during the second drying process at a temperature not greater than 45°C. Preferably, the de-oiled marine macro-algae is dried during the second drying process at a temperature not greater than 40°C. Advantageously, the de-oiled marine macro-algae is dried during the second drying process at a temperature not greater than 35°C. Ideally, the de-oiled marine macro-algae is dried during the second drying process at a temperature of approximately 35°C.

In one embodiment ofthe invention the drying ofthe de-oiled marine macro-algae in the second drying process is carried out in a convection oven.

In one embodiment ofthe invention the drying ofthe de-oiled marine macro-algae in the second drying process is carried out prior to the mechanical processing ofthe marine macro-algae to form the microparticles.

It is important to reduce the residual solvent content ofthe de-oiled marine macro-algae in order to avoid any change in the chemistry ofthe marine macro-algae which would reduce its biodegradability.

In one embodiment ofthe invention the marine macro-algae is bleached.

In another embodiment of the invention the marine macro-algae is bleached afterthe marine macro-algae has been formed into the microparticles.

Preferably, the microparticles are bleached. In one embodiment of the invention the bleaching of the marine macro-algae is carried out with an oxidising agent.

Preferably, the oxidising agent comprises a mild oxidising agent. In another embodiment of the invention the oxidising agent comprises one or more of the following oxidising agents: hydrogen peroxide (H 2 0 2 ); sodium percarbonate (Na 2 C0 .5H 2 0 2 ); sodium perborate (NaB0 3 -nH 2 0); Sodium Hypochlorite (NaOCI); Calcium Hypochlorite (Ca(OCI) 2 ); Zinc Dust (Zn); Thiourea dioxide (CH 4 N 2 0 2 S); Sodium Dithionite(Na 2 S 2 0 4 ). The marine macro-algae may be selected from any suitable marine macro-algae, or any suitable combination of marine macro-algae. For example, the marine macro-algae may be selected from any one or more of brown marine macro-algae, green marine macro-algae and red marine macro-algae. Suitable brown marine macro-algae, for example, are ascophyllum; fucus serratus; fucus vesiculosus; pelvetia canaliculate; cystoseira tamariscifolia; cystoseira nodicaulis; laminaria digitata; laminaria ochroleuca. Suitable green marine macro-algae, for example, are porphyra dioica; cladophora rupestris; codium tomentosum; ulva intestinalis; ulva fenestrate. Suitable red marine macro-algae, for example are calliblepharis ciliate; ceramium virgatum; Chondrus crispus; furcellaria lumbricalis; palmaria palmata; vertebrata lanosa. The above list of brown, green and red marine macro-algae is not to be considered as being exhaustive or limiting, it is given solely as an example of suitable marine macro-algae.

In one embodiment of the invention the marine macro-algae comprises ascophyllum.

The invention also provides microparticles produced from the marine macro-algae according to the process according to the invention.

In one embodiment of the invention the microparticles are of size lying in the range of 1 micron to 1,000 microns. Preferably, the microparticles are of size lying in the range of 2.5 microns to 800 microns. Advantageously, the microparticles are of size lying in the range of 10 microns to 600 microns. Preferably, the microparticles are configured for use in a personal care product, and the size of the microparticles lies in the range of 50 microns to 600 microns. In one embodiment of the invention the microparticles are configured for use as microbeads in a personal care cleansing product for use on the face and on other sensitive parts of the human body, and the size of the microparticles lies in the range of 100 microns to 180 microns.

In another embodiment of the invention the microparticles are configured for use as microbeads in a personal care cleansing product for use on the hands and on other less sensitive parts of the human body, and the size of the microparticles lies in the range of 100 microns to 350 microns.

In another embodiment of the invention the microparticles are configured for use as microbeads in a personal care body scrub product, and the size of the microparticles lies in the range of 300 microns to 600 microns.

In another embodiment of the invention the microparticles are configured for use as microbeads in an exfoliant product, and the size of the microparticles lies in the range of 100 microns to 600 microns. In another embodiment of the invention the microparticles are configured for use as microbeads in a dentifrice, and the size of the microparticles lies in the range of 100 microns to 350 microns.

In another embodiment of the invention the microparticles are configured for use as a microbead filler in a cosmetic product, and the size of the microparticles are less than 100 microns, and preferably, the size of the microparticles is less than 50 microns.

In a further embodiment of the invention the microparticles are configured for use as microbeads in a household domestic cleansing product, and the microparticles are of size lying in the range of 100 microns to 500 microns.

In a still further embodiment of the invention the microparticles are configured for use as microbeads in an industrial cleansing product, and the microparticles are of size lying in the range of 100 microns to 900 microns. Additionally, the invention provides a process for producing a personal care product comprising mixing the microparticles produced by the process according to the invention with a composition suitable for the personal care product.

In one embodiment of the invention the personal care product comprises a cosmetics product, the process comprising mixing the microparticles with a composition suitable for the cosmetic product.

In another embodiment of the invention the personal care product comprises an exfoliant product the product comprising mixing the microparticles with a composition suitable for the exfoliant product.

In another embodiment of the invention the personal care product comprises a cleansing product for use on the face and other sensitive parts of the human body, the process comprising mixing microparticles with a suitable cleansing composition.

In another embodiment of the invention the personal care product comprises a cleansing product for use on the hands and on other less sensitive parts of the human body, the process comprising mixing the microparticles with a suitable cleansing composition. In another embodiment of the invention the personal care product comprises a body scrub product, the process comprising mixing the microparticles with a suitable body scrub composition.

In another embodiment of the invention the personal care product comprises a dentifrice, the process comprises mixing the microparticles with a suitable dentifrice composition.

In another embodiment of the invention the personal care product comprises a filler, the process comprises providing the microparticles as the filler, and mixing the microparticles with a suitable composition for producing the personal care product. In a further embodiment of the invention the oil recovered and saved from the de-oiling of the marine macro-algae is mixed with the microparticles and the composition.

Further the invention provides a personal care product comprising the microparticles produced by the process according to the invention.

In one embodiment of the invention the personal care product comprises a cleansing product for use on the face and other sensitive parts of the human body.

In another embodiment of the invention the personal care product comprises a cleansing product for use on the hands and other less sensitive parts of the human body.

In a further embodiment of the invention the personal care product comprises a body scrub.

In another embodiment of the invention the personal care product comprises an exfoliant product.

In a further embodiment of the invention the personal care product comprises a dentifrice. In another embodiment of the invention the personal care product comprises a cosmetic product, and the microparticles form a filler in the cosmetic product.

The invention also provides a household domestic cleansing product comprising the microparticles produced by the process according to the invention.

Further the invention provides an industrial cleansing product comprising the microparticles produced by the process according to the invention.

The advantages of the microparticles according to the invention are many. A particularly important advantage of the microparticles according to the invention is that the microparticles are biodegradable, and in particular, are marine biodegradable. Accordingly, when returned to the sea or ocean, the microparticles readily biodegrade, and cause no harm to the marine ecosystem. Indeed, it is believed that once the microparticles according to the invention enter the waste water system, the microparticles commence to biodegrade. Accordingly, by using the microparticles according to the invention in personal care products, personal cleansing products and other cleansing products, as microbeads in place of conventional microbeads of plastics material, the microparticles according to the invention on entering the waste water system commence to biodegrade, and biodegrading of the microparticles is completed in the ocean, thereby avoiding the microparticles entering the food chain in particulate form. Even if the microparticles are ingested by marine life, the microparticles, being of marine micro-algae, are digestible, and therefore are unlikely to have any adverse effect on marine life, animal life or human life.

A further important advantage of the invention is also achieved when products, and in particular personal care products comprising the microparticles according to the invention also include the oil extracted from the ascophyllum, in that since the extracted oil is a marine product, it likewise readily biodegrades in a marine environment when returned thereto, and furthermore in many cases depending on the type of marine macro-algae from which the microparticles are produced, and from which the oil is extracted, the extracted oil may have beneficial health effects as well as anti-inflammatory effects.

Further advantages of the invention are achieved by bleaching the marine macro-algae in that the microparticles formed therefrom become invisible in the personal care or other products into which the microparticles are incorporated.

The advantage of bleaching the marine macro-algae after de-oiling thereof is twofold. Firstly, the oil is extracted from the marine macro-algae without any danger of the oil being contaminated by the bleaching agent or agents, and secondly, the oil in many marine macro-algae tends to be of a relatively dark colour, and therefore, by bleaching the marine macro-algae after de-oiling thereof, the amount of the bleaching agent required is significantly reduced.

A particularly important advantage is achieved by deferring the bleaching of the marine macro-algae until the microparticles have been formed, since this reduces in many cases the volume of the marine macroalgae requiring bleaching, since for some applications, to which the microparticles are put, bleaching may not be required. Whether to bleach or not to bleach the marine macro-algae microparticles will to some extent be dependent on the use to which the microparticles will be put.

The invention will be more clearly understood from the following description of an embodiment thereof, which is given by way of example only, with reference to the accompanying drawing, which illustrates a block representation of a process according to the invention for producing microparticles also according to the invention.

Referring to the drawing the process according to the invention for producing the microparticles also according to the invention will now be described. The microparticles according to the invention are produced for use as microbeads in personal care products, such as, body scrubs, cosmetic products, fillers for cosmetic products, exfoliant products, dentifrice products, personal cleansing products and other cleansing products and the like, for the human or animal body, and in particular, for the human body. The microparticles produced according to the invention are also of size suitable for use in a dentifrice, shower gel, shampoo, eye shadow, deodorant, blush powders, makeup foundation, skin creams, hairspray, nail polish, liquid makeup, mascara, shaving cream, baby products, facial cleansers, bath products, skincare lotions, sunscreen, and hair colouring products, as well as other cosmetic and healthcare products, and personal cleansing products. The microparticles produced according to the invention are also of size suitable for use in domestic household cleansing products, and in industrial cleansing products.

The microparticles according to the invention are solid microparticles and are substantially homogeneous throughout, and are produced from marine macro-algae, which in this case comprises ascophyllum. The ascophyllum is harvested from the North Atlantic Ocean. However, it is envisaged that the marine macroalgae may comprise any suitable marine macro-algae or any suitable combination of marine macro-algae. For example, the marine macro-algae may be selected from any one or more of brown, green or red marine macro-algae. For example, suitable brown marine macro-algae may, for example, be any of ascophyllum; fucus serratus; fucus vesiculosus; pelvetia canaliculate; cystoseira tamariscifolia; cystoseira nodicaulis; laminaria digitata; laminaria ochroleuca. Suitable green marine macro-algae, for example, are porphyradioica; cladophora rupestris; codiumtomentosum; ulva intestinalis; ulva fenestrate. Suitable red marine macro-algae, for example, are calliblepharis ciliate; ceramium virgatum; Chondrus crispus; furcellaria lumbricalis; palmaria palmata; vertebrata lanosa. However, it is envisaged that many other suitable marine macro-algae, of the type commonly referred to as seaweed, may be used. It will also of course be appreciated that the marine macro-algae may be harvested from any other suitable ocean or sea instead of the North Atlantic Ocean.

The process according to the invention comprises a number of steps in order to produce the microparticles according to the invention from the marine macro-algae, comprises a number of steps, which will now be described with reference to the drawing.

Block 1 of the drawing represents the first step in the process for producing the microparticles from the marine macro-algae, and in the first step, the marine macro-algae is harvested from the North Atlantic Ocean, and in this embodiment of the invention has been harvested from the Irish coastline. Once the marine macro-algae has been harvested from the ocean, it is subjected to a desalting process represented by block 2 of the drawing. The harvested marine macro-algae is subject to two desalting processes. In both desalting processes the marine macro-algae is subjected to two soaks in fresh water at ambient temperature in respective baths. The marine macro-algae is sequentially immersed in the respective baths of fresh water for respective first and second predefined time periods each of approximately 120 minutes. While immersed in the first bath during the first time period, the marine macro-algae is periodically agitated by pressing it down into the fresh water in the bath, to ensure that it is fully immersed in the fresh water in the bath. At the end of the first predefined time period of 120 minutes, the marine macro-algae is transferred from the first bath into the second bath and is immersed in fresh water in the second bath for a second predefined time period of 120 minutes, during which time it is also periodically agitated by pressing it down into the fresh water. At the end of the second predefined time period of 120 minutes the marine macro-algae is removed from the second bath, and at that stage should have a salt content not exceeding 2% by weight. The baths are recharged with fresh water prior to each soak of the marine macro-algae therein. While the first and second predefined time periods have been described as being of equal duration, it is envisaged that the first and second predefined time periods may be the same or different. For example, it is envisaged that the first predefined time period may be of duration lying in the range of 60 minutes to 180 minutes, while the duration of the second predefined time period may lie in the range of 90 minutes to 150 minutes.

On completion of the desalting of the marine macro-algae in block 2, the desalted marine macro-algae is then subjected to a first drying process as indicated by block 3 of the drawing. During the first drying process, the desalted marine macro-algae is suspended from racks, and a stream of warm dehumidified air at a temperature in the range of 25°C to 40°C is passed over the suspended desalted marine macroalgae. The first drying process continues until the moisture content of the dry desalted marine macro- algae is reduced to less than 5% by weight, and preferably, is reduced to 3% by weight.

The dried desalted marine macro-algae is then subjected to a chopping process as indicated by block 4 of the drawing. The chopping process is carried out in a multi-bladed drum chopper, and the drum chopper is configured to chop the dried marine macro-algae into pieces of an intermediate size of maximum dimension not exceeding 20mm, and preferably, of maximum dimension not exceeding 5mm, and advantageously, of maximum dimension lying in the range of 0.9mm to 2.5mm.

On completion of the chopping process of block 4, the chopped pieces of the marine macro-algae of the intermediate size are de-oiled as indicated by block 5 of the drawing whereby the oil content of the marine macro-algae pieces is reduced to approximately 0.1 % by weight or less. The de-oiling process whereby the marine macro-algae is de-oiled may be carried out by any suitable process, for example, a solvent extraction process, a mechanical pressing process, a supercritical extraction process, or any other suitable process. In this embodiment of the invention the de-oiling of the marine macro-algae is carried out by a solvent extraction process, and the extracted oil is recovered and saved.

On completion of the de-oiling of the chopped pieces of the marine macro-algae of the intermediate size, the marine macro-algae pieces are subjected to a second drying process as indicated by block 6 of the drawing in order to reduce the residual solvent content in the marine macro-algae pieces remaining after the de-oiling process. The second drying process in this embodiment of the invention is carried out in a convection oven under vacuum at a pressure not greater than 20 mbar absolute pressure, at a temperature of approximately 35°C. The second drying process of block 6 is continued until the residual solvent content of the de-oiled marine macro-algae does not exceed 0.1% by weight, and preferably, does not exceed 0.01% by weight.

It is important to reduce the residual solvent content of the dried de-oiled marine macro-algae as low as possible, in order to avoid any possible change in the chemistry of the marine macro-algae which would reduce its biodegradability.

While the second drying process of block 6 may be carried out at higher temperatures, it is preferable that the second drying process temperature should not exceed 45°C, and more preferably, the drying temperature should not exceed 40°C. A maximum drying temperature of 35°C is most preferable in order to avoid any chemical change in the marine macro-algae, which could reduce its biodegradability.

On completion of the second drying process, the dried, de-oiled marine macro-algae pieces are subjected to a mechanical process indicated by block 7 of the drawing, whereby the marine macro-algae pieces are reduced in size to form the microparticles. The mechanical process of block 7 for reducing the marine macro-algae pieces to form the microparticles comprises a milling process, and is carried out in either a ball mill or a hammer mill. The ball or hammer mill typically produces the microparticles to be of a spherical or a partly spherical shape, and since the microparticles are produced from marine macro-algae, the microparticles are essentially solid microparticles and are also homogeneous microparticles. The ball or hammer mill is configured to produce the microparticles of selectable sizes up to 1,000 microns. The size of the microparticles produced by the ball or hammer mill is dependent on the uses to which the microparticles are to be put. The microparticles may be produced to be of a substantially constant size, or may be produced in ranges of sizes, depending on the use to which the microparticles are to be put. However, in general, the microparticles are produced to be of size in the range of 1 micron to 1 ,000 microns.

Typically, if the microparticles are for use in a cleansing product or other personal care product for use on the sensitive parts of the human body, for example, the face and other such sensitive parts of the human body, the microparticles typically are formed to be of size lying in the range of 100 microns to 180 microns. On the other hand, if the microparticles are for use in a cleansing product, for example, soaps, both liquid and solid, or other personal care cleansing products for use on less sensitive parts of the human body, for example, the hands of the human body, typically, the microparticles are formed to be of size lying in the range of 100 microns to 350 microns. On the other hand, where the microparticles are for use in a body scrub, the microparticles are formed to be of size lying in the range of 300 microns to 600 microns. Where the microparticles are for use as a functional filler in a personal care product, or a cosmetics product, the microparticles are formed to be of size lying in the range of 2.5 microns to 50 microns, and in some filler applications up to 100 microns. Where the microparticles are for use in a personal care exfoliant product, the microparticles are formed to be of size lying in the range of 100 microns to 600 microns. Where the microparticles are for use in a dentifrice product, the microparticles are formed to be of size lying in the range of 100 microns to 350 microns.

Depending on the use for which the microparticles are produced, the microparticles may be subjected to a process indicated by block 8 of the drawings, whereby the microparticles are subjected to a bleaching process, in order to whiten the microparticles so that they will visually blend in with other ingredients of the composition in which the microparticles are to be one of the ingredients. It is envisaged that the microparticles produced for use in certain personal care and cosmetic products will be subjected to the bleaching process.

The bleaching of the microparticles is carried out by the process of block 8 using a mild oxidising agent, which may be any one or more of the following oxidising agents: hydrogen peroxide (H 2 0 2 ); sodium percarbonate (Na 2 C0 .5H 2 0 2 ); sodium perborate ( NaB0 3 -nH 2 0); Sodium Hypochlorite (NaOCI); Calcium Hypochlorite (Ca(OCI) 2 ); Zinc Dust (Zn); Thiourea dioxide (CH 4 N 2 0 2 S); Sodium Dithionite(Na 2 S 2 0 4 ). Once the bleaching of the microparticles of the marine macro-algae, which require bleaching has been completed, the microparticles are then ready for use, and those not requiring bleaching are similarly ready for use.

It will of course be appreciated that in some embodiments of the invention the bleaching process may be omitted.

The invention also provides a process for producing a personal care product according to the invention, for example, a cleansing product for use in cleansing of the skin of the human or animal body, which may be a cleansing product for sensitive skin, for example, the face and other such sensitive parts of the body, or a less sensitive part of the body, for example, the hands of a subject. The process for producing a personal care product, may also include personal care products, such as, for example, cosmetic products, body scrubs, exfoliant products, dentifrices, shampoos, foundation creams, moisturising creams and the like. The process according to the invention for producing such personal care products comprises mixing the microparticles produced by the process according to the invention described with reference to the drawing with a suitable cleansing composition or other suitable relevant composition depending on the product being produced. In producing a personal care cleansing product for the face and other sensitive parts of the human body, the microparticles will be selected to be of a suitable size, and typically, will be selected to be in the range of 100 microns to 180 microns.

In producing a personal care product for cleansing the hands and other less sensitive parts of the human body, the microparticles will be selected to be of a suitable size, and typically, will be selected to be in the range of 100 microns to 350 microns.

In producing a body scrub product for scrubbing the human body, the microparticles will be selected to be of a suitable size, and typically, will be selected to be of size in the range of 300 microns to 600 microns.

In producing a dentifrice, the microparticles will be selected to be of a suitable size, and typically, will be of size in the range of 100 microns to 350 microns.

In producing an exfoliant product, the microparticles will be selected to be of a suitable size, and typically, will be of size in the range of 100 microns to 600 microns. In producing a cosmetic product, the microparticles will be selected to be of a suitable size, and typically, will be selected to be of size less than 100 microns, and where the microparticles are to provide a filler for a cosmetic product, the microparticles will be selected to be of size less than 50 microns.

In producing a household domestic cleansing product, the microparticles will be selected to be of a suitable size, and typically, will be selected to be of size lying in the range of 100 microns to 500 microns.

In producing an industrial cleansing product, the microparticles will be selected to be of a suitable size, and typically, will be selected to be of size in the range of 100_microns to 900 microns.

In general, it is envisaged that the microparticles will constitute in the range of 2% by weight to 25% by weight ofthe total weight of the above described personal care products, cosmetic products, dentifrices, body scrub products, household domestic cleansing products and industrial cleansing products, although in the majority of personal care products, in general, it is envisaged that the microparticles will constitute in the range of 2% to 10% by weight ofthe total weight ofthe personal care product.

The process according to the invention for producing a personal care product according to the invention, may also comprise mixing the recovered and saved extracted oil from the marine macro-algae during the de-oiling process with the mixture ofthe microparticles and the cleansing composition and/or other relevant composition to produce personal care products, dentifrices, cosmetic products, personal cleansing products, household domestic cleansing products and industrial cleansing products also according to the invention. It is believed that the personal care and cleansing products comprising the recovered and saved oil may have anti-inflammatory properties for topical applications. It is expected that the proportion ofthe recovered and saved oil in the products, in general, will lie in the range of 0.1% by weight to 0.5% by weight ofthe total weight ofthe product.

While the products according to the invention, which have been described as containing the microparticles according to the invention, have been described as being personal care products and cosmetic products, as well as exfoliant products, it is envisaged that personal care products according to the invention including the microparticles according to the invention will include many different types of personal care products, for example, shower gels, shampoos, eye shadows, deodorants, blush powders, makeup foundations, skin creams, moisturising creams, hair sprays, nail polish, nail polish removers, liquid makeup, mascara, shaving creams, baby products, facial cleansers, bath products, skincare lotions, sunscreens, anti-aging products and hair colouring products to name but a few, all of which will be according to the invention. The microparticles may be used to fulfil many functions including but not limited to: viscosity regulators; emulsifiers; exfoliants; film formers; opacifying agents; liquid absorbent binders; bulking agents, for example, fillers; and optical blurring agents, for example, to reduce the appearance of facial lines. However, as discussed above the size of the microparticles will be selected to be suitable for the type of products in which they are for use, and the functions for which they are to fulfil. Indeed, it will be readily apparent to those skilled in the art that the microparticles according to the invention may be used in any other product or application, where microbeads are required, for example, in domestic and industrial cleansing products and detergents.

While the personal care and the cosmetics products described have been described as comprising the oil extracted from the marine macro-algae, while this in some cases may be desirable, it is not essential. In general, cleansing products for domestic and industrial purposes will not be provided with the oil extracted from the marine macro-algae. However, the percentage of the microparticles would most likely be higher in domestic and industrial cleansing products than in cleansing products for the human body.

While in the specific embodiment described for producing the microparticles, the marine macro-algae has been described as being chopped into pieces of specific intermediate size, it is envisaged that the marine macro-algae may be chopped into intermediate sizes of any suitable size. Needless to say, any other suitable means for chopping the marine macro-algae into pieces of intermediate size may be used besides a drum chopper.

Additionally, it will be appreciated that while the process steps have been described as reducing moisture, oil, salt and solvent contents to specific values, it will be readily apparent to those skilled in the art that the moisture, oil, salt and solvent contents may vary, depending on the embodiment of the invention.

It will also be appreciated that the desalting of the marine macro-algae may be carried out at any suitable time in the process, and may be carried out before or after chopping the marine macro-algae into pieces of the intermediate size, and in some embodiments of the invention it is envisaged that the desalting of the marine macro-algae may be carried out after de-oiling thereof.

Further, it will be appreciated that any other suitable mechanical processing may be used for producing the microparticles besides a ball mill or a hammer mill. Indeed, other suitable milling processes may be used for producing the microparticles besides a ball mill or a hammer mill.

In the event that the de-oiling process is carried out by a de-oiling process not based on a solvent extraction process, for example, a mechanical pressing process or a supercritical fluid extraction process, it is envisaged that the second drying process of block 6 may be omitted.

While in the embodiments of the invention described, the microparticles have been produced from ascophyllum, and the oil extract has also been produced from ascophyllum, it is envisaged that the microparticles may be produced from any other suitable marine macro-algae, and likewise, the oil extract may be extracted from any other marine macro-algae. For example, it is envisaged that the microparticles and the extracted oil may be formed, and extracted, respectively, from any one or more of the following marine macro-algae: ascophyllum; fucus serratus; fucus vesiculosus; pelvetia canaliculate; cystoseira tamariscifolia; cystoseira nodicaulis; laminaria digitata; laminaria ochroleuca; porphyra dioica; cladophora rupestris; codiumtomentosum; ulva intestinalis; ulva fenestrate; calliblepharis ciliate; ceramium virgatum; Chondrus crispus; furcellaria lumbricalis; palmaria palmata; vertebrata lanosa, and any other suitable marine macro-algae.

While the desalting of the marine macro-algae has been described as being carried out in two steps in respective first and second baths of fresh water, the marine macro-algae may be desalted by any other suitable desalting process. Needless to say, the first drying process whereby the desalted marine macroalgae is dried may be carried out by any other suitable drying process, and may be carried out at any other suitable drying temperatures. Similarly, the drying of the de-oiled marine macro-algae which is carried out in the second drying process, may be carried out by any other suitable drying process.

It will be appreciated that in some embodiments of the invention bleaching of the microparticles may not be required, for example, bleaching of the microparticles for use in domestic and industrial cleansing and detergent products may be unnecessary, and it will also be appreciated that the bleaching of the marine macro-algae may be carried out at any other suitable part of the process.