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Title:
A BITUMINOUS MIXTURE COMPRISING POLYURETHANE OBTAINED BY A POLYMERIZATION REACTION OF BHET OBTAINED FROM CHEMICAL DEPOLYMERISATION OF PET WASTE AND A PREPARATION METHOD THEREOF
Document Type and Number:
WIPO Patent Application WO/2019/009836
Kind Code:
A4
Abstract:
A method for preparing a modified bituminous mixture is developed according to the present invention, this method comprising the steps of fluidizing bitumen as the main component of the mixture at 130-140°C; transferring the fluidized bitumen into a mechanical mixer running at 120 rpm stirring speed; producing a polyurethane-bitumen mixture by adding polyurethane, as an additive in hot form, obtained through a polymerization reaction of BHET monomers obtained through a recycling reaction of waste PET products, as a diol monomer with diisocyanate monomer and a chain extender into bitumen in said mixer while stirring continues; stirring further this mixture for a predetermined time at a predetermined stirring speed to obtain a homogeneous polyurethane-bitumen mixture; following the completion of the stirring process, obtaining a homogeneous polyurethane-added modified bituminous mixture.

Inventors:
CANIAZ RAMAZAN OGUZ (TR)
CETINTAS REFIKA (TR)
ARCA SERHAT (TR)
BASKENT EMEL (TR)
KOCAMAN ELIF (TR)
KOSTERELI ZIYA (TR)
YASAR MUZAFFER (TR)
GURDAL SAVAS (TR)
Application Number:
PCT/TR2017/050594
Publication Date:
June 13, 2019
Filing Date:
November 23, 2017
Export Citation:
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Assignee:
TURKIYE PETROL RAFINERILERI ANONIM SIRKETI TUPRAS (TR)
International Classes:
C08L53/02; C08L75/04; C08L75/06; C08L95/00
Attorney, Agent or Firm:
CAYLI, Hulya (TR)
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Claims:
AMENDED CLAIMS

received by the International Bureau on 16 May 2019 (16.05.2019)

1- A method for preparing a modified bituminous mixture, characterized by comprising the steps of

- Washing waste PET products gathered in collection areas with a predetermined amount of water to free PET products from Impurities;

- Drying the washed waste PET products;

- Turning the dried waste PET products Into scrap PET suitable for use in the recycling reactions;

- Loading the scrap PETs into a reactor in which the recycling reaction is to be carried out;

- Adding Ethylene Glycol Into the reactor to which the scrap PETs were loaded to carry out the recycling reaction;

- Conducting the recycling reaction in the presence of at least one catalyst; - Following the completion of the recycling reaction, obtaining a product comprising monomelic BHET, ethylene glycol and impurities;

- in order to purify the obtained product from said impurities, washing it with a predetermined amount of water;

- Taking the fractions from the washed product, which make up impurities in the product by remaining water-insoluble, into a first container;

- After separating the fraction forming impurities from the product, taking the remaining BHET monomers and ethylene glycol into a second container;

- Crystallizing the BHET monomers by keeping the remaining BHET monomers and ethylene glycol in the second container in a cold environment;

- Generating a phase separation with the crystallized BHET monomers sinking to the bottom in ethylene glycol;

- Filtering the sunk BHET monomers to separate them from ethylene glycol;

Obtaining BHET monomers suitable for use in polyurethane reactions by purifying BHET monomer crystals obtained after filtration from the whole ethylene glycol.

- adding MDI as an isocyanate monomer into a reactor comprising a mechanical mixer;

- adding into the MDI-comprising reactor BHET monomers, as a diol monomer, obtained through recycling reactions from waste PET products; - following the addition of BHET monomer* into the reactor, adding butanediol «8 a chain extender so that the polymerization reaction is initiated;

- following the completion of the polymerization reaction, obtaining polyurethane suitable for use as an additive in modified bituminous mixtures.

- Flurdizing bitumen, as the main component of the mixture, at 130-140'C;

- Transferring the fluidized bitumen into a mechanical mixer;

- Producing polyurethane-bitumen mixture by adding polyurethane as an additive in hot form to bitumen, whose temperature is between 130-140'C, in said mixer while stirring process continues, wherein the polyurethane is synthesized as a result of a polymerization reaction of BHET monomers, as a diol monomerobtalned through a recycling reaction of waste PET products with diteocyanate monomer and a chain extender as a dloi monomer is synthesized as a result of a polymerization reaction of BHET monomers, , obtained through a recycling reaction of waste PET products with diisocyanate monomer and a chain extender*

- Stirring further this mixture for a predetermined time at a predetermined stirring speed to obtain a homogeneous polyurethane-bitumen mixture;

- Following the completion of the stirring process, obtaining a homogeneous polyurethane-added modified bituminous mixture.

2- The method for preparing a modified bftuminoue mixture according to daim 1, characterized in that the bitumen is fluidized at 135'C.

3- The method for preparing a modified bituminous mixture according to claim 1, characterized in that the stirring speed is 120 rpm.

4- The method for preparing a modified bituminous mixture according to claim 1, characterized in that said time period is 60 minutes.

5- The method for preparing a modified bituminous mixture according to claim 1, characterized in that the method further comprises the steps of adding a predetermined amount of SBS to the obtained polyurethane-added modified bituminous mixture;

- obtaining a polyurethane- and SBS-added modified bituminous mixture; - stirring further this mixture for a predetermined time at a predetermined stirring speed to obtain a homogeneous polyurethane- and SBS-added modified bituminous mixture;

following the completion of the stirring process, obtaining a homogeneous polyurethane- and SBS-added modified bituminous mixture.

6- The method for preparing a modified bituminous mixture according to claim 5, characterized In that the SBS is divided Into 10 equal portions and is added in this way to polyurethene-added modified bituminous mixture.

7- The method for preparing a modified bituminous mixture according to claim 5, characterized In that the SBS is added to the obtained polyurethane-added modified bituminous mixture at 180'C. 8- The method for preparing a modified bituminous mixture according to claim 5, characterized in that the SBS is added to polyurethane-added modified bituminous mixture by means of a mechanical mixer running at 400 rpm speed.

9- The method for preparing a modified bituminous mixture according to claim 5, characterized in that 10% of the total amount of SBS to be added is added each time at 3-minute intervals to the polyurethane-added modified bituminous mixture.

10- The method for preparing a modified bituminous mixture according to claim 5, characterized In that the polyurethane- and SBS-added modified bituminous mixture is stirred for 60 minutes.

11- The method for preparing a modified bituminous mixture according to claim 5, characterized in that the obtained homogeneous polyurethane- and SBS-added modified bituminous mixture comprises 3% or less than 3% by weight of polyurethane and 3% or less than 3% by weight of SBS.

12- The method for preparing a modified bituminous mixture according to claim 5, characterized in that the obtained homogeneous polyurethane- and SBS-added modified bituminous mixture comprises 3% by weight of polyurethane. 13- The method for preparing a modified bituminous mixture according to claim 6, characterized in that the obtained homogeneous polyurethane- and SBS-added modified bituminous mixture comprises 3% by weight of SBS.

14- The method for preparing a modified bituminous mixture according to claim 1, characterized in that MDI Is added in a melt form at 80#C.

16- The method for preparing a modified bituminous mixture according to claim 1, characterized in that said reactor is a batch reactor.

16- The method for preparing a modified bituminous mixture according to claim 1, characterized in that BHET monomers are added dropwise In a mett form at 110°C. 17· The method for preparing a modified bituminous mixture according to claim 1, characterized in that said mixer la coupled to the reactor from the top.

18- The method for preparing a modified bituminous mixture according to claim 1, characterized in that the polymerization reaction is carried out under a nitrogen blanket

18- The method for preparing a modified bituminous mixture according to claim 1, characterized in that BHET monomers, butanediol and MDI are added to said reactor In a maaa proportion of 1:1:8 (BHET:butanediol:MDI).

20- The method for preparing a modified bituminous mixture according to claim 1, characterized in that the remaining BHET monomers and ethylene glycol present in the second container are held in a cooler at 4 to 6'C for 24 hours. 21 -The method for preparing a modified bituminous mixture according to claim 1, characterized in that said scrap PETs have a size of 1cmx1cm.

22- The method for preparing a modified bituminous mixture according to claim 1, characterized in that said reactor is made of glass. 23- The method for preparing a modified bituminous mixture according to clalml or claim 24, characterized in that laid reactor is three-necked.

24- The method for preparing a modified bituminous mixture according to claim 1, characterized in that said catalyst is a zinc acetate catalyst.

26- The method for preparing a modified bituminous mixture according to claim 1, characterized in that said recycling reaction Is carried out at a temperature of 195- 200°C.

26- The method for preparing a modified bituminous mixture according to daim 1 , characterized In that the recycling reaction is earned out for 3 hours.