FIELD OF THE TECHNOLOGY

The field of the present technology relates to, among others, catalysts for use in the polymerization of olefins and a method of preparing thereof

BACKGROUND

Currently, the bulk of olefin polymerization is catalyzed by Ziegler-Natta catalysts. Ziegler-Natta catalysts are well known in the art and are based on a mixture of catalysts, specifically, a transition metal catalyst and an organoaluminum co-catalyst. Ziegler-Natta catalysts have provided for efficient, commercially viable polymerization of olefins.

Ziegler-Natta catalysts can be classified as heterogeneous or homogeneous depending on the type of transition metal catalyst and organoaluminum co-catalyst employed. Heterogeneous Ziegler-Natta catalysts can include: a transition metal catalyst comprising a transition metal compound, such as, titanium tetrachloride (TiCI ₄ ); and an organoaluminum co-catalyst, such as, triethylaluminum (Al(C ₂ H ₅ ) ₃ ). Transition metal catalysts used in heterogeneous Ziegler-Natta catalysts typically also include a magnesium compound, most commonly magnesium chloride (MgCI ₂ ), and can be bound to a support such as silica.

The manufacture of transition metal catalysts typically includes a multi-step process requiring the time consuming steps of dissolution of a magnesium compound in an alcohol solvent and subsequent evaporation of the alcohol solvent. The resulting magnesium compound is then halogenated with a transition metal halide in a hydrocarbon diluent to form a crude catalyst. Finally, the crude catalyst is purified using filtration, washing, reflux extraction, and the like. The manufacturing process can require the use of multiple reactors, carcinogenic solvents and/or diluents, and large amounts of energy over extended periods of time in order to dissolve solids and evaporate solvents and/or diluents used at various stages of the process thereby leading to increased manufacturing times and costs. As such, a time efficient and cost effective method of preparing a transition metal catalyst is needed.

SUMMARY

A first aspect of the present disclosure provides a method of preparing a catalyst comprising: providing a dihydrocarbyloxide magnesium compound (e.g., the dihydrocarbyloxide magnesium compound can be magnesium ethoxide or Mg(OEt) ₂ ); contacting the dihydrocarbyloxide magnesium compound with carbon dioxide to form a magnesium hydrocarbyl carbonate compound; and reacting the magnesium hydrocarbyl carbonate compound with a transition metal halide to form a crude catalyst.

A second aspect of the present disclosure provides a Ziegler Natta catalyst comprising: a catalyst prepared according to a method of the disclosure; and an organoaluminum cocatalyst.

A third aspect of the present disclosure provides a method of preparing a solid catalyst component for a Ziegler-Natta catalyst comprising: reacting a magnesium compound (e.g., a dihydrocarbyloxide magnesium compound, such as, magnesium ethoxide) with carbon dioxide in the presence of a solvent and a diluent to form a magnesium carbonate solution (e.g., a magnesium hydrocarbyl carbonate solution); adding a porous particulate support to the magnesium carbonate solution in the presence of the excess diluent to form a slurry and impregnating the porous particulate support with the magnesium carbonate solution to form an impregnated support slurry; reacting said the impregnated support slurry with a transition metal halide in the presence of the excess diluent in the presence of an electron donor to form a final reaction mixture; decanting or filtering the final reaction mixture to obtain a solid crude catalyst component; and purifying the solid crude catalyst component by a discontinuous batch-wise extraction and decantation step with an extraction solution to form a solid purified catalyst component.

A fourth aspect of the present disclosure provides a transition metal catalyst for use in a Ziegler-Natta catalyst comprising: a magnesium halide; a transition metal halide; and, an electron donor; wherein the magnesium halide is produced by a reaction of the transition metal and a carbonated micronized Mg(OR) ₂ compound; wherein R is selected from the group consisting of an aryl group, alkyl group, alkene group and cycloalkyl group; and said the transition metal catalyst is prepared and purified in a one-pot process.

A fifth aspect of the present disclosure provides a polymer prepared using a transition metal catalyst of the present disclosure.

Another aspect of the present disclosure provides a method of preparing a catalyst comprising: micronizing a magnesium compound to obtain a micronized magnesium compound; contacting the micronized magnesium compound with carbon dioxide to form a carbonated micronized magnesium compound; and reacting the carbonated micronized magnesium compound with a transition metal halide to form a crude catalyst.

Yet another aspect of the present disclosure provides a method of preparing a solid catalyst component for a Ziegler-Natta catalyst comprising: reacting a dihydrocarbyloxide magnesium compound with carbon dioxide in the presence of a solvent and a diluent to form a magnesium hydrocarbyl carbonate solution; adding a porous particulate support to the magnesium hydrocarbyl carbonate solution in the presence of the excess diluent to form a slurry and impregnating the porous particulate support with the magnesium hydrocarbyl carbonate solution to form an impregnated support slurry; reacting said the impregnated support slurry with a transition metal halide in the presence of the excess diluent in the presence of an electron donor to form a final reaction mixture; decanting or filtering the final reaction mixture to obtain a solid crude catalyst component; and purifying the solid crude catalyst component by a discontinuous batch-wise extraction and decantation step with an extraction solution to form a solid purified catalyst component.

The foregoing summary is illustrative only and is not intended to be in any way limiting. In addition to the illustrative aspects, embodiments, and features will become apparent by reference to the drawings and the following detailed description. BRIEF DESCRIPTION OF THE DRAWING

Embodiments of the disclosure are described herein with reference to the drawing in which:

FIG 1 is a flow chart of an embodiment of a one-pot synthesis and purification method of preparing a transition metal catalyst of the present disclosure; and

DETAILED DESCRIPTION

In the following detailed description, reference is made to the accompanying drawings, which form a part hereof. In the drawings, similar symbols typically identify similar components, unless context dictates otherwise. The illustrative embodiments described in the detailed description, drawings, and claims are not meant to be limiting. Other embodiments can be utilized, and other changes can be made, without departing from the spirit or scope of the subject matter presented herein.

Unless specified otherwise, the terms "comprising" and "comprise" as used herein, and grammatical variants thereof, are intended to represent "open" or "inclusive" language such that they include recited elements but also permit inclusion of additional, un-recited elements.

As used herein, the term "about", in the context of concentrations of components of the formulations, conditions, other measurement values, etc., means +/- 5% of the stated value, or +/- 4% of the stated value, or +/- 3% of the stated value, or +/- 2% of the stated value, or +/- 1% of the stated value, or +/- 0.5% of the stated value, or +/- 0% of the stated value.

Throughout this disclosure, certain embodiments may be disclosed in a range format. It should be understood that the description in range format is merely for convenience and brevity and should not be construed as an inflexible limitation on the scope of the disclosed ranges. Accordingly, the description of a range should be considered to have specifically disclosed all the possible sub-ranges as well as individual numerical values within that range. For example, description of a range such as from 1 to 6 should be considered to have specifically disclosed sub-ranges such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6 etc., as well as individual numbers within that range, for example, 1, 2, 3, 4, 5, and 6. This applies regardless of the breadth of the range.

The present technology provides a transition metal catalyst that can be used in a Ziegler-Natta catalyst. In embodiments, the present technology provides a transition metal catalyst that can be used in a heterogeneous Ziegler-Natta catalyst. The transition metal catalyst can be produced in a manner that provides for a decrease in initial business investment costs, a decrease in process set-up time, a decrease in process or method complexity, a reduction of transition metal catalyst manufacturing time, a reduction in equipment and/or instrument maintenance requirements, a reduction in manufacturing costs, a reduction in operational costs, an increase in manufacturing facility capacity and/or a more environmentally friendly process. Additionally, a magnesium compound for the transition metal catalyst can be selected and used that provides for at least one of a decreased carbonation time and decreased dissolution time. In a number of embodiments, the magnesium compound selected and used is magnesium ethoxide. Further, the physical characteristics, e.g., particle size, of the magnesium compound of the transition metal catalyst can be adjusted or modified thereby enabling at least one of a decreased carbonation time and decreased dissolution time.

In accordance with the present disclosure, a Zeigler-Natta catalyst is formed from a transition metal catalyst and an organoaluminum co-catalyst. Organoaluminum co-catalysts are known in the art and include, for example, trialkylaluminum compounds, dialkylaluminum halides, alkylaluminium dihalides and dialkylaluminum alkoxides.

For simplicity and clarity of illustration/various embodiments of the present disclosure are described hereinafter with reference to FIG. 1 in which like elements are numbered with like reference numerals.

An embodiment of a one-pot synthesis process of preparing a transition metal catalyst of the present disclosure is depicted in FIG. 1. In embodiments, a magnesium compound 10 can be provided and micronized 12 to form a micronized magnesium compound 14. The micronized magnesium compound 14 can be added 16 to a reactor 18 In a number of embodiments, the micronized magnesium compound 14 is magnesium ethoxide.

The continuing discussion below discusses the one-pot synthesis in the case where the magnesium compound 10 has been micronized 12. However, it is important to note that in some embodiments the magnesium compound 10 can be added 16 to the reactor 18 without being micronized. In a number of embodiments, the magnesium compound 10 that is added 16 to the reactor 18 without being micronized is magnesium ethoxide.

A solvent 20 and diluent 22, and carbon dioxide 24 can be added 26 to the reactor 18. The carbon dioxide 24 can contact and react with 28 the micronized magnesium compound 14 in the presence of the solvent 20 and diluent 22 to form a carbonated micronized magnesium compound solution 30. The carbon dioxide 24 can contact and react 28 with the micronized magnesium compound 14 in the presence of the solvent 20 and diluent 22 at about room temperature or higher while stirring to form the carbonated micronized magnesium compound solution 30. In embodiments, carbonation of the micronized magnesium compound 14 can occur at, for example, about 20°C to about 60°C. The mixture of the micronized magnesium compound 14, carbon dioxide 24, solvent 20 and diluent 22 can be stirred during carbonation at a rate of from about 70 rpm to about 1000 rpm. The micronized magnesium compound can be in dissolved form in the carbonated micronized magnesium compound solution 30. In embodiments, the micronized magnesium compound 14 can be carbonated and dissolved in from about 10 minutes to about 60 minutes. In embodiments, the micronized magnesium compound 14 can be carbonated and dissolved in from about 5 minutes to about 60 minutes.

In embodiments, in the case of about a 1 liter manufacturing scale, the reaction of the micronized magnesium compound 14, solvent 20, diluent 22, and carbon dioxide 24 can proceed in an accelerated manner such that the insoluble micronized magnesium compound 14 can be converted to a carbonated magnesium compound (e.g., a magnesium hydrocarbyl carbonate compound) and completely dissolved in the solvent and diluent in 60 minutes or less, 15 minutes or less, 10 minutes or less, or 5 minutes or less.

In embodiments, in the case of about a 1 liter manufacturing scale, the reaction of the magnesium compound 10 (e.g., magnesium ethoxide that is not micronized) solvent 20, diluent 22, and carbon dioxide 24 can proceed in an accelerated manner such that the insoluble magnesium compound can be converted to a carbonated magnesium compound (e.g., a magnesium hydrocarbyl carbonate compound) and completely dissolved in the solvent and diluent in 60 minutes or less, 15 minutes or less, 10 minutes or less, or 5 minutes or less. A support 32 can be added 34 to the carbonated micronized magnesium compound solution 30 in the reactor 18 to form a slurry 36. The slurry 36 includes the carbonated micronized magnesium compound solution 30 and the support 32. The dissolved carbonated magnesium compound of the carbonated micronized magnesium compound solution 30 can impregnate 40 the support particles 32 to form an impregnated support slurry 42. The slurry 36 can be stirred to impregnate 38 the support 32 with the dissolved carbonated magnesium compound to form the impregnated support slurry 40. The impregnated support slurry 40 can be stirred at a rate of from about 70 rpm to about 1000 rpm for about 10 minutes to about 100 minutes. The impregnated support slurry 40 can then be cooled 42 to form a cooled impregnated support slurry 44. The impregnated support slurry 40 can be cooled 42 to a temperature of about -10°C to about 25°C.

A transition metal halide compound 46 can be added to the cooled impregnated support slurry 44 in the reactor 18 to form a supported transition metal halide slurry 48. The transition metal halide compound 46 can be added to the cooled impregnated support slurry 44 while stirring over the course of about 30 minutes to about 120 minutes to form the supported transition metal halide slurry 48. The supported transition metal halide slurry 48 can then be heated to from about 50°C to about 120°C. An electron donor 50 can be added 52 to the supported transition metal halide slurry 48 in the reactor 18 to form a reaction mixture 54. The reaction mixture 54 can be heated and stirred 56 to form a final reaction mixture 58 that includes a crude catalyst 60 and a supernatant 62. The reaction mixture 54 can be heated to from about 50°C to about 120°C and stirred at a rate of from about 70 rpm to about 1000 rpm. The reaction mixture 54 can be stirred for about 10 minutes to about 100 minutes.

A separate evaporation step for evaporating the solvent 20 (e.g., alcohol) from the carbonated micronized magnesium compound solution 30 is not required (e.g., can be omitted or excluded) thereby resulting in the reduction of energy consumption. Further, a separate removal step for removing the carbon dioxide 24 from the solid magnesium compound particles is also not required thereby resulting in the reduction of energy consumption.

The rate of reaction to form the crude catalyst 60 can vary depending on the scale of manufacturing with longer times required for commercial scale manufacturing and shorter times required for micro-scale manufacturing. For example, in embodiments, at about a 1 liter scale, the overall reaction to form the crude catalyst 60 can occur in about 10 hours or less, 9 hours or less, 8 hours or less, 7 hours or less, 6 hours or less, 5.5 hours or less, or 5 hours or less.

The final reaction mixture 58 can be filtered 64 through a filter at the bottom of the reactor 18 above a drain valve. The supernatant 62 can be filtered 64 through the filter to form a filtrate that can be discarded, while the crude catalyst 58 can remain in the reactor 18.

In embodiments, the filtration step can be replaced by direct decantation of the supernatant 62 via a dip-tube followed by washing of the crude catalyst 60 with fresh solvent, and subsequently decanting the supernatant formed from the washing with the fresh solvent. Here also, the crude catalyst 60 remains in the reactor 18.

The crude catalyst 60 can then be purified 66 in the reactor 18. The purification 66 of the crude catalyst 60 can include discontinuous extraction and decantation 68 via a dip-tube using an extraction solution to obtain a solid purified catalyst 70. The extraction solution can include a transition metal halide in a solvent.

In embodiments, the micronized magnesium compound 14, carbon dioxide 24, support 32, transition metal halide component 46 and/or electron donor 50 can be added to the reactor 18 in a different sequence than described in the above embodiment.

In embodiments, the synthesis of the crude catalyst 60 and purification 66 (e.g., discontinuous extraction and decantation 68) of the crude catalyst 60 are performed in the same reactor 18.

In an embodiment, the micronized magnesium compound 14, carbon dioxide

24, support 32, transition metal halide component 46 and/or electron donor 50 can be added simultaneously to the reactor 18 along with the solvent 20 and diluent 22.

The resulting solid purified catalyst 70 exhibits high catalytic activity and provides for the production of polymers of a-alk-l-enes having good morphology and bulk density. In embodiments, the solid purified catalyst 70 can be combined with an organoaiuminum co-catalyst to provide a Ziegler-Natta catalyst for the polymerization of olefins. In embodiments, the solid purified catalyst 70 can be combined with an organoaiuminum co-catalyst to provide a Ziegler-Natta catalyst for the polymerization of olefins, wherein the resulting polymer can have a percent atactic polymer fraction or percent xylene soluble fraction (%XS) of from about 1.2 % to about 1.6 %.

A transition metal catalyst and a process of preparing thereof are disclosed herein. In embodiments, the transition metal catalyst according to the present disclosure can be a catalyst produced by a one-pot synthesis and purification process. In embodiments, the transition metal catalyst according to the present disclosure can be a heterogeneous catalyst produced by a one-pot synthesis and purification process. The process of the present disclosure does not require the use of extremely high temperatures, multiple reactors, and/or solvent evaporation. Additionally, the process of the present disclosure uses minimal amounts of solvents. Thus, in view of the above, the process can be more energy efficient and cost efficient compared to known processes for preparing transition metal catalysts.

In embodiments, the process uses only a small amount of alcohol solvent in combination with a hydrocarbon diluent. In embodiments, the alcohol includes from 1 to 8 carbon atoms. In some embodiments, the alcohol includes a hydrocarbyloxy group similar to or the same as the hydrocarbyloxy groups of the magnesium compound. In some embodiments, the alcohol is replaced with another polar solvent, such as, for example, acetone, dimethyl formamide, or tetrahydrofuran (THF). Additionally, in embodiments, use of micronized starting material can result in accelerated carbonation of the starting material and accelerated dissolution of the magnesium hydrocarbyl carbonate. In embodiments, this accelerated carbonation and accelerated dissolution can allow for completion of the one-pot synthesis and purification process in about 10 hours or less. In embodiments, the accelerated carbonation and acceleration dissolution can allow for completion of the one-pot synthesis and purification process in about 9 hours or less.

Components

The components used in accordance with the present disclosure can include, for example, some or all of the following: a magnesium compound; a solvent or solvent mixture; carbon dioxide; a support; a transition metal halide; and an electron donor.

Magnesium Compound

In embodiments, the magnesium compound can be a dihydrocarbyloxide magnesium compound or magnesium alkoxide compound of the formula MgiOR^OR ² ), in which R ¹ and R ² are identical or different, and wherein Rl and R2 are each an alkyl radical having from 1 to 6 carbon atoms. The magnesium compound can be, for example, Mg(OCH ₃ ) ₂ , Mg(OC ₂ H ₅ ) ₂ , Mg(0-iso-C ₃ H ₇ ) ₂ , Mg(0-n- C ₄ H ₉ ) ₂ , Mg(OCH ₃ )(OC ₂ H ₅ ) and Mg(OC ₂ H ₅ )(0-n-C ₃ H ₇ ). It is also possible to use a magnesium alkoxide of the formula Mg(OR) _n X _m , in which: X = a halogen, (S0 ₄ )i/ ₂ , OH, (C0 ₃ )i/2, (P0 ₄ )i/ ₃ or CI; R = R ¹ or R ² as defined above; and n + m = 2. In some embodiments, the magnesium compound can be, for example, a mixture of MgfOR^OR ² ) and MgX ₂ , in which (OR ¹ ), (OR ² ), and X can be as defined above. In embodiments, the magnesium compound is magnesium ethoxide (Mg(OC ₂ H ₅ ) ₂ ).

In an embodiment, the magnesium compound can be a magnesium halide, for example, MgCl ₂ .

In some embodiments, the magnesium compound can be micronized.

Carbon Dioxide

In accordance with the present disclosure, the magnesium compound or the micronized magnesium compound can be contacted with carbon dioxide (C0 ₂ ). The C0 ₂ can be in the form of gaseous C0 ₂ , dry ice, or supercritical C0 ₂ .

Solvent

In accordance with some embodiments of the present disclosure, the magnesium compound or micronized magnesium compound is solubilized during carbonation in one or more solvents. In embodiments, the one or more solvents can include a monohydric alcohol (R'OH) where R' is a methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, tert-butyl, iso-butyl, n-hexyl, n-heptyl, n-octyl, 2-ethyl hexyl group, or mixture of two or more thereof. In embodiments, the one or more solvents can include ethanol. In embodiments, other polar solvents, such as, acetone, dimethyl formamide or THF can be used alone or in combination with the monohyric alcohol. However, if an alcohol is used, such alcohol preferably contains from 1 to 8 carbon atoms. In embodiments, in order to prevent undesirable transesterification reactions from occurring, an alcohol having a hydrocarbyloxy group similar to or the same as a hydrocarbyloxy group of the magnesium compound or micronized magnesium compound can be added. The use of excess solvent and/or excess diluent can be avoided to prevent catalyst poisoning.

Diluent

In some embodiments, one or more hydrocarbon diluents can be added at one or more points during the preparation of the transition metal catalyst. The hydrocarbon diluent can be, for example, an aromatic hydrocarbon or an aliphatic hydrocarbon, such as, an n-alkane, iso-alkane or cycloalkane-based hydrocarbon. In some embodiments, the hydrocarbon can be, for example, ethylbenzene, benzene, toluene, xylene, pentane, hexane, heptane, octane, hydrogenated diesel oil fractions, cyclopentane, cyclohexane, cycloheptane, cyclooctane or a combination of one or more thereof. In embodiments, the diluent can include ethylbenzene, heptane or a mixture thereof.

In some embodiments, an additional diluent can be added during carbonation of the micronized magnesium compound. The molar ratio of diluent relative to the solvent can be from about 50 : 1 to about 5 : 1. In embodiments, the molar ratio of the diluent to the solvent can be about 30 : 1 to 40 : 1. In embodiments, the molar ratio of the diluent to the solvent can be about 35 : 1. In embodiments where the diluent is ethylbenzene and the solvent is ethanol, the ratio of ethylbenzene to ethanol can be about 35: 1.

In embodiments of the present disclosure, solvents or diluents that include halides such as halocarbons or halohydrocarbons are not used.

Support

In some embodiments, a support can be used in the preparation or manufacture of the transition metal catalyst. In embodiments, the support can be a porous particulate support. The support can be any type of support commonly used in Ziegler-Natta type catalystsand that is compatible with the polymerization of olefins. In embodiments, the support can be a particulate inorganic oxide support. In embodiments, the support or particulate inorganic oxide support can have a specific surface area of from about 10 to about 1000 m ² /g, preferably of from about 50 to about 700 m ² /g, and more preferably from about 100 to about 600 m ² /g- In embodiments, the support or particulate inorganic oxide support can have a mean particle diameter in the range from about 5 to about 200 μητι, preferably from about 10 to about 100 μητι, and more preferably from about 10 to about 60 μιτι. The mean particle diameter as defined herein can refer to the volume average mean of the particle size distribution as determined by Frauenhofer laser light scattering. In embodiments, the average particle size of the support or particulate inorganic oxide support can be about 50 μιη. In embodiments, the particulate inorganic oxide support can include granules. In an embodiment, the granules can be irregularly shaped. In embodiments, the particulate inorganic oxide support can be prepared using a spray-drying step. In an embodiment, a support prepared via spray-drying can have particles having a semi-spherical and/or micro-spheroidal shape. In embodiments, the support can be fumed silica.

In embodiments, the inorganic oxide can include, for example, an oxide of silicon, aluminum, titanium, zirconium, a metal from the main groups I and II of the Periodic Table, or mixture of one or more thereof. In embodiments, the inorganic oxide can be, for example, aluminum oxide, magnesium oxide, layered silicates or a mixture of one or more thereof. In embodiments, the inorganic oxide can be silicon oxide. In embodiments, the inorganic oxide can be silica gel. In embodiments, the inorganic oxide can be a mixed oxide. In embodiments, the mixed oxide can include, for example, aluminum silicates and/or magnesium silicates. In embodiments, the porous particulate support can be a magnesium/aluminum silicate clay.

In embodiments, the particulate inorganic oxide support can have pore volumes of from about 0.1 to about 10 cm ³ /g, and preferably from about 1.0 to about 4.0 cm ³ /g- Addition of a support to the diluted carbonated micronized magnesium compound solution can result in a slurry or suspension.

Transition Metal Halide

In embodiments, a transition metal halide can be added to the carbonated micronized magnesium compound solution. In embodiments, a transition metal halide can be added to the slurry or suspension resulting from the addition of a support to the carbonated micronized magnesium compound solution. In embodiments, the transition metal halide can be a compound including titanium and/or vanadium. In embodiments, the titanium compound can be a halogenide of tri-valent titanium, a halogenide of tetra-valent titanium, or a combination thereof. In embodiments, the titanium compound can be a titanium alkoxy halogenide compound. In embodiments, the transition metal halide can be a mixture or combination of two or more titanium compounds. Examples of suitable titanium compounds include TiCI ₃ , TiCI ₄ , Ti(OCH ₃ )CI ₃ , Ti(OC ₂ H ₅ )CI ₃ , Ti(0-iso-C ₃ C ₇ )Cl ₃ , Ti(0-n- C ₄ H ₉ )CI ₃ , Ti(OCH ₃ ) ₂ CI ₂ , Ti(OC ₂ H ₅ ) ₂ CI ₂ , Ti(0-n-C ₄ H ₉ ) ₂ Cl _2/ Ti(OCH ₃ ) ₃ CI, Ti(OC ₂ H ₅ ) ₃ CI, Ti(0- n-C Hg) ₃ CI. In embodiments the transition metal halide can be titanium tetrachloride (TiCI ₄ ).

The vanadium compound can be a vanadium halogenide, vanadium oxyhalogenide, or a combination thereof. In some embodiments, the transition metal halide can be vanadium tetrachloride (VCI ₄ ). In some embodiments, the transition metal halide can be a combination of two or more transition metal halide.

Electron Donor

In embodiments, an electron donor/internal electron donor can be added after the addition of the transition metal halide. The electron donor can alter or change the non-specific binding sites of the transition metal catalyst to isospecific binding sites when added after the addition of the transition metal halide. In embodiments, the electron donor/internal electron donor can be added before the addition of the transition metal halide and can prevent the formation of non-specific binding sites. When a transition metal catalyst having isospecific binding sites is used, the propagation rate constant (k _p ) of polymer chain growth can be about an order of magnitude higher in comparison to the propagation rate constant (kp) of polymer chain growth when a transition metal catalyst having non-specific binding sites is used. Electron donors used to convert the catalyst from a non-specific catalyst to an isospecific catalyst, or prevent formation of non-specific sites, can be, for example, mono or polyfunctional carboxylic acids, carboxylic anhydrides, carboxylic esters, , ketones, ethers, alcohols, lactones, organophophorous compounds or organosilicon compounds. In embodiments, the electron donor compound can include carboxylic acid derivatives, for example, phthalic acid derivatives having the general formula (C ₆ H ₄ )(COX)(COY), wherein X and Y each represent a halogen or a Ci-Cio alkoxy group, or wherein X and Y can be merged together to represent an oxygen atom thereby forming an anhydride functional group. In some embodiments, the electron donor compounds can be phthalic esters wherein X and Y each are a C C ₈ alkoxy group, for example, a methoxy, ethoxy, n-propyloxy, isoproyloxy, n-butyloxy, sec-butyloxy, or tert-butyloxy group. In embodiments, the phthalic esters can include, for example, diethyl phthalate, di-n-butyl phthalate (DBP), di-iso-butyl phthalate, di-n-pentyl phthalate, di-n-hexyl phthalate, di-n-heptyl phthalate, di-n-octylphthalate or di-2- ethylhexyl phthalate.

Further examples of electron donor compounds include diesters of 3- and 4- membered, optionally substituted cycloalkane 1,2-dicarboxylic acids. Further examples of suitable electron donor compounds include non-substituted and substituted (Ci-Cio alkyl)-l,3-propane diethers, and derivatives of succinates. In embodiments, one electron donor can be used. In embodiments, mixtures or combinations of two or more of any of the foregoing electron donors can be used. Process Steps

Micronization

In embodiments, the magnesium compound can be micronized. Micronization can be achieved, for example, by milling, grinding, supercritical fluid methods and/or the use of other fluid energy mills. Micronization of the magnesium compound forms a micronized magnesium compound. The micronizing step / micronization step can be a continuous process wherein micronized particles can be produced at a rate of about 20 kg/hour, and wherein micronized particles can be obtained within about one minute. The particle size of the micronized magnesium compound can be, for example, from about 0.1 μιτι to about 100 μητι. In embodiments, the particle size of the micronized magnesium compound can be from about 1 μιη to about 30 μιη. In some embodiments, the particle size of the micronized magnesium compound can be less than (<) 10 μητι (d ₉₈ ) and less than (<) 5 μηι (d ₅₀ ). "d ₉₈ "stands for top-cut and means that 98% by weight of the particles are smaller than the dg ₈ size value, while "d ₅₀ " stands for weight average particle size and means that 50% by weight of the particles are smaller than the d ₅₀ size value.

In embodiments, micronization of the magnesium compound, for example, a dihydrocarbyloxide magnesium compound, such as, magnesium ethoxide (Mg(OC2H5)2), prior to contact with C0 ₂ can accelerate both the carbonation of the magnesium compound and subsequent dissolution of the magnesium hydrocarbyl carbonate. In embodiments, the micronized magnesium compound can be carbonated and dissolved in from about 5 minutes to about 60 minutes. The rate of dissolution is dependent upon multiple factors including, for example, the particle size of the magnesium hydrocarbyl carbonate, the C0 ₂ concentration, the amount of alcohol, and the temperature condition. Increasing certain mass-transfer limitations can lead to longer carbonation and dissolution times. In embodiments, the micronized magnesium compound can be carbonated and dissolved in about 15 minutes. The accelerated carbonation and accelerated dissolution greatly increases the rate of the overall reaction forming the transition metal catalyst of the present disclosure.

One-Pot Synthesis and Purification

In accordance with the present disclosure, the process of preparing a transition metal catalyst can be a one-pot synthesis and purification process. The phrase "one-pot synthesis and purification" is meant to indicate that the components, simultaneously or sequentially, are placed into a single reactor within which the process steps can take place, including carbonation, dissolution, formation of a slurry with a support, reaction with a transition metal halide, reaction with an electron donor, and purification. In embodiments, a separate device or reactor for removal of C02, excess alcohol solvent, and/or excess diluent and purification of the crude catalyst is neither required nor used due to the unique one-pot synthesis and purification process of the present disclosure. Use of a single reactor can result in a reduction in initial business investment costs, a reduction in maintenance requirements, reduced operation costs, reduced batch reaction time, an increase in manufacturing plant capacity, a simpler process, and/or a safer process.

Addition of Solvent and Diluent

In embodiments, the micronized magnesium compound can be added to a solvent and an optional diluent to form a micronized magnesium compound - solvent mixture. The molar ratio of the magnesium compound to the solvent can be, for example, 1 : 3. A molar ratio where the solvent amount is too low may result in a ratio that does not completely dissolve the magnesium compound even when a diluent is added. Additionally, a molar ratio where the solvent amount is too high can cause catalyst poisoning. In embodiments, the molar ratio of the magnesium compound to the optional diluent can be, for example, 1 : 60 to 1 : 20. In some embodiments, the ratio of the magnesium compound to the diluent can be, for example, 1 : 40. If the amount of diluent is too large, this can result in reactant concentrations that are too low and reactor volumes that are large. If the amount of diluent is too low, this can cause difficulties in component mixing thereby causing heat and mass transfer limitations.

In embodiments, the use or addition of a diluent in the process of the present disclosure is optional.

Carbonation

In embodiments, the micronized magnesium compound - solvent mixture can be contacted with dry gaseous C0 ₂ by feeding the C0 ₂ gas into the micronized magnesium compound - solvent mixture that includes a micronized magnesium compound, a solvent and, optionally, a diluent. In some embodiments, the C0 ₂ can be added in solid, liquid or supercritical form. The molar ratio of C0 ₂ added to the micronized magnesium compound - solvent mixture can be at least 2 : 1, based on magnesium. If the amount of C0 ₂ added is too low, the carbonation can be incomplete leading to partial dissolution.

Contact of the micronized magnesium compound with the C0 ₂ can result in the formation of a carbonated micronized magnesium compound. The resulting carbonated micronized magnesium compound will be dependent on the starting magnesium compound. For example, carbonation of magnesium ethoxide results in magnesium ethyl carbonate.

In embodiments, carbonation of the micronized magnesium compound can occur at about room temperature or higher. In embodiments, carbonation of the micronized magnesium compound can occur at, for example, about 20°C to about 60°C. In embodiments, the carbonation of the micronized magnesium compound occurs at a temperature of about 25 C. The micronized magnesium compound - solvent mixture and C0 ₂ can be stirred during carbonation at a rate of from about 70 rpm to about 1000 rpm. In embodiments, the mixture of the micronized magnesium compound - solvent mixture and C0 ₂ is stirred during carbonation at a rate of about 400 rpm. In embodiments, the micronized magnesium compound can be carbonated and dissolved in from about 10 minutes to about 60 minutes. In embodiments, the micronized magnesium compound can be carbonated and dissolved in about 15 minutes or less. The contacting/reacting of the micronized magnesium compound - solvent mixture with C0 ₂ results in the formation of a carbonated micronized magnesium compound solution.

Addition of a Support

Following carbonation of the micronized magnesium compound in the presence of the solvent and diluent to form a carbonated micronized magnesium compound solution, a support can be added to the carbonated micronized magnesium compound solution. The amount of support added is dependent on the amount of magnesium compound present. The molar ratio of the support to the magnesium compound can be, for example, 0.5 : 1 to about 5 : 1. In some embodiments, the molar ratio of the support to the magnesium compound can be, for example, 2 : 1.

Addition of the support to the carbonated micronized magnesium compound solution can form a slurry or suspension. The slurry can be stirred at a rate of from about 70 rpm to about 1000 rpm. In some embodiments, the slurry can be stirred at about 400 rpm and at an elevated temperature, for example, about 50°C to about 90°C. In some embodiments, the slurry can be heated, for example, to about 80°C. The slurry can be stirred for about 10 minutes to about 100 minutes. In embodiments, the slurry can be stirred for about 60 minutes. In the slurry, the dissolved carbonated magnesium compound of the carbonated micronized magnesium compound solution can impregnate the support particles to form an impregnated support slurry.

The impregnated support slurry can then be cooled to a temperature of about -10°C to about 25°C. In some embodiments, the slurry can be cooled to about 18°C.

The support does not contribute to the above described reaction(s); rather the support provides a stable morphological structure to the resulting transition metal catalyst. Addition of a Transition Metal Halide

A transition metal halide can be added to the cooled impregnated support slurry while stirring over the course of about 30 minutes to about 120 minutes to form a supported transition metal halide slurry. In some embodiments, a transition metal halide is added, for example, over the course of about 60 minutes. The molar ratio of transition metal halide added to the slurry to magnesium compound is from about 10 : 1 to about 3 : 1. In embodiments, the molar ratio of transition metal halide to magnesium compound can be about 6 : 1.

In an embodiment, the transition metal halide can be added to a carbonated micronized magnesium compound solution that does not include a support.

Addition of an Electron Donor

After the reaction of a transition metal halide with a carbonated micronized magnesium compound solution (e.g., without a support) or impregnated support slurry (e.g., with a support), an electron donor can be added to form a reaction mixture. In embodiments where a supported transition metal halide slurry is formed, the supported transition metal halide slurry can be heated before electron donor addition to from about 50°C to about 120°C. In embodiments, the supported transition metal halide slurry can be heated to about 60°C before electron donor addition.

In embodiments, the electron donor can be added before or during the reaction of the transition metal halide with the carbonated magnesium compound solution (e.g., without a support) or impregnated support slurry (i.e. with a support).

Following addition of the electron donor to form the reaction mixture, the reaction mixture can be heated to about 50°C to about 120°C. In embodiments, the reaction mixture is heated to about 100°C. The reaction mixture can be stirred at a rate of from about 70 rpm to about 1000 rpm. In embodiments, the reaction mixture is stirred at a rate of about 400 rpm. The reaction mixture can be stirred for about 10 min to about 100 minutes. In embodiments, the reaction mixture can be stirred for about 60 minutes. The addition of the electron donor to the carbonated micronized magnesium compound solution (i.e. without a support) or supported transition metal halide slurry (i.e. with a support) results in the formation of a crude catalyst.

Purification

Purification of the crude catalyst involves filtering the crude catalyst from the solvent and diluent. Alternatively, the filtration step can be replaced by a first decantation step to remove supernatant solution, followed by washing of the crude catalyst with pure solvent, and subsequently decanting the supernatant solution formed from the washing with the pure solvent. In an embodiment, the crude catalyst can then be continuously extracted or discontinuously extracted and decanted using an extraction solution. In embodiments, the extraction solution can include a transition metal halide in a solvent. The amount of transition metal halide in the solvent can be from about 10% to about 40%. In embodiments, the transition metal halide of the extraction solution can be the same as the transition metal halide used in the previous steps of the process. The solvent of the extraction solution can be the same as the solvent used in the previous steps of the process or a different solvent.

The continuous extraction step or the discontinuous extraction and decantation step can be performed as long as necessary or as many times as necessary to obtain a pure transition metal catalyst. For example, continuous extraction can be performed over about 3 hours to about 6 hours. In embodiments, continuous extraction can be performed over about 4 hours.

In a discontinuous extraction and decantation step, for example, extraction and decanting can be performed from about 1 to about 5 times. In embodiments, decanting can be performed about 2 times. Each extraction can be performed over about 30 minutes to about 60 minutes.

The reaction of the transition metal halide of the extraction solution with the transition metal halide by-products of the previous steps of the synthesis process can proceed, for example, according to the following reactions: TiC /EB

Si0 ₂ » MgCI ₂ » Donor / TiCI ₄ + TiCI (OR) ₃ Si0 ₂ » MgCI ₂ » Donor / TiCI ₄ + TiCI ₂ (OR) ₂ + TiCI ₃ (OR);

+ Tici ₄ /EB

Si0 ₂ · MgCI ₂ · Donor / TiCI ₄ + TiCI (OR) ₃ + TiCI ₂ (OR) ₂ . Si0 ₂ · MgCI ₂ · Donor / TiCI ₄ + TiCI ₃ (OR);

(EB = ethylbenzene)

Higher chlorinated TiCI ₃ (OR) (e.g., the transition metal halide by-product of the previous steps of the synthesis process) and TiCI ₄ (e.g., the transition metal halide of the extraction solution) are soluble in ethylbenzene (heated to a temperature of about 80°C to about 130°C or higher) and other hydrocarbon solvents (heated to a temperature of about 80°C to about 130°C or higher), and removed from solid transition metal catalyst during the purification step.

Although the transition metal halide is represented in the foregoing equation by TiCI ₄ and the support is represented by Si0 ₂ , any transition metal halide and any support in accordance with the present disclosure can be substituted in the equation. Additionally, the solvent ethylbenzene (denoted in the above equation as EB), can be replaced by any other solvent of suitable polarity and inertness.

The resulting solid purified catalyst exhibits high catalytic activity and provides for the production of polymers of a-alk-l-enes having good morphology and bulk density. In embodiments, the solid purified catalyst can be combined with an organoaluminum cocatalyst to provide a Ziegler-Natta catalyst for the polymerization of olefins. In embodiments, the solid purified catalyst can be combined with an organoaluminum co-catalyst to provide a Ziegler-Natta catalyst for the polymerization of olefins, wherein the resulting polymer can have a percent atactic polymer fraction or percent xylene soluble fraction (%XS) of from about 1.2 % to about 1.6 %.

In embodiments where magnesium ethoxide is used as the starting magnesium compound, the magnesium ethoxide plus the carbon dioxide can provide a carbonated magnesium ethoxide compound that dissolves very quickly in an ethanol solvent and ethylbenzene diluent when compared to MgCI ₂ . For example, in embodiments, the magnesium ethoxide can be carbonated and completely dissolved in the ethanol solvent and ethylbenzene diluent in 60 minutes or less, 15 minutes or less, 10 minutes or less, or 5 minutes or less. In embodiments, the resulting magnesium hydrocarbyl carbonate solution (e.g., magnesium ethoxide carbonate solution) impregnates support particles and reacts with TiCI ₄ to form a crude catalyst.

In embodiments where a discontinuous batch-wise extraction and decantation step is used to purify the crude catalyst, the purification step is much faster when compared to other known purification methods. The reduction in purification time achieved by use of the discontinuous batch-wise extraction and decantation step may also apply to the case where MgCI ₂ is used as the starting magnesium compound.

Further, the reduction in the purification time is achieved even while attaining a highly stereo-regular transition metal catalyst, which provides a low % Xylene Soluble fraction in the polypropylene product formed via use of the transition metal catalyst.

The combination of both advantages (e.g., faster dissolution of the magnesium compound plus faster purification of the crude catalyst) leads to a large decrease in transition metal catalyst preparation time and an increase in plant manufacturing capacity at lower initial business investment costs and operational costs.

EXAMPLE

The present technology is further illustrated by the following example, which should not be construed as limiting in any way.

Example

Preparation of a catalyst was achieved as follows:

Commercial magnesium ethoxide, Mg(OEt) ₂ , having an average particle size of 700 μΐΎΐ, was placed in a jet mill (HOSOKAWA ALPINE Opposed Jet Mill 200AFG) to obtain a micronized Mg(OEt) ₂ . The micronized Mg(OEt)2 had a top cut (d98) particle size of less than about 10 μιη and an average particle size of less than about 5 μπι. The micronizing step is a continuous process wherein micronized particles can be produced at a rate of about 20 kg/hour, and wherein micronized particles can be obtained within about one minute.

About 7 grams of micronized Mg(OEt) ₂ was added to a diluent of about 300 milliliters (mL) ethylbenzene and added to a solvent of about 8.9 mL ethanol in a 1 liter, 2-layer glass reactor. The obtained micronized Mg(OEt) ₂ mixture was agitated/stirred by means of a mechanical motor overhead stirrer with magnetic coupling and equipped with a paddle stirrer at 400 rpm at ambient temperature. Gaseous carbon dioxide, C0 ₂ was fed via stainless-steel tubing to the bottom of the glass reactor at a controlled feed rate that kept the reactor pressure around 2 barg, which is well below the maximum operating pressure of about 6 barg. The C0 ₂ feeding time was about 15 minutes or until the carbonation reaction was completed (e.g., about 15 minutes) and a clear magnesium ethyl carbonate solution formed.

The reaction of the micronized Mg(OEt) ₂ , ethanol solvent, ethylbenzene diluent, and C0 ₂ gas proceeded in an accelerated manner such that the insoluble Mg(OEt) ₂ was converted to magnesium ethyl carbonate and completely dissolved in the ethanol solvent and ethylbenzene diluent within 15 minutes. The accelerated carbonation and accelerated dissolution can be attributed to the use of the micronized Mg(OEt) ₂ .

Additionally, the use of micronized Mg(OEt) ₂ as a starting material resulted in the use of less energy consumption compared to known processes using a MgCI ₂ adduct solution as a starting material. In those known processes, dissolving an amount of MgCI ₂ in ethanol to produce a MgCI ₂ -ethanOl adduct required at least one hour at a temperature above 80°C. In the process of the present disclosure, the same amount of micronized Mg(OEt) ₂ was converted to magnesium ethyl carbonate using C0 ₂ and dissolved in ethanol and ethylbenzene within 15 minutes at room temperature. About 7.3 grams of silicon dioxide or Si0 ₂ (ES70X from PQ. Corporation; average particle size (d ₅₀ ) of about 45 μπι) was added to the resulting magnesium ethyl carbonate- solution in the reactor to form a slurry.

The slurry was heated to 80°C and stirred at about 400 rpm for about 1 hour to allow for the impregnation of the silicon dioxide particles with the magnesium ethyl carbonate. The impregnation step was followed by cooling of the impregnated silicon dioxide slurry to about 18°C in the reactor. All heating and cooling procedures were controlled by a programmable oil-thermostat by pumping temperature controlled thermo-fluid through the jacket of the 2-layer glass reactor.

About 42.9 mL of titanium tetrachloride (TiCI ₄ )was added to the cooled impregnated silicon dioxide slurry in the reactor within about 1 hour to form a supported TiCI4 slurry . Then the supported TiCI ₄ slurry was re-heated to about 60°C. Thereafter, about 7.8 mL di-n-butyl phthalate (DBP) was added to the heated supported TiCI4 slurry to form a reaction mixture. The resulting reaction mixture was then heated to about 100°C and stirred for about 1 hour at about 400 rpm in the reactor to form a final reaction mixture including a crude catalyst and supernatant.

At about 100°C, agitation/stirring was suspended. After solid sedimentation, the supernatant solution was siphoned off or decanted via a dip-tube or alternatively filtered through a sintered glass filter frit (20-30 μηι pore size) to obtain the crude catalyst.

The crude catalyst was discontinuously extracted (batch wise) with about 250 ml equimolar 10% TiCI ₄ in ethylbenzene at 120°C for about 1 hour in the reactor. Then the supernatant solution was decanted via the dip-tube after solid sedimentation. This procedure was repeated a second time to obtain a solid purified catalyst of the present disclosure.

In accordance with the present disclosure, the ethylbenzene and ethanol dissolve the ethyl carbonate that is formed via the reaction of C0 ₂ with undissolved solid MgOEt ₂ .

The solid purified catalyst can be combined with an organoaluminum cocatalyst to provide a Ziegler-Natta catalyst for the polymerization of olefins. Comparative Example

In a reactor, Si0 ₂ (7.31 g, 0.12 mol) (ES757 from PQ Corporation; average particle size (d ₅₀ ) of about 25 μητι) was admixed with fine anhydrous MgCI ₂ (5.80 g, 0.06 mol) and ethanol (EtOH, 8.86 ml, 0.15 mol) in ethylbenzene (300 ml, 2.45 mol) at a temperature of about 70°C under agitation to form a slurry. The molar ratio of ethylbenzene to ethanol was 16 : 1.

The slurry was heated to about 80-85°C and stirred for 4 hours to completely dissolve the MgCI ₂ .

Next, the slurry was cooled to 18°C and TiCI (43 ml, 0.39 mol) was added with continuous mixing within about 1 hr.

The resulting mixture including TiCI ₄ was then re-heated to 60°C and di-n- butyl phthalate (DBP, 7.7 ml, 0.029 mol) was added to form a final reaction mixture. The final reaction mixture was stirred at 400 rpm for 1 hour at a temperature of 100°C to form a crude catalyst slurry.

The crude catalyst slurry was then transferred to a separate extractor vessel, filtered through a sintered glass filter frit (20-30 μηη pore size) and washed with ethylbenzene.

The crude catalyst was then continuously extracted under reflux while agitating/stirring in the separate extractor vessel, equipped with a glass filter frit bottom, for 4 hrs at 120°C with a 10% solution of TiCI ₄ in ethylbenzene to obtain a comparative catalyst.

Although the ratio of ethylbenzene to ethanol is the same in the comparative example as in the example of an embodiment of the disclosure above, in the comparative example, upon cooling, the MgCI ₂ impregnated the Si0 ₂ and recrystallized on the Si0 ₂ . In the comparative example, it took a long time for the MgCl ₂ to dissolve in the ethylbenzene and ethanol. Additionally, in the comparative example, the MgCI ₂ may not have completely dissolved in the ethylbenzene and ethanol.The Example catalyst and Comparative Example catalyst are compared in the table below: Table 1

As shown in Table 1, purification causes a decrease in the titanium content of the resulting example and comparative example catalysts: 6.8% by weight to 4.1% by weight n the comparative example catalyst and 6.1% by weight to 3.6% by weight in the example catalyst. The lower titanium content observed in the example and comparative purified catalysts reflects removal of the titanium ester compound byproducts (TiCI (OR) ₃ , TiCI ₂ (OR) ₂ , and TiCl ₃ (OR)) from both the example and comparative example crude As shown in Table 1, purification causes a decrease in the titanium content of the resulting example and comparative example catalysts: 6.8% by weight to 4.1% by weight in the comparative example catalyst and 6.1% by weight to 3.6% by weight in the example catalyst. The lower titanium content observed in the example and comparative purified catalysts reflects removal of the titanium ester compound by-products (TiCI (OR) ₃ , TiCI ₂ (OR) ₂ , and TiCI ₃ (OR)) from both the example and comparative example crude catalysts. However, the titanium content of the crude and purified comparative example catalyst is significantly higher than that of example catalyst, indicating formation of more by-products and less effective removal during continuous reflux extraction for the comparative example catalyst. Polymerization using the Example Catalyst and Comparative Example Catalyst

Both the example and comparative example catalysts were used to polymerize polypropylene under the following conditions:

Temperature = 70°C

Pressure = 28 Bar

Catalyst amount = 150 mg (dry)

Al/Si ratio = 10 : 1 (Al, triethyl aluminum = 15.0 mmol; Si, isobutyl isopropyl dimethoxysilane = 1.5 mmol)

Time = 90 minutes

The polymerization procedure was as follows:

About 300 g of polypropylene seeding powder was added into a 20 liter autoclave under N ₂ flow with an agitator operating at 70 rpm. The polypropylene seeding powder was purged with propylene gas at a pressure of 5 bars three consecutive times.

15 mmol of co-catalyst triethyl aluminum and 1.5 mmol external donor isopropyl isobutyl dimethoxysilane were introduced consecutively under a propylene gas purge.

150 mg of the catalyst (Comparative or Example) was added to the autoclave followed by the addition of 0.4 mol hydrogen gas from a metering pot. Then propylene gas was added to bring the pressure to 7 bars. The agitator speed was raised to 350 rpm.

A steam/hot water reactor-jacket circulation was used to heat the autoclave to 70°C with the addition of propylene gas until the pressure was 28 bars. These conditions were maintained for 90 minutes by controlled propylene feed.

The propylene gas was released and the reactor was cooled to room temperature. The autoclave was purged with N ₂ at 5 bars three times and the product powder collected. The productivity was calculated in the unit of weight polypropylene/weight of catalyst (g PP/g catalyst). The Xylene Soluble fraction, representing atactic polyproplylene, was determined according to ASTM D5492. Average Particle Size (APS) and weight fractions of different powder size ranges were obtained by Sieve Sizer Analyzer.

Results for the example and comparative example catalysts and their respective resulting polymers are delineated in Table 2 below:

Table 2

*based on dry catalyst (solvent free) The performance and productivity of both the example and comparative example catalysts is comparable and within the margins of error.

The % Xylene Soluble fraction (e.g., the atactic polypropylene fraction of the polypropylene product formed using the example catalyst) was much lower when using the Example catalyst indicating a greater stereospecificity when forming the polymer. This can be attributed to the more efficient extraction of by-products from the crude catalyst by the discontinuous batch-wise extraction and decantation step. Even much longer continuous extraction under reflux of the comparative catalyst cannot compensate for the reduced extraction efficiency of the continuous extraction step. The example catalyst exhibited high catalytic activity and allowed for the production of polypropylene having good morphology and bulk density.

Fiscal benefits of the process for preparing the example catalyst can be calculated on a specific basis (e.g., depending on the facility's specific costs) based on the advantages listed in Table 3 below:

Table 3

The much shorter total preparation time of the example purified catalyst results in a significant increase in plant capacity at lower initial business investment costs and lower operational costs. These benefits can be attributed to the: use of a single reactor for the synthesis of the crude catalyst and the purification of the crude catalyst; use of a micronized magnesium compound; accelerated carbonation of the micronized magnesium compound; accelerated dissolution of the carbonated micronized magnesium compound; and reduction in the time required to purify the crude catalyst achieved by use of the discontinuous batch-wise extraction and decantation step. It is important to note that the reduction in the purification time is achieved even while attaining a highly stereo-regular catalyst, which provides a low % Xylene Soluble fraction in the polypropylene product formed via use of the catalyst. While various aspects and embodiments have been disclosed herein, it will be apparent that various other modifications and adaptations of the invention will be apparent to the person skilled in the art after reading the foregoing disclosure without departing from the spirit and scope of the invention and it is intended that all such modifications and adaptations come within the scope of the appended claims. The various aspects and embodiments disclosed herein are for purposes of illustration and are not intended to be limiting, with the true scope and spirit of the invention being indicated by the appended claims.