Catalyst Process For Spherical Particles

Patent metadata

Field	Value
Publication number	US-2016347882-A1
Application number	US-201514933760-A
Country	US
Kind code	A1
Filing date	Nov 5, 2015
Priority date	Nov 7, 2014
Publication date	Dec 1, 2016
Grant date	—

Abstract

The present invention describes a process for preparing spherical particles of a catalyst composition, the process comprising contacting an organomagnesium precursor with a transition metal compound in presence of an internal donor to obtain a reaction mixture. Thereafter heating the reaction mixture from a first pre-determined temperature to a second pre-determined temperature and then heating the reaction mixture from second pre-determined temperature to a third pre-determined temperature to obtain spherical particles of the catalyst composition. The present invention also relates to a process for preparing of a spherical catalyst system from said spherical catalyst composition and preparing a spherical polyolefins having free flowing characteristics with bulk densities (BD) of at least about 0.4 g/cc from the spherical catalyst system.

First claim

We claim:

1 . A process for preparing spherical particles of a catalyst composition, the process comprising:
contacting an organomagnesium precursor with a transition metal compound in presence of an internal donor to obtain a reaction mixture; heating the reaction mixture from a first pre-determined temperature to a second pre-determined temperature and thereafter heating the reaction mixture from second pre-determined temperature to a third pre-determined temperature to obtain spherical particles of the catalyst composition, wherein heating the reaction mixture from the first pre-determined temperature to the second pre-determined temperature is instigated for a fixed period of time in the range of 5 to 200 minutes at a rate of 0.01 to 10.0° C./minute.

2 . The process of claim 1 , wherein heating is instigated for a fixed period of time at a rate of 0.1 to 5.0° C./minute.

3 . The process of claim 1 , wherein the first pre-determined temperature is the temperature of the reaction mixture and is in the range of about −50° C. to about 50° C., or about −30° C. to about 30° C.

4 . The process of claim 1 , wherein the second pre-determined temperature is in the range of 20 to 40° C.

5 . The process of claim 1 , wherein the third pre-determined temperature is in the range of 100 to 120° C.

6 . The process of claim 1 , wherein molar ratio of the organomagnesium precursor:transition metal compound:internal donor is used in the range of 1:1-200:0.01-0.05.

7 . The process of claim 1 , wherein the heating of the reaction mixture from the first pre-determined temperature to the second pre-determined temperature is done at an agitation/stirring speed of about 100 to about 1000 rpm.

8 . The process of claim 1 , wherein the agitation/stirring speed is in the range of about 200 rpm to about 800 rpm.

9 . The process of claim 1 , wherein the size of the spherical catalyst particles is in the range of 10 to 40 μm.

10 . The process of claim 1 , wherein the internal electron donor used is selected from a group comprising of phthalates, benzoates, succinates, malonates, carbonates, diethers, and combinations thereof, wherein:
(a) the phthalate is selected from a group comprising of di-n-butyl phthalate, di-i-butyl phthalate, di-2-ethylhexyl phthalate, di-n-octyl phthalate, di-i-octyl phthalate, di-n-nonyl phthalate; (b) the benzoate is selected from a group comprising of methyl benzoate, ethyl benzoate, propyl benzoate, phenyl benzoate, cyclohexyl benzoate, methyl toluate, ethyl toluate, p-ethoxy ethyl benzoate, p-isopropoxy ethyl benzoate; (c) the succinate is selected from a group comprising of diethyl succinate, di-propyl succinate, diisopropyl succinate, dibutyl succinate, diisobutyl succinate; (d) the malonate is selected from a group comprising of diethyl malonate, diethyl ethylmalonate, diethyl propyl malonate, diethyl isopropylmalonate, diethyl butylmalonate; (e) the carbonate compound is selected from a group comprising of diethyl 1,2-cyclohexanedicarboxylate, di-2-ethylhexyl 1,2-cyclohexanedicarboxylate, di-2-isononyl 1,2-cyclohexanedicarboxylate, methyl anisate, ethyl anisate; and (f) the diether compound is selected from a group comprising of 9,9-bis(methoxymethyl)fluorene, 2-isopropyl-2-isopentyl-1,3-dimethoxypropane, 2,2-diisobutyl-1,3-dimethoxypropane, 2,2-diisopentyl-1,3-dimethoxypropane, 2-isopropyl-2-cyclohexyl-1,3-dimethoxypropane.

11 . The process of claim 1 , wherein, the transition metal compound represented by M(OR) p X 4-p , where M is selected from a group comprising of Ti, V, Zr and Hf; X is a halogen atom; R is a hydrocarbon group and p is an integer having value equal or less than 4, the transition metal compound is selected from a group comprising of transition metal tetrahalide, alkoxy transition metal trihalide/aryloxy transition metal trihalide, dialkoxy transition metal dihalide, trialkoxy transition metal monohalide, tetraalkoxy transition metal, and mixtures thereof, wherein:
(a) the transition metal tetrahalide is selected from a group comprising of titanium tetrachloride, titanium tetrabromide and titanium tetraiodide and the likes for V, Zr and Hf; (b) alkoxy transition metal trihalide/aryloxy transition metal trihalide is selected from a group comprising of methoxytitanium trichloride, ethoxytitanium trichloride, butoxytitanium trichloride and phenoxytitanium trichloride and the likes for V, Zr and Hf; (c) dialkoxy transition metal dihalide is diethoxy transition metal dichloride and the likes for V, Zr and Hf; (d) trialkoxy transition metal monohalide is triethoxy transition metal chloride and the likes for V, Zr and Hf; and (e) tetraalkoxy transition metal is selected from a group comprising of tetrabutoxy titanium and tetraethoxy titanium and the likes for V, Zr and Hf.

12 . The process of claim 11 , wherein the transition metal compound is titanium compound represented by Ti(OR) p X 4-p , where X is a halogen atom; R is a hydrocarbon group and p is an integer having value equal or less than 4.

13 . The process of claim 1 , wherein the organomagnesium precursor is liquid in nature and is prepared by contacting magnesium source with organohalide and alcohol in presence of a solvent in a single step.

14 . The process of claim 1 , wherein the organomagnesium precursor is solid in nature and is prepared by first contacting the magnesium source with organohalide in presence of solvating agent as the first step and then followed by addition of alcohol.

15 . The process of claim 1 , wherein the organomagnesium precursor is spray dried organomagnesium precursor having spherical morphology and is prepared by first contacting the magnesium source with organohalide in presence of solvating agent as the first step and then followed by addition of alcohol and then subjected to spray dried to obtain spherical morphology of the organomagnesium precursor.

16 . The process of claim 14 , wherein the solvating agent is selected from a group comprising of dimethyl ether, diethyl ether, dipropyl ether, diisopropyl ether, ethylmethyl ether, n-butylmethyl ether, n-butylethyl ether, di-n-butyl ether, di-isobutyl ether, isobutylmethyl ether, and isobutylethyl ether, dioxane, tetrahydrofuran, 2-methyl tetrahydrofuran, tetrahydropyran and combination thereof.

17 . The process of claim 13 , wherein the magnesium source is selected from a group comprising of magnesium metal, dialkyl magnesium, alkyl/aryl magnesium halides and mixtures thereof; wherein:
(a) the magnesium metal is in form of powder, ribbon, turnings, wire, granules, block, lumps, chips; (b) the dialkylmagnesium compounds is selected from a group comprising of dimethylmagnesium, diethylmagnesium, diisopropylmagnesium, dibutylmagnesium, dihexylmagnesium, dioctylmagnesium, ethylbutylmagnesium, and butyloctylmagnesium; and (c) alkyl/aryl magnesium halides is selected from a group comprising of methylmagnesium chloride, ethylmagnesium chloride, isopropylmagnesium chloride, isobutylmagnesium chloride, tert-butylmagnesium chloride, benzylmagnesium chloride, methylmagnesium bromide, ethylmagnesium bromide, isopropylmagnesium bromide, isobutylmagnesium bromide, tert-butylmagnesium bromide, hexylmagnesium bromide, benzylmagnesium bromide, methylmagnesium iodide, ethylmagnesium iodide, isopropylmagnesium iodide, isobutylmagnesium iodide, tert-butylmagnesium iodide, and benzylmagnesium iodide.

18 . The process of claim 13 , wherein the organohalide is selected from a group comprising of alkyl halides either branched or linear, halogenated alkyl benzene/benzylic halid

Assignees

• Indian Oil Corp Ltd

Inventors

• Singh Gurmeet
• Kaur Sukhdeep
• Bantu Bhasker
• Kumar Naresh
• Shashikant
• Kapur Gurpreet Singh
• Basu Biswajit
• Malhotra Ravinder Kumar

Classifications

• C08F110/06 Primary

  Propene · CPC title

• C08F2410/06

  Catalyst characterized by its size · CPC title