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Olefin polymerization catalyst and preparation method thereof

A technology for olefin polymerization and catalysts, applied in the field of olefin polymerization catalysts and their preparation, can solve the problems of unfavorable production of polymers, poor hydrogenation sensitivity of catalysts, etc., and achieve the effect of suitable molecular weight distribution and good comprehensive performance

Inactive Publication Date: 2012-05-23
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The inventors have found through research that although this type of electron donor catalyst has high catalytic activity, the hydrogen tuning sensitivity of the catalyst is poor, which is very unfavorable for the production of high melt index polymers, which limits the 1,4 -Application of diester internal electron donor compounds

Method used

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  • Olefin polymerization catalyst and preparation method thereof
  • Olefin polymerization catalyst and preparation method thereof
  • Olefin polymerization catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] 1. Synthesis of bicyclo[2,2,1]-2,3-α,β-diethyl succinate electron donor

[0043] Add 1.17g of maleic anhydride, 5.00g of norbornene and 0.58g of benzophenone in 150mL of dichloromethane, and irradiate with ultraviolet light for 12 hours while stirring; add 30mL of ethanol and 0.1g of p-toluenesulfonate after removing the solvent acid, heated to reflux at 100°C for 48 hours; removed the solvent again, extracted with 3×50mL ether, washed with saturated sodium bicarbonate solution, and dried over anhydrous magnesium sulfate; filtered to remove the ether to obtain 1.67g colorless viscous bicyclo[2, 2,1]-Diethyl 2,3-[alpha,[beta]succinate.

[0044] through 1 H NMR (CDCl 3 , 300MHz) analysis results: δ1.30-1.55 (m, 12H, 6CH 2 , 6CH 3 ); δ2.04(m, 2H, CH); δ3.14(m, 2H, CH); δ4.12(m, 4H, CH 2 ).

[0045] 2. Preparation of solid titanium catalyst

[0046] Add 5.0 g of anhydrous MgCl to the glass bottle reactor fully replaced by high-purity nitrogen 2 , 50 mL of toluene, 6...

Embodiment 2

[0056] In addition to changing the addition of bicyclo[2,2,1]-2,3-α,β-diethyl succinate and diisobutyl phthalate to 3mmol, other processes and operations are consistent with the examples 1, the results are shown in Table 1. Solid content titanium (wt%) 2.1, specific surface area 256m 2 / g. Catalyst particle size (D50): 19.84 microns, particle size distribution (SP): 0.9. SEM showed that the particles were spherical in shape.

Embodiment 3

[0058] In addition to changing the amount of bicyclo[2,2,1]-2,3-α,β-diethyl succinate and diisobutyl phthalate to 0.4mmol and 7.6mmol, other processes and operations Same as Example 1, the results are shown in Table 1. Solid content titanium (wt%) 2.2, specific surface area 255m 2 / g. Catalyst particle size: D50: 22.8 microns, particle size distribution (SP): 1.2. SEM showed that the particles were spherical in shape.

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Abstract

The invention discloses an olefin polymerization catalyst, which consists of two electron-donating compounds, including a polycyclic 1,4-diester compound shown as a general formula (I) and a phthalic acid ester compound and can be used for effectively solving the problems of poor hydrogen regulation sensitivity, over-narrow molecular weight distribution of a product and the like of a catalyst caused by separate use of an electron-donating compound. The average particle size of the obtained catalyst is 5-100 microns, and the specific surface area is more than 100 m<2> / g. The catalyst is approximately spherical, has high comprehensive performance, and can be well suitable for the requirements of slurry, gas-phase and mass propylene polymerization processes. The molecular weight distribution of an obtained polymerization product is appropriate.

Description

technical field [0001] The invention relates to an olefin polymerization catalyst and a preparation method thereof. Background technique [0002] Ziegler-Natta catalyst based on magnesium, titanium, halogen and electron donor for CH 2 =CHR Polymerization of olefins, especially in the polymerization of α-olefins with 3 carbon atoms or more, can give polymers with higher yield and higher stereoregularity. Among them, the internal electron donor compound, as an important component of Ziegler-Natta catalyst, plays a vital role in improving the performance of the catalyst. [0003] In the prior art, there are many compounds that can be used as electron donors in Ziegler-Natta catalysts, including polycarboxylic acids, monobasic or polycarboxylic acid esters, acid anhydrides, ketones, monoethers or polyethers and their derivatives. Aromatic carboxylic acid esters, such as di-n-butyl phthalate or diisobutyl phthalate (US6365685, US2001020073), etc., have the disadvantage of narro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/00C08F4/649C08F110/06C08F4/646
Inventor 徐人威朱博超贾军纪任峰胡徐腾赵旭涛姜立刚白虹张士玉邵月君
Owner PETROCHINA CO LTD
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