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Ultra-high molecular weight polyolefin catalyst as well as preparation method and application thereof

A catalyst, polyolefin technology, applied in the field of polyolefin catalyst

Active Publication Date: 2020-06-23
叶平山
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The shape of the polymer is an approximate copy of the shape of the catalyst. For UHMWPE, how to prepare a catalyst with good shape, good particle size distribution, and high polymerization activity, so as to obtain a polymer with high bulk density and easy processing is of great importance to scientific research. Workers still face challenges

Method used

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  • Ultra-high molecular weight polyolefin catalyst as well as preparation method and application thereof
  • Ultra-high molecular weight polyolefin catalyst as well as preparation method and application thereof
  • Ultra-high molecular weight polyolefin catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example

[0078] Preparation example: Synthesis of 3-(3,4-dimethylphenyl)-isoxazole-4,5-diethyl carbonate

[0079]

[0080] Replace the air with nitrogen in the reaction flask, add 12.0ml tetrahydrofuran and 1.04g 3,4-dimethylbromobenzene, cool down to -50°C, slowly add 4.62ml butyllithium (1.55mol, n-hexane), and react for 30 Minutes, add 556.0 microliters of dimethylformamide, slowly rise to room temperature, react for 1 hour, then add 624mg of hydroxylamine hydrochloride and 1.42g of potassium carbonate, react at room temperature for 2 hours, then remove the solvent, add 30.0 ml acetonitrile, 8.0ml hydrochloric acid (1.0mol / L), 22.0ml water, 1.5g diethyl propiolate, 5.46g dioxane, after three minutes, rise to room temperature, and react for 1 hour, extract with ethyl acetate , dried over sodium sulfate, and the product was isolated.

[0081] Referring to the above method, other isoxazole ester compounds used in the examples were synthesized.

Embodiment 1

[0083] A kind of preparation method of ultrahigh molecular weight polyethylene catalyst, this preparation method comprises the following steps:

[0084] (1) After dispersing 2 grams of ethoxymagnesium with 4ml octanol and 15ml n-heptane solvent, place it in a reactor under the protection of an inert gas, and then add 0.03mol 3-phenyl-isoxazole-4 to the reactor , 5-dimethyl carbonate, heated to 40°C and mixed for 2h;

[0085] (2) Cool the system prepared in step (1) to -25°C, slowly add 20ml TiCl 4 Solution, heated up to 10°C and reacted for 2 hours;

[0086] (3) Add 0.4 g of methyl tert-butyldimethoxysilane to the system prepared in step (2) and react at 80° C. for 2 hours, and filter off the supernatant after the reaction;

[0087] (4) Add 25ml TiCl to the filtered solid in step (3) 4 mixed solution with ethyl titanate, TiCl 4 The molar ratio with ethyl titanate was 1:1, and the temperature was gradually raised to 110°C for 2 hours, filtered, washed, and vacuum-dried to o...

Embodiment 2

[0090] A kind of preparation method of ultrahigh molecular weight polyethylene catalyst, this preparation method comprises the following steps:

[0091] (1) After dispersing 2 grams of ethoxymagnesium with 4ml octanol and 15ml n-heptane solvent, place it in a reactor under the protection of an inert gas, and then add 0.03mol 3-(3-isopropylphenyl )-isoxazole-4,5-diethyl carbonate, heated to 80°C and mixed for 1 hour;

[0092] (2) Cool the system prepared in step (1) to -30°C, slowly add 20ml TiCl 4 Solution, after heating up to 25°C, react for 1.5h;

[0093] (3) Add 0.4 g of diisobutyldimethoxysilane to the system prepared in step (2) and react at 80° C. for 2 hours, and filter off the supernatant after the reaction;

[0094] (4) Add 25ml TiCl to the filtered solid in step (3) 4 Mixed solution with n-butyl titanate, TiCl 4 The molar ratio with n-butyl titanate is 2:1, and the temperature is gradually raised to 90°C for 3 hours, filtered, washed, and vacuum-dried to obtain a...

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Abstract

The invention belongs to the technical field of polyolefin catalysts, and particularly relates to an ultra-high molecular weight polyolefin catalyst as well as a preparation method and application thereof. The invention provides a polyolefin catalyst as well as a preparation method and application thereof. An isoxazole ester compound is used for treating the surface and pore structure of a carrier; the solubility of the carrier in a solvent is increased; a catalytic system has proper Ti<3+> and Ti<4+> distribution; the particle morphology of the catalyst and the growth capacity of a polymer onthe active sites of the catalyst are improved, the addition of the titanium compound is combined to promote the stable release of the catalyst activity, the granularity and the powder stacking density of the polymer are favorably controlled, the molecular weight of the polymer is easy to adjust, and the molecular weight of the polymer can reach 4,200,000 or above. When the prepared catalyst is used for olefin polymerization, UHMWPE having the advantages of high activity, flexible molecular weight adjustment and high polymer stacking density can be obtained, and the catalyst has an excellent industrial prospect.

Description

technical field [0001] The invention belongs to the technical field of polyolefin catalysts, and in particular relates to an ultrahigh molecular weight polyolefin catalyst and its preparation method and application. Background technique [0002] Ultra-high molecular weight polyethylene (UHMWPE) has unparalleled impact resistance, abrasion resistance, chemical corrosion resistance, low temperature resistance, stress crack resistance, anti-adhesion ability, excellent insulation, safety and health and other engineering plastics. Self-lubricating properties, can be widely used in machinery, papermaking, mining, electric power, agriculture, sports, transportation and other fields. [0003] UHMWPE generally has a molecular weight greater than 1.5 million and a low melt index, and the product is mainly in the form of powder. The morphology, particle size distribution and resulting bulk density of the powder are its important characteristics, which seriously affect the processing p...

Claims

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Application Information

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IPC IPC(8): C08F10/00C08F110/02C08F4/646C08F4/651C08F4/656
CPCC08F10/00C08F110/02C08F4/6465C08F4/651C08F4/656C08F2500/01C08F2500/18
Inventor 叶平山
Owner 叶平山
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