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Random copolymer polypropylene catalyst and preparation method thereof

A polypropylene catalyst and random copolymerization technology, applied in the field of polypropylene, can solve the problems of low activity and low catalyst orientation ability, and achieve the effect of high random phase content, high ethylene content and increasing ethylene copolymerization ability.

Active Publication Date: 2017-11-24
谢炳
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 1954 Natta invented TiCl 3 / AlR 3 Polypropylene Ziegler-Natta (Z-N) catalyst, but at that time the catalyst orientation ability was low and the activity was very low

Method used

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  • Random copolymer polypropylene catalyst and preparation method thereof
  • Random copolymer polypropylene catalyst and preparation method thereof
  • Random copolymer polypropylene catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0054] Preparation method of a part of internal electron donor

[0055] (1) Dimethyl N-methyl-7-azabicyclo[2.2.1]hept-5-ene-2,3-dicarboxylate

[0056] In a 250ml round bottom flask, add 8.1g (0.1mol) N-methylpyrrole and 14.4g (0.1mol) dimethyl maleate, 100mL solvent toluene, install a reflux condenser, and heat to reflux under magnetic stirring for 8 Hour. Pure crystallization after completion of the reaction, the product obtained is a white solid with a yield of 83%. 1H NMR (400MHz, CDCl3): 2.27(3H), 3.08(2H), 3.56(2H), 3.67(6H), 5.59(2H), MS(EI) m / z: 225(M+).

[0057] (2) Dicyclopentyl 1-chloro-N-methyl-7-azabicyclo[2.2.1]hept-5-ene-2,3-dicarboxylate

[0058] Add 11.5g (0.1mol) 1-chloro-N-cyclopentylpyrrole and 25.2g (0.1mol) dicyclopentyl maleate in a 250ml round bottom flask, 100mL solvent toluene, a reflux condenser tube, The reaction was heated under reflux for 10 hours under magnetic stirring. Pure crystallization after completion of the reaction, the product obtai...

Embodiment 1

[0063] Under anhydrous and oxygen-free conditions, 5.0 grams of microspherical magnesium chloride alcoholate particles (self-made, the preparation steps are the same as the document CN1110281A, the average particle size is 50 μm, the specific surface is 150-300m / g, and the molar ratio of alcohol and magnesium chloride content is 2.76 : 1, molecular formula: MgCl 2 ·2.76CH 3 CH 2 OH) was added to 30 ml of titanium tetrachloride liquid at -20°C, and after 1 hour of reaction, the temperature was gradually raised to 60°C; 0.82g of N-methyl-7-azabicyclo[2.2.1]hept-5 Dimethyl-ene-2,3-dicarboxylate, gradually heated to 120°C, reacted for 2 hours, and filtered; then added 30 ml of titanium tetrachloride, reacted at 120°C for 1 hour, and filtered. Wash with 20 ml of hexane at 60° C. for 5 times, wash once with 10 ml of hexane at room temperature, and dry in vacuum to obtain a magnesium chloride-supported catalyst.

[0064] The content of each component in the catalyst is shown in ...

Embodiment 2～9

[0072] Preparation of supported catalyst: In addition to the internal electron donor compound, 1-chloro-N-methyl-7-azabicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid dicyclopenta Dimethyl 1-chloro-2-methyl-N-methyl-7-azabicyclo[2.2.1]hept-5-ene-2,3-dicarboxylate, 5-methyl- Dimethyl 7-azabicyclo[2.2.1]hept-5-ene-2,3-dicarboxylate, N-cyclopentyl-7-azabicyclo[2.2.1]hept-5-ene -Dibutyl 2,3-dicarboxylate, N-phenyl-7-azabicyclo[2.2.1]hept-5-ene-2,3-dicarboxylate dimethyl, N-methyl- Dimethyl 5-chloro-7-azabicyclo[2.2.1]hept-5-ene-2,3-dicarboxylate, N-methyl-1-chloro-2-methyl-7-aza Dimethyl bicyclo[2.2.1]hept-5-ene-2,3-dicarboxylate, N-methyl-2-methyl-5-chloro-7-azabicyclo[2.2.1]heptane -5-ene-2,3-dicarboxylic acid dimethyl ester, all the other are the same as embodiment 1.

[0073] The content of each component in the catalyst is shown in Table 1.

[0074] The content of each component in the catalyst of table 1 is shown in the table

[0075]

[0076]

[0077] three-catalys...

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Abstract

The invention provides a random copolymer polypropylene catalyst. The random copolymer polypropylene catalyst comprises, by weight, 10-25% of magnesium, 1-15% of titanium, 40-60% of halogens and 1-20% of an internal electron donor. The internal electron donor is a 7-oxabicyclo[2. 2. 1]hepta-5-ene-2, 3-dicarboximide compound. The random copolymer polypropylene catalyst has high catalytic activity and stereoregularity. In olefin polymerization and especially in propylene polymerization, ultra-high polymerization activity of the ether catalyst is kept and the molecular weight distribution of the polypropylene is remarkably improved.

Description

technical field [0001] The invention relates to the field of polypropylene, in particular to a random copolymerization polypropylene catalyst and a preparation method thereof. Background technique [0002] Polypropylene is one of the fastest growing polyolefin materials, and its output is second only to polyethylene in the world. In 1954 Natta invented TiCl 3 / AlR 3 Polypropylene Ziegler-Natta (Z-N) catalyst, but at that time the catalyst orientation ability was low and the activity was very low. By the middle and late 1960s, certain Lewis bases (called internal electron donors) were mixed into titanium trichloride crystals by mechanical grinding or chemical methods, so that the surface area of ​​the catalyst was greatly increased, and the obtained polypropylene isotacticity reached 90-96%. People have gradually found that the electron donor introduced in the catalyst plays a key role in improving the performance of the catalyst. The electron donor can not only improve t...

Claims

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Application Information

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IPC IPC(8): C08F210/06C08F210/16C08F4/649C08F4/02
CPCC08F210/06C08F210/16C08F4/6495C08F4/022Y02P20/52
Inventor 谢炳
Owner 谢炳
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