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A kind of composite catalyst for synthesizing polyisobutylene and its preparation method and application

A composite catalyst and polyisobutylene technology, applied in the field of boron/titanium composite catalyst and its preparation, can solve the problems of a large amount of energy consumption, equipment maintenance costs, complex catalyst composition, low activity, etc., and achieve low catalyst residue and clear and translucent appearance. , the effect of high activity

Active Publication Date: 2020-06-02
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] At present, BASF is the manufacturer with the most complete grades and the best quality of high molecular weight polyisobutylene in the world. BASF introduced the preparation method of high molecular weight polyisobutylene in the patent CN104136470. 3 , iron halide, AlCl 3 Or a Lewis acid complex of an alkylaluminum halide or a Lewis acid combined with an organic sulfonic acid as an initiator as a polymerization catalyst, plus at least one reaction accelerator and at least one chain length regulator, using the "BASF ribbon" The polymerization process can produce high molecular weight polyisobutylene with a molecular weight of 400,000 to 5,000,000, but the composition of the catalyst is complex and the activity is low. energy consumption and equipment maintenance costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Under the protection of high-purity nitrogen, add 50ml of isobutylene, 100ml of solvent n-hexane and deionized water into the polymerization bottle at -30°C, and then add BF 3 · Ether · TiCl 4 Initiating system, wherein BF in the initiating system 3 The content accounts for 4% of the mass of raw material isobutene, BF 3 , ether, TiCl 4 1. The molar ratio of water is 1:1:1:1. After reacting for 30 minutes, add 3ml of ethanol solution containing NaOH (concentration is 3%wt.) to terminate the reaction. Polymerization product Mn=34650, Mw=118503, molecular weight distribution 3.42, polymer yield 79.88%, catalyst activity 1.35×10 3 gPIB·mol (BF3+TiCl4) -1 h -1 .

Embodiment 2

[0039] Under the protection of high-purity nitrogen, add 50ml of isobutene, 100ml of solvent n-hexane and quantitative deionized water into the polymerization bottle at -30°C, and then add BF 3 · Methanol · TiCl 4 Initiating system, wherein BF in the initiating system 3 The content accounts for 0.1% of the mass of raw material isobutylene, BF 3 , methanol, TiCl 4 1. The molar ratio of water is 1:1:1:1. After reacting for 30 minutes, add 3ml of ethanol solution containing NaOH (concentration is 3%wt.) to terminate the reaction. Polymerization product Mn=22026, Mw=280170, molecular weight distribution 12.72, polymer yield 62.26%, catalyst activity 4.22×10 4 gPIB·mol (BF3+TiCl4) -1 h -1 .

Embodiment 3

[0041] Under the protection of high-purity nitrogen, add 50ml of isobutene, 100ml of solvent n-hexane and quantitative deionized water into the polymerization bottle at -30°C, and then add BF 3 ·Ethanol·TiCl 4 Initiating system, wherein BF in the initiating system 3 The content accounts for 0.05% of the mass of raw material isobutylene, BF 3 , ethanol, TiCl 4 1. The molar ratio of water is 1:1:1:1. After reacting for 30 minutes, add 3ml of ethanol solution containing NaOH (concentration is 3%wt.) to terminate the reaction. Polymerization product Mn=32104, Mw=462618, molecular weight distribution 14.41, polymer yield 63.97%, catalyst activity 8.6×10 4 gPIB·mol (BF3+TiCl4) -1 h -1 .

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PUM

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Abstract

The invention relates to a novel boron / titanium composite catalyst for synthesizing polyisobutene, a preparation method and application thereof. In the isobutylene raw material system, the use of BF 3 The composite catalyst system formed by complexing oxygen-containing complexes with titanium-containing compounds and oxygen- and / or nitrogen-containing ligands initiates the polymerization of isobutylene, and can prepare medium and high-molecular-weight polyisobutenes with narrow molecular weight distribution at higher temperatures. The weight-average molecular weight of polyisobutylene is between 50,000 and 5,000,000, and the catalyst has high polymerization activity, the highest measurable activity can reach 1.03×10 7 gPIB·mol (BF3+TiCl4) ‑1 h ‑1 .

Description

technical field [0001] The invention relates to a composite catalyst for synthesizing polyisobutene and a preparation method thereof, in particular to a boron / titanium composite catalyst for synthesizing medium and high molecular weight polyisobutene, a preparation method and application thereof. Background technique [0002] Polyisobutylene is a homopolymer obtained by cationic polymerization of isobutylene. According to the molecular weight, it can be divided into low molecular weight polyisobutene, medium molecular weight polyisobutene and high molecular weight polyisobutene. [0003] Low molecular weight polyisobutene generally refers to isobutylene homopolymer with a molecular weight between 500 and 5000, which is a liquid with good fluidity or viscous, mainly used in the production of lubricating oil additives or fuel oil additives; high activity low molecular weight polyisobutene is generally Refers to low-molecular-weight polyisobutene with terminal α-double bond co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F110/10C08F4/16C08F4/14
CPCC08F4/14C08F4/16C08F110/10
Inventor 刘柏平黎源董科陈海波刘振孙双翼程瑞华胡兵波华卫琦
Owner WANHUA CHEM GRP CO LTD
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