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Initiation system based on boron trifluoride and method for preparing polyisobutylene using initiation system

A technology for initiating systems and compounds, applied in the field of polyisobutene, can solve the problems of difficulty in increasing the molecular weight of polyisobutene, extremely high equipment requirements, complex production equipment, etc., and achieve the effects of improving initiation efficiency, increasing molecular weight, and improving utilization rate.

Active Publication Date: 2012-12-05
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The main technical problems are: the catalyst is unstable and easy to separate; it is difficult to solve the problem of β-H removal when initiating the polymerization of isobutene, which makes it difficult to increase the molecular weight of polyisobutene. Therefore, when the polymerization temperature is higher than -30 ° C Usually only polyisobutene with low molecular weight and high reactivity can be obtained; the production equipment used to prepare medium molecular weight and high molecular weight polyisobutene is complex, and the requirements for equipment are extremely high, such as conveyor belt devices, the production cost is high, and the molecular weight distribution of polyisobutene obtained It is wide; it is difficult to directly initiate the polymerization of the by-product carbon four fractions of petroleum cracking or catalytic cracking to synthesize polyisobutene products of medium molecular weight; extremely low polymerization temperature (such as -104 ° C, the boiling point of ethylene) is required to obtain high molecular weight polyisobutene product, high energy consumption

Method used

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  • Initiation system based on boron trifluoride and method for preparing polyisobutylene using initiation system
  • Initiation system based on boron trifluoride and method for preparing polyisobutylene using initiation system

Examples

Experimental program
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Effect test

Embodiment 1

[0027] At -40°C and under the protection of high-purity nitrogen, add 20 mL of a solution containing isobutene (IB) and n-hexane ([IB]=2mol / L), and then add 3 、H 2 The initiator system solution composed of O, tetrahydrofuran (THF), n-hexane and dichloromethane makes BF 3 / H 2 O=9.7 (molar ratio), BF 3 / THF=1.3 (molar ratio), BF 3 / IB=2.9×10 -3 (The molar ratio of). After polymerization for 10min, add 3mL of 0.1g / L NaOH / C 2 h 5 OH solution to terminate the reaction. The polymer product was precipitated with ethanol, washed repeatedly with deionized water and ethanol, and finally dried in a vacuum oven at 40°C until constant weight. The weight average molecular weight of polyisobutylene (M w ) is 9.5×10 4 , molecular weight distribution (M w / M n ) is 2.4.

Embodiment 2

[0029] At -42°C and under the protection of high-purity nitrogen, add 20 mL of a solution containing isobutene (IB) and n-hexane ([IB]=2mol / L), and then add 3 , methanol, tetrahydrofuran composition of the initiation system, so that the BF 3 / methanol = 9 (molar ratio), BF 3 / tetrahydrofuran=20 (molar ratio), BF 3 / IB=1.6×10 -3 (The molar ratio of). After polymerization 10min, termination reaction and aftertreatment method are with embodiment 1. Polyisobutylene yield was 26%, M w 8.5×10 4 ,M w / M n is 2.7.

Embodiment 3

[0031] At -37°C and under the protection of high-purity nitrogen, add 20 mL of a solution containing isobutene (IB) and n-hexane ([IB]=2mol / L), and use the method described in Example 1 to add the initiator system, so that BF 3 / phenol=160 (molar ratio), BF 3 / tetrahydrofuran = 8 (molar ratio), BF 3 / IB=2.8×10 -3 (The molar ratio of). After polymerization 10min, termination reaction and aftertreatment method are with embodiment 1. Polyisobutylene yield was 69%, M w 7.8×10 4 ,M w / M n is 3.5.

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Abstract

The invention relates to an initiation system based on boron trifluoride and a method for preparing polyisobutylene using the initiation system. The initiation system is composed of BF3, a proton donor and an electron donor, wherein the proton donor can be selected from water, methanol, ethanol, phenol, orthocresol, aromatic alcohol or aromatic acid compound; and the electron donor is an organic compound containing C3-C10 saturated oxa heterocyclic ether, cyclic amine aza heterocycle or epithio ether heterocycle. Two kinds of polyisobutylene with different molecular weights and narrower molecular weight distribution can be prepared according to needs by using the initiation system and adopting a common tank reactor: (1) medium-molecular-weight polyisobutylene, which has the molecular weight of 5*10<4>-1.5*10<5>, narrower molecular weight distribution and distribution index number (Mw / Mn) of 2.3-3.5; and (2) high-molecular-weight polyisobutylene, which has the molecular weight of 2.0*10<5>-1.5*10<6>, narrower molecular weight distribution and distribution index number (Mw / Mn) of 2.3-3.5. The production process is simple and the production cost is saved.

Description

technical field [0001] The present invention relates to a kind of based on boron trifluoride (BF 3 ) Initiation system and method for preparing polyisobutylene. Specifically, it involves adopting an initiating system composed of an initiator, boron trifluoride and organic compound ligands to initiate cationic polymerization of isobutene in a liquid phase to prepare polyisobutenes of medium molecular weight and high molecular weight series. Background technique [0002] Polyisobutylene is a versatile polymer with a wide range of applications depending on its molecular weight. Low molecular weight polyisobutylene, its number average molecular weight (M n ) between 500 and 5000, mainly used as lubricating oil additives, insecticides, electrical cable insulating oil, etc.; the weight average molecular weight of medium molecular weight polyisobutylene is usually 3×10 4 ~1.5×10 5 Among them, it is mainly used as sealant, adhesive, chewing gum base material, paraffin wax modifi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/10C08F4/14
Inventor 吴一弦周鹏张来宝
Owner BEIJING UNIV OF CHEM TECH
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