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

A technique for initiating systems and compounds, applied in the field of polyisobutylene, which can solve problems such as difficulty in increasing the molecular weight of polyisobutylene, complex production equipment, unstable catalyst, etc., and achieve the effects of improving initiating efficiency, increasing molecular weight, increasing solubility and stability

Active Publication Date: 2014-04-02
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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] At -40°C and under the protection of high-purity nitrogen, 20 mL of a solution containing isobutene (IB) and n-hexane ([IB]=2mol / L) was added, and then BF was added. 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 terminated 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 to constant weight. The weight average molecular weight of polyisobutylene (M w ) is 9.5×10 4 , the molecular weight distribution (M w / M n ) is 2.4.

Embodiment 2

[0029] Under the protection of high-purity nitrogen at -42 °C, 20 mL of a solution containing isobutene (IB) and n-hexane ([IB]=2mol / L) was added, and then BF was added. 3 , methanol, tetrahydrofuran composition of the initiation system, so that BF 3 / methanol = 9 (molar ratio), BF 3 / tetrahydrofuran=20 (molar ratio), BF 3 / IB=1.6×10 -3 (The molar ratio of). After 10min of polymerization, the termination reaction and post-processing method are the same as those in Example 1. The yield of polyisobutylene was 26%, M w 8.5×10 4 , M w / M n is 2.7.

Embodiment 3

[0031] Under the protection of high-purity nitrogen at -37°C, 20 mL of a solution containing isobutene (IB) and n-hexane ([IB]=2mol / L) was added, and the initiation system was added in the same manner as described in Example 1, 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 10min of polymerization, the termination reaction and post-processing method are the same as those in Example 1. The yield of polyisobutylene 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 boron trifluoride (BF 3 ) and a method for preparing polyisobutylene. Specifically, it involves using an initiation system composed of an initiator, boron trifluoride and an organic compound ligand to initiate cationic polymerization of isobutene in a liquid phase to prepare polyisobutene of medium molecular weight and high molecular weight series. Background technique [0002] Polyisobutylene is a versatile polymer that has different applications depending on its molecular weight. Low molecular weight polyisobutene, its number average molecular weight (M n ) between 500 and 5000, mainly used as lubricating oil additive, armyworm agent, electrical cable insulating oil, etc.; the weight average molecular weight of medium molecular weight polyisobutylene is usually 3×10 4 ~1.5×10 5 It is mainly used as sealant, adhesive, chewing gum base, paraffin modifier, asphalt modifier, etc.; the weight average molecula...

Claims

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Application Information

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Patent Type & Authority Patents(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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