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Initiation system for preparation of high reaction activity polyisobutylene and application

A technology of high reactivity and initiation system, which is applied in the field of preparing two series of high reactivity polyisobutenes with low molecular weight or medium molecular weight. Reduce the double bond content and other issues, achieve the effect of stable and controllable cationic polymerization of isobutylene, and increase the molecular weight

Active Publication Date: 2012-11-14
BEIJING UNIV OF CHEM TECH
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AI Technical Summary

Problems solved by technology

[0012] 1. When preparing low-molecular-weight high-reactivity polyisobutene, when the terminal α-double bond content is greater than 80%, the molecular weight distribution is wider (such as industrial products, M w / M n ~2.0), and the α-double bond content decreases with the increase of molecular weight, especially for initiating systems containing transition metals such as manganese, nickel, chromium or zinc, there is also the problem of slow polymerization rate;
[0013] 2. When preparing polyisobutene with medium molecular weight and high reactivity, the α-double bond content decreases with the increase of molecular weight, and the molecular weight distribution is wide, so it is difficult to achieve the goal of increasing molecular weight and reducing molecular weight distribution while synthesizing high terminal α-double bond content , especially for SnCl-based 4 Initiation system, there is also the problem of unstable polymerization, product end group structure, molecular weight and molecular weight distribution are difficult to control

Method used

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  • Initiation system for preparation of high reaction activity polyisobutylene and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] At 0°C and under the protection of high-purity nitrogen, add 20 mL of a solution containing isobutene (IB) and dichloromethane (IB=2.0mol L -1 ) in order to add H 2 O, isopropyl ether and SnCl 4 Initiate the polymerization of isobutylene, so that H 2 O / IB=9.5×10 -4 (molar ratio), isopropyl ether / IB=3.3×10 -3 (molar ratio), SnCl 4 / IB=2.6×10 -3 (The molar ratio of). After 30min, add 1mL 0.1g L -1 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 for 24 hours to remove volatile impurities. The number average molecular weight (M n ) is 1400, the molecular weight distribution index (M w / M n ) was 1.39, and the terminal α-double bond content was 87%.

Embodiment 2

[0039] at 20°C and high-purity N 2 Under protection, dichloromethane, water, isopropyl ether and SnCl 4 Add to the reactor in order to prepare the initiator system solution, in which isopropyl ether / SnCl 4 =0.3,H 2 O / SnCl 4 =0.4, put it for 120h before use.

[0040] The polymerization raw material is the same as in Example 1. Under the protection of high-purity nitrogen at 0°C, the above-mentioned initiator system solution is added to initiate the polymerization of isobutylene, so that isopropyl ether / IB=7.9×10 -4 (molar ratio), H 2 O / IB=9.5×10 -4 (molar ratio), SnCl 4 / IB=2.6×10 -3 (The molar ratio of). After 30min, add 1mL 0.1g L -1 NaOH / C 2 h 5 OH solution to terminate the reaction. The post-treatment method of the polymerized product is the same as in Example 1. Obtained polyisobutene 1.6g, M n for 1900, M w / M n is 2.07, and the terminal α-double bond content is 86%.

Embodiment 3

[0042] The dosage of each component of the initiation system and the preparation steps are the same as in Example 2, except that the preparation temperature is -30°C.

[0043] Initiating system consumption, polymerization raw materials, reaction steps and polymerization product post-treatment method are the same as implementation 2. Obtain polyisobutene 1.5g, M n for 2300, M w / M n is 2.01, and the terminal α-double bond content is 90%.

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Abstract

The invention relates to an initiation system for preparation of high reaction activity polyisobutylene and application. The initiation system consists of SnCl4, water and an organic compound containing oxygen, nitrogen and / or sulphur. The initiation system is added into an isobutene-containing polymerization raw material to induce cationic polymerization. The polymerization temperature is controlled at -60-30DEG C, and the polymerization reaction is stable and easy to control. Optimally, the terminal group alpha-double bond content can reach 98%. And according to needs, the initiation system can be used to prepare high reaction activity polyisobutylene with a number average molecular weight of 500-5000, a molecular weight distribution index up to 1.3 and an alpha-double bond content greater than 80%mol, a low molecular weight and narrow molecular weight distribution, and high reaction activity polyisobutylene with a number average molecular weight of 8000-15000, a molecular weight distribution index up to 1.6, an alpha-double bond content over 80%mol, a medium molecular weight and narrow molecular weight distribution.

Description

technical field [0001] The invention relates to an initiation system for the preparation of highly reactive polyisobutene, in particular based on SnCl 4 Initiation system for the preparation of low molecular weight (M n =500-5000) or medium molecular weight (M n =8000-15000) two series of highly reactive polyisobutenes. Background technique [0002] The preparation of polyisobutene from isobutene is a typical carbocationic polymerization reaction. During the carbocation polymerization reaction, proton removal and rearrangement reactions can occur at the end of the active chain. According to the position of the proton removal, the generated double bonds are also located at the "end" (α-double bond) and "inside" of the macromolecule. (Internal double bonds, including three-substituted double bonds and some double bonds located inside the polyisobutylene molecule). The structural formula of the α-double bond at the "end" of the macromolecular chain is as follows: [0003] ...

Claims

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Application Information

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IPC IPC(8): C08F10/10C08F4/16
Inventor 吴一弦张瑜刘强
Owner BEIJING UNIV OF CHEM TECH
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