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Method for catalyzing vinyl monomer polymerization by using hindered Lewis acid-base pairs based on binuclear aluminum Lewis acid

A technology of Lewis acid-base pair and Lewis acid, which is applied in the field of polymer synthesis, can solve the problems that polymers cannot be obtained at the same time, monomers cannot be converted, and side reactions can be terminated, so as to achieve narrow molecular weight distribution, improve catalytic activity, and precisely control Effect

Active Publication Date: 2020-06-23
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most existing Lewis acid-base pairs catalyze the polymerization of polar vinyl monomers with low initiation efficiency, complete conversion of monomers, high molecular weight and narrow molecular weight distribution. Transfer and chain termination side reactions
In addition, the most current research is the mononuclear aluminum Lewis acid system, and the catalytic system based on the binuclear aluminum Lewis acid has not been reported yet.

Method used

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  • Method for catalyzing vinyl monomer polymerization by using hindered Lewis acid-base pairs based on binuclear aluminum Lewis acid
  • Method for catalyzing vinyl monomer polymerization by using hindered Lewis acid-base pairs based on binuclear aluminum Lewis acid
  • Method for catalyzing vinyl monomer polymerization by using hindered Lewis acid-base pairs based on binuclear aluminum Lewis acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] In the glove box, the indicated amount of Lewis acid ([Al(mbmp)Me] 2 ) specified amount of MMA, then add 2mL of toluene solution, stir evenly, then add specified amount of Lewis base ( iPr I m ) feeding is completed, the reaction begins timing, after the reaction, the Schlenk bottle is taken out from the glove box, and quenched by adding methanol solution containing 5% BHT, getting 0.2mL to measure its NMR in deuterated chloroform, then using the remaining liquid A large amount of methanol is extracted, the solid is taken out, dried in a vacuum oven at 40°C to constant weight, the conversion rate is calculated according to the NMR results, and the molecular weight and molecular weight distribution of the obtained polymer are measured by gel permeation chromatography. The reaction conditions and test results are as follows:

[0043] Table 1 base ( iPr I m ) as a Lewis base obtained under different reaction conditions of the polymerization results are as follows

[0...

Embodiment 2

[0046] The reaction was carried out in a glove box, and 0.024 mmol of Lewis acid ([Al(mbmp)Me] 2 ), 2mL of toluene and 0.5mL (4.8mmol) of MMA, after stirring evenly, add 0.024mmol of Lewis base. Quenched with methanol solution, take 0.2mL in 0.4mL deuterated chloroform to measure its NMR, then extract the remaining liquid with a large amount of methanol, take out the solid, dry it in a vacuum oven at 40°C to constant weight, and calculate according to the NMR results Conversion rate, molecular weight and molecular weight distribution of the obtained polymer were measured by gel permeation chromatography. The reaction conditions and test results are as follows:

[0047] Table 2 [Al(mbmp)Me] 2 Synergistic Catalysis of MMA Polymerization with Different Lewis Bases

[0048]

[0049] Through this group of experiments, it is proved that the initiation efficiency of the MMA monomer based on the binuclear aluminum Lewis acid and the adopted Lewis base is 100%. The superiority of ...

Embodiment 3

[0051] The reaction was carried out in a glove box, and the designated Lewis acid ([Al(mbmp)Me] 2 ), 2mL of solvent and quantitative MMA, after stirring evenly, add Lewis base ( iPr I m ), the feeding was completed, and the reaction began to be timed. After the reaction, the schlenk bottle was taken out from the glove box, and the methanol solution containing 5% BHT was added to quench, and 0.2mL was measured in 0.4mL deuterated chloroform to measure its NMR, and then the remaining The liquid was extracted with a large amount of methanol, and the solid was taken out, dried in a vacuum oven at 40°C to constant weight, the conversion rate was calculated according to the NMR results, and the molecular weight and molecular weight distribution of the obtained polymer were measured by gel permeation chromatography. The reaction conditions and test results are as follows:

[0052] Table 3 Polymerization of MMA in different solvents

[0053]

[0054] Through the above experiment...

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Abstract

The invention discloses a method for catalyzing vinyl monomer polymerization by using hindered Lewis acid-base pairs based on binuclear aluminum Lewis acid, which belong to the technical field of polymer synthesis. According to the method, the vinyl monomer is efficiently catalyzed under mild conditions, the molecular weight and molecular weight distribution of the polymer are controllable, and anew strategy and the method are provided for controllable synthesis of the polymer. The polymerization mechanism in the invention relates to conjugate addition under the synergistic catalytic action of binuclear aluminum. The binuclear aluminum catalytic system disclosed by the invention has the advantages of low cost, easiness in obtaining, convenience in operation, mild reaction conditions, widemonomer adaptability and the like. In addition, efficient conversion of different monomers can be achieved by adjusting pKa of Lewis acid / base, the molecular weight and molecular weight distributionof the polymer can be accurately regulated and controlled, and the initiation efficiency is close to 100%. The catalytic system can efficiently catalyze homopolymerization and copolymerization reactions of methyl methacrylate and butyl acrylate, and also provides a new synthesis strategy and approach for copolymer thermoplastic elastomers of methyl methacrylate and butyl acrylate.

Description

technical field [0001] The invention relates to a method for catalyzing the polymerization of vinyl monomers by a hindered Lewis acid-base pair based on a binuclear aluminum Lewis acid, which belongs to the technical field of polymer synthesis, and specifically relates to a preparation method of a binuclear organometallic aluminum Lewis acid and a method for catalyzing vinyl polar monomers. A living polymerization system for the synthesis of high molecular weight polymers. Background technique [0002] Polymethyl methacrylate, or PMMA, commonly known as plexiglass, is a transparent organic polymer material. Because of its unique physical and chemical properties, it has the advantages of light texture, easy processing, good light transmittance, and resistance, and is widely used in automobiles, construction, medicine and other fields. At present, China's demand for PMMA is increasing day by day, but the production technology of PMMA is mainly mastered by enterprises in devel...

Claims

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Application Information

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IPC IPC(8): C08F120/14C08F120/18C08F4/54
CPCC08F120/14C08F120/18C08F4/54C08F2500/03
Inventor 王晓武王哲咸漠
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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