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A method for the polymerization of vinyl monomers catalyzed by hindered Lewis acid-base pairs based on binuclear aluminum Lewis acids

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 the initiation efficiency is low, so as to achieve narrow molecular weight distribution, improve catalytic activity, and low price Effect

Active Publication Date: 2022-02-15
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • 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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  • A method for the polymerization of vinyl monomers catalyzed by hindered Lewis acid-base pairs based on binuclear aluminum Lewis acids
  • A method for the polymerization of vinyl monomers catalyzed by hindered Lewis acid-base pairs based on binuclear aluminum Lewis acids
  • A method for the polymerization of vinyl monomers catalyzed by hindered Lewis acid-base pairs based on binuclear aluminum Lewis acids

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, the polymerization results are as follows

[004...

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 a hindered Lewis acid-base pair based on dinuclear aluminum Lewis acid, and belongs to the technical field of polymer synthesis. The invention realizes high-efficiency catalysis of vinyl monomers under mild conditions with controllable polymer molecular weight and molecular weight distribution, and provides a new strategy and method for the controllable synthesis of polymers. The polymerization mechanism of the present invention involves the synergistic catalysis of binuclear aluminum for conjugate addition. The dual-nuclear aluminum catalyst system of the invention has the advantages of cheap and easy to obtain, convenient operation, mild reaction conditions, wide monomer adaptability and the like. In addition, the efficient conversion of different monomers can be realized by adjusting the pKa of Lewis acid / base, which can precisely control the molecular weight and molecular weight distribution of the polymer, and the initiation efficiency is close to 100%. This type of catalytic system can efficiently catalyze the homopolymerization and copolymerization of methyl methacrylate and butyl acrylate, and also provides a new synthesis strategy and approach for the copolymer thermoplastic elastomer of the two.

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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Patent Type & Authority Patents(China)
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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