Activity-controllable (gamma-methyl)-alpha-methylene-gamma-butyrolactone polymerizing method

A methylene and butyrolactone technology is applied in the field of active controllable polymerization catalyst systems, which can solve the problems of long reaction time, difficult to achieve complete conversion of monomers, etc., and achieves easy availability of raw materials, good chain extension, and high conversion rate. Effect

Active Publication Date: 2018-06-12
JILIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The polymerization requires a long reaction time, and it

Method used

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  • Activity-controllable (gamma-methyl)-alpha-methylene-gamma-butyrolactone polymerizing method

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Experimental program
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Effect test

Embodiment 1

[0045] Embodiment 1 A kind of specific synthetic method of enol silyl ether described in the present invention

[0046] Synthesis of dimethylketene-methyl-dimethylethoxy acetal Me 2 C=C(OMe)OSiMe 2 (EtO) ( Me2 (EtO) SKA).

[0047] 1) Synthesis of dimethylethoxychlorosilane (Me 2 (EtO)SiCl)

[0048]

[0049] In a glove box filled with nitrogen, take ethanol (5.08mL, 90.0mmol) and B(C 6 f 5 ) 3 (461mg, 0.90mmol) into a 200mL Schlenk bottle, add dichloromethane (100mL) and seal it with an inversion plug, take out the glove box and connect it to the Schlenk line, cool to -78°C and keep it for 20min. Dimethylchlorosilane (10.0 mL, 90.0 mmol) was slowly added dropwise into the system via a syringe. Slowly warm up to room temperature (over 30 min), dichloromethane was removed in vacuo (be careful not to extract the product), and distillation under reduced pressure gave a colorless oily product. 12.48 g of the product was obtained with a yield of 91%. 1 H NMR (500MHz, Be...

Embodiment 2

[0053] Example 2 Polymerization of γ-methyl-α-methylene-γ-butyrolactone (MMBL) and α-methylene-γ-butyrolactone (MBL)

[0054] The polymerization reaction was carried out in a glove box, and the Lewis acid was weighed in a 20 ml reaction bottle, and MMBL (0.5ml, 4.68mmol) or MBL (0.41mL, 4.68mmol) was added. After the monomer reacted fully with the Lewis acid, two Chloromethane solvent (the total volume of the solution after adding is 5mL), add the enol silyl ether that has been weighed ( R SKA), and start timing, stir for a period of time until the monomer is completely converted, the reaction bottle is taken out from the glove box, and 5% HCl / methanol solution is added to terminate the polymerization reaction. The polymer was filtered off, washed thoroughly with methanol, and dried in vacuum at 60°C until constant weight. The molecular weight and molecular weight distribution of the resulting polymers were determined by gel permeation chromatography.

[0055] The characteri...

Embodiment 3

[0064] Example 3 Chain extension of MMBL

[0065] The polymerization reaction was carried out in the glove box, and the Al(C 6 f 5 ) 3 In a 20 ml reaction bottle, add MMBL (0.5 ml, 4.68 mmol), after the monomer and Lewis acid have fully reacted, add tetrahydrofuran solvent (the total volume of the solution after adding is 5 mL), add the weighed iBu SKA, and start timing, stir for a period of time until the monomers are completely converted, then add MMBL (0.5ml, 4.68mmol), and then add MMBL (0.5ml, 4.68mmol) after a period of time to make the monomers completely converted, and wait until all the monomers are completely converted After complete conversion of the body, the reaction bottle was taken out of the glove box, and 5% HCl / methanol solution was added to terminate the polymerization reaction. The polymer was filtered off, washed thoroughly with methanol, and dried under vacuum at 60°C to constant weight. The molecular weight and molecular weight distribution of the re...

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Abstract

The invention relates to an activity-controllable (gamma-methyl)-alpha-methylene-gamma-butyrolactone polymerizing method and belongs to the technical field of polymer synthesis. Silyl enol ether is applied as initiator and Lewis acid as catalyst to catalyzing activity-controllable polymerization and copolymerization of MMBL ((gamma-methyl)-alpha-methylene-gamma-butyrolactone) and MBL (alpha-methylene-gamma-butyrolactone). According to the activity-controllable (gamma-methyl)-alpha-methylene-gamma-butyrolactone polymerizing method, monomers to be polymerized are renewable resources and has a wide application prospect; the polymerization system of the monomers has the advantages of being convenient to operate, mild in reaction conditions, rapid, high in conversion rate and the like; the prepared polymer is controllable in molecular weight and narrow in molecular weight distribution and accordingly achieves activity-controllable polymerization.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and specifically relates to an activity controllable polymerization catalytic system. The system uses Lewis acid as a catalyst and enol silyl ether as an initiator and can be applied to a renewable monomer (γ-methyl)-ɑ - Living-controlled polymerization of methylene-γ-butyrolactone ((M)MBL), and copolymerization between two monomers. Background technique [0002] Energy issues are the main issues in today's human society. Since humans began to use fossil energy. Coal, oil and natural gas are rapidly developing as the most important sources of energy and chemicals. Currently, approximately 86% of energy and 96% of chemicals are derived from these non-renewable petroleum products. It is foreseeable that petroleum products will not be able to meet the increasing demands of human society in the near future. What's more serious: According to the prediction of relevant experts, at the cur...

Claims

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Application Information

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IPC IPC(8): C08G63/08C08G63/84
CPCC08G63/08C08G63/823
Inventor 张越涛何江华胡路
Owner JILIN UNIV
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