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Controllable polymerization method of industrial-grade monomer

A polymerization method and an industrial-grade technology, which are applied in the field of preparing polymethyl methacrylate by atom transfer radical polymerization, can solve the problems of troublesome polymerization of inhibitors and increased costs, and achieve industrial production convenience, low toxicity, and The effect of reducing production costs

Inactive Publication Date: 2010-12-15
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The addition of the polymerization inhibitor has brought troubles to the implementation of the polymerization reaction. During the polymerization, it is often necessary to remove the polymerization inhibitor in the monomer in advance so that the reaction can proceed smoothly, which adds additional costs to industrial production.

Method used

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  • Controllable polymerization method of industrial-grade monomer
  • Controllable polymerization method of industrial-grade monomer
  • Controllable polymerization method of industrial-grade monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment one: synthesis polymethyl methacrylate (PMMA) under deoxygenation condition

[0028] Add MMA, EBiB, FeCl in a molar ratio of 300:1:0.2:0.6 based on 3mL MMA (unrefined) into several clean 5mL ampoules 3 ·6H 2 O and PPh 3 , add a small stirrer, seal each ampoule via argon gas for 20 minutes, place it in an oil bath at 90°C for reaction, and take samples at certain intervals. Open the seal, dissolve the polymer with a small amount of THF, then pour the solution into a beaker filled with 200mL industrial methanol (with two drops of concentrated hydrochloric acid added in advance) to precipitate, put the beaker in a fume hood and let it stand for more than 10h, and collect the precipitate by suction filtration. Place in a constant temperature oven at 50°C and dry to constant weight, weigh, calculate the conversion rate, and save the product for GPC characterization.

[0029] The result is as figure 1 , figure 2 shown, from figure 1 , we can see that the pol...

Embodiment 2

[0030] Embodiment two: synthesizing PMMA under the presence of air

[0031] Add MMA, EBiB, and FeCl in a molar ratio of 300:1:0.2:0.6 based on 3mL MMA (unrefined) into several clean 5mL ampoules 3 ·6H 2 O and PPh 3 , after adding a small stirring bar, seal it directly under air atmosphere (without excluding oxygen), place it in an oil bath at 90°C for reaction, and take samples at certain intervals. Open the seal, dissolve the polymer with a small amount of THF, then pour the solution into a beaker filled with 200mL industrial methanol (with two drops of concentrated hydrochloric acid added in advance) to precipitate, put the beaker in a fume hood and let it stand for more than 10h, and collect the precipitate by suction filtration. Place in a constant temperature oven at 50°C and dry to constant weight, weigh, calculate the conversion rate, and save the product for GPC characterization.

[0032] The result is as image 3 , Figure 4 shown by image 3 It can be seen that...

Embodiment 3

[0033] Example 3: Effect of Catalyst Consumption on Polymerization under the Condition of Deoxygenation

[0034] Add 3mL MMA (unrefined) to 10 clean 5mL ampoules as a basis, different ratios (molar ratios are 300 / 1 / 0.05 / 0.15, 300 / 1 / 0.1 / 0.3, 300 / 1 / 0.2 / 0.6 , 300 / 1 / 0.3 / 0.9, 300 / 1 / 0.5 / 1.5) MMA, EBiB, FeCl 3 ·6H 2 O and PPh 3, two experiments were done for each group of ratios, a small stirring bar was added, each ampoule was sealed with argon gas for 20 minutes, and placed in an oil bath at 90°C for the set time. Open the seal, dissolve the polymer with a small amount of THF, then pour the solution into a beaker containing 200mL industrial methanol (with two drops of concentrated hydrochloric acid added in advance) to precipitate, put the beaker in a fume hood and let it stand for more than 10h, and collect the precipitate by suction filtration. Place in a constant temperature oven at 50°C and dry to constant weight, weigh, calculate the conversion rate, and save the product fo...

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Abstract

The invention relates to a method for carrying out living polymerization by directly using an industrial-grade monomer, in particular to a method for preparing polymethyl methacrylate by carrying out atom transfer radical polymerization (AGET ATRP) reaction generating a catalyst through electron transfer by directly using the monomer, i.e. industrial-grade methyl methacrylate containing a polymerization inhibitor, belonging to the field of organic polymerization. The method comprises the following steps of: adding the monomer, an initiator, the catalyst and a coordinating agent according to the mole ratio of monomer:initiator:catalyst:coordinating agent=(100-1000):1:(0.05-1):(0.15-3) by taking the industrial-grade methyl methacrylate as the monomer; and carrying out the atom transfer radical polymerization (AGET ATRP) reaction generating the catalyst through the electron transfer to synthesize a high molecular polymer under the catalysis of ferric salt. The invention decreases the steps of eliminating the polymerization inhibitor by carrying out the AGET ATRP polymerization by directly using the industrial-grade methyl methacrylate containing the polymerization inhibitor, simplifies the polymerization process and greatly reduces the production cost.

Description

technical field [0001] The invention belongs to the field of organic polymerization, and relates to a method for directly using industrial-grade monomers for active polymerization, in particular to a method for directly using industrial-grade methyl methacrylate monomers containing polymerization inhibitors to generate catalysts through electron transfer Atom Transfer Radical Polymerization (AGET ATRP) is a method for preparing polymethyl methacrylate. Background technique [0002] A substance that can completely terminate the free radical polymerization of vinyl monomers. This effect is called polymerization inhibition. [0003] In order to avoid polymerization of ethylenic monomers during storage, transportation, etc., a small amount (about several hundred ppm) of polymerization inhibitors are often added to the monomers, for example, during transportation of methyl methacrylate monomers, polymerization inhibitors are usually added : Hydroquinone, hydroquinone methyl eth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/14C08F2/40C08F4/40
Inventor 张丽芬程振平朱秀林贡晶晶
Owner SUZHOU UNIV
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