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Method for producing polymer

A manufacturing method and polymer technology, applied in the field of polymer manufacturing, can solve the problems of increase, damage of stirring paddle, high viscosity, etc.

Pending Publication Date: 2021-09-28
NISSAN CHEM IND LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method requires time for cooling when the scale of production is enlarged, and it is difficult to control the target molecular weight with good reproducibility.
In addition, for example, when the scale is too large and cooling is delayed due to failure in the cooling device, the molecular weight increases excessively, so there is a risk of high viscosity of the reaction liquid and damage to the stirring blade of the reactor.
[0003] On the other hand, as a method of suppressing the increase in molecular weight, generally, there is a method of greatly shifting the equivalent ratio of the diepoxy monomer and the reactive monomer from 1:1 (for example, 1:1.2, etc.), Although a large increase in molecular weight can be suppressed, it cannot be stabilized at the target molecular weight. In addition, since the excessively charged monomer remains in the system, a purification process for removing the residual monomer is required. From the viewpoint of productivity, not preferred

Method used

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  • Method for producing polymer
  • Method for producing polymer
  • Method for producing polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0194] A 200 mL reaction flask was charged with (A) 12.6 g of monoallyl diglycidyl isocyanuric acid, (B) 6.6 g of adipic acid, and (C) ethyltriphenylphosphonium bromide as a polymerization catalyst 0.84 g, (D) 0.18 g of pyridine as a co-catalyst, and 60 g of propylene glycol monomethyl ether were used to prepare a raw material solution. The molar ratio of (C)component and (D)component is 1:1, and the equivalent ratio of (A)component and (B)component is 1:1.01.

[0195] Next, this solution was heated and refluxed at 121° C., and reacted for 1 to 6 hours to synthesize a polymer. GPC analysis of the produced polymer showed that Mw=6400 at 1 hour after reaching reflux temperature, Mw=10100 at 2 hours, Mw=10500 at 4 hours, Mw=10400 at 5 hours, and at 6 hours Mw=10400, after 4 hours after reaching the reflux temperature, the weight average molecular weight Mw stabilized.

Embodiment 2

[0197] A 200 mL reaction flask was charged with (A) 12.6 g of monoallyl diglycidyl isocyanuric acid, (B) 6.6 g of adipic acid, and (C) ethyltriphenylphosphonium bromide as a polymerization catalyst 0.84 g, (D) 0.26 g of pyridine as a co-catalyst, and 60 g of propylene glycol monomethyl ether were used to prepare a raw material solution. The molar ratio of (C)component and (D)component is 1:1.5, and the equivalent ratio of (A)component and (B)component is 1:1.01.

[0198] Next, this solution was heated and refluxed at 121° C., and reacted for 1 to 7 hours to synthesize a polymer. GPC analysis of the produced polymer showed that Mw=6500 in the first hour after reaching the reflux temperature, Mw=8100 in the second hour, Mw=8100 in the fourth hour, Mw=8000 in the fifth hour, and Mw in the sixth hour Mw = 7900, Mw = 7800 at the 7th hour, and the weight average molecular weight Mw was stabilized after 2 hours after reaching the reflux temperature.

Embodiment 3

[0200] A 200 mL reaction flask was charged with (A) 12.6 g of monoallyl diglycidyl isocyanuric acid, (B) 6.6 g of adipic acid, and (C) ethyltriphenylphosphonium bromide as a polymerization catalyst 0.84 g, (D) 0.09 g of pyridine as a co-catalyst, and 60 g of propylene glycol monomethyl ether were used to prepare a raw material solution. The molar ratio of (C)component and (D)component is 1:0.5, and the equivalent ratio of (A)component and (B)component is 1:1.01.

[0201]Next, this solution was heated and refluxed at 121° C., and reacted for 1 to 7 hours to synthesize a polymer. GPC analysis of the produced polymer showed that Mw=8500 in the first hour after reaching the reflux temperature, Mw=13200 in the second hour, Mw=15000 in the fourth hour, Mw=14900 in the fifth hour, and Mw in the sixth hour Mw=14800 at 7 hours, Mw=14600 at 7 hours, after 4 hours after reaching the reflux temperature, the weight average molecular weight Mw stabilized.

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Abstract

Provided is a method for producing a polymer, characterized by reacting (A) an epoxy compound having two or more epoxy groups in the molecule with (B) a reactive compound having, in the molecule, two or more functional groups reactive with epoxy groups, in the presence of (C) a polymerization catalyst and (D) a cocatalyst.

Description

technical field [0001] The present invention relates to a method for producing a polymer by reacting an epoxy compound having two or more epoxy groups in a molecule with a reactive compound having two or more functional groups that react with epoxy groups in a molecule. Background technique [0002] In general, the molecular weight of a polymer has a great influence on physical properties, so the control of the molecular weight can be said to be a common problem in the production of polymers. The method described in Non-Patent Document 1 is known as a general method for producing a polymer in which at least one diepoxide compound is reacted with a compound having two or more reactive functional groups (reactive compound). Conventionally, in order to control the molecular weight of the polymer within the target range, the method of forcibly stopping the polymerization reaction by cooling at the stage where the target molecular weight is reached by strictly controlling the rea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/14C08G73/02G03F7/11C08G63/42
CPCC08G73/02C08G63/42G03F7/091G03F7/094G03F7/038C08G59/4207C08G59/423C08G59/688C08G59/686C08G59/26C08G59/14C08G59/245C08G59/3245G03F7/11
Inventor 津田悠太朗山口大希
Owner NISSAN CHEM IND LTD
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