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Manufacturing method of resin

A manufacturing method and resin technology, applied in the field of resin manufacturing, can solve problems such as large amount of residual monomers and insufficient batch productivity, and achieve the effect of suppressing pollution of manufacturing equipment and less volatilization

Active Publication Date: 2020-11-27
RESONAC CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, conventional methods for producing resins obtained by radical polymerization have problems such as molecular weight reproducibility, insufficient mass productivity, and large amounts of residual monomers.

Method used

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  • Manufacturing method of resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0081] Hereinafter, an Example and a comparative example are shown, and this invention is demonstrated concretely.

[0082] The measurement of the amount of residual monomers in the following examples and comparative examples was performed under the above-mentioned conditions by GPC in the same manner as the measurement of the weight average molecular weight.

[0083] In addition, the reproducibility of a weight average molecular weight was judged by the following criteria.

[0084] Reproducibility criteria

[0085] ○: The same polymerization reaction is repeated twice, and the rate of change of the weight average molecular weight of the second time ((weight average molecular weight of the second time - weight average molecular weight of the first time) / weight average molecular weight of the first time × 100) is in Within ±10%

[0086] ×: The same polymerization reaction is repeated twice, and the change rate of the weight average molecular weight of the second time deviat...

Embodiment 2

[0092] The thermal radical polymerization initiator was changed to 1,1,3,3-tetramethylbutyl peroxy-2-ethylhexanoate (manufactured by NOF Corporation, PEROCTA (registered trademark) O: 10 hours half-life temperature 65°C ), except that the reaction temperature was set at 109° C., the reaction was carried out in the same manner, and a carboxyl group-containing resin solution with a weight average molecular weight of 18,500 and a solid content acid value of 180 KOHmg / g was obtained. As a result of measuring the total amount of residual monomers, it was 0.7% by mass. Moreover, the same reaction was performed again, and as a result, the weight average molecular weight was 19300 and the reproducibility of molecular weight was favorable.

Embodiment 3

[0094] The thermal radical polymerization initiator was changed to tert-butyl peroxybenzoate (manufactured by Nippon Kayaku Co., Ltd., KAYABUTYL B (registered trademark): 10-hour half-life temperature 105°C), and the reaction temperature was set to 127°C. The reaction was carried out to obtain a carboxyl group-containing resin solution with a weight average molecular weight of 14800 and a solid content acid value of 180KOHmg / g. As a result of measuring the total amount of residual monomers, it was 0.6% by mass. Moreover, the same reaction was performed again, and as a result, the weight average molecular weight was 15100 and the reproducibility of molecular weight was favorable.

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Abstract

An object of the present invention is to provide a method for producing a resin using radical polymerization, which can obtain sufficient molecular weight reproducibility and has a small amount of residual monomers. In order to achieve the above object, the present invention provides a method for producing a resin, which includes: adding a radical polymerizable monomer and a thermal radical polymerization initiator to a reaction vessel, and making the radical polymerizable monomer more thermally free than the Polymerize at a temperature 20-70°C higher than the 10-hour half-life temperature of the polymerization initiator.

Description

technical field [0001] The present invention relates to a method for producing a resin obtained by radical polymerization. Specifically, it relates to a method for producing a resin at a specific temperature when polymerizing a radically polymerizable monomer using a thermal radical polymerization initiator. Background technique [0002] In recent years, from the viewpoint of resource saving and energy saving, photosensitive resin compositions curable by active energy rays such as ultraviolet rays and electron beams have been widely used in the fields of various coatings, printing, paints, adhesives, and the like. In addition, in the field of electronic materials such as printed wiring boards, photosensitive resin compositions curable by active energy rays are also used for solder resists, color filters, and black matrices. matrix), photo spacers, resists for protective films, etc. [0003] The use of resins obtained by radical polymerization is known in the above-mentione...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F2/00C08F20/06
CPCC08F20/06C08F2/00C08F2/44C08F220/325
Inventor 木下健宏斋藤健川口恭章柳正义仓本拓树
Owner RESONAC CORPORATION