Process for production of dispersion, dispersion, coating material, coating film, and film

A manufacturing method and dispersion technology, applied in chemical instruments and methods, coatings, thin material treatment, etc., can solve the problems of easy whitening of the coating film, poor fusion, hardness and other coating film properties that cannot meet the required level, and achieve Thickening suppression, stable gelation, and good productivity

Active Publication Date: 2013-06-05
DIC CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has the following problems: since the resin component and the inorganic fine particles are difficult to fuse, the properties such as hardness and transparency of the coating film cannot reach the required level, the coating film is phase-separated and easily whitened, and the storage stability is insufficient. Generation of aggregates, etc. in the resin composition
However, the method of using such a paint mixer has the following problems: the pulverization of alumina fine particles and the dispersion into the resin cannot be sufficiently performed, and the fusion of dipentaerythritol hexaacrylate and alumina fine particles added after dispersion is poor, and coatings such as hardness are poor. The performance of the film cannot reach the required level, and the coating film is prone to whitening due to phase separation, etc.

Method used

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  • Process for production of dispersion, dispersion, coating material, coating film, and film
  • Process for production of dispersion, dispersion, coating material, coating film, and film
  • Process for production of dispersion, dispersion, coating material, coating film, and film

Examples

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Embodiment

[0247] Examples and comparative examples are given below to describe the present invention more specifically. As long as there is no special record, the parts and % in the examples are mass standards.

[0248] In addition, in the Example of this invention, weight average molecular weight (Mw) and number average molecular weight (Mn) are the values ​​measured using gel permeation chromatography (GPC) under the following conditions.

[0249] Measuring device: HLC-8220 manufactured by Tosoh Corporation

[0250] Column: Guard column H manufactured by Tosoh Corporation XL -H

[0251] +TSKgel G5000H manufactured by Tosoh Corporation XL

[0252] +TSKgel G4000H manufactured by Tosoh Corporation XL

[0253] +TSKgel G3000H manufactured by Tosoh Corporation XL

[0254] +TSKgel G2000H manufactured by Tosoh Corporation XL

[0255] Detector: RI (Differential Refractometer)

[0256] Data processing: SC-8010 manufactured by Tosoh Corporation

[0257] Determination conditions: column...

Synthetic example 1（

[0262] Synthesis Example 1 (Synthesis of Acryloyl Acrylate A1)

[0263] In a reaction device equipped with a stirring device, a condenser, a dropping funnel, and a nitrogen gas introduction pipe, 500 parts by mass of methyl isobutyl ketone was charged, and the temperature in the system was raised to 110° C. while stirring, and then, it was used for 2 hours from The dropping funnel was dripped with 250 parts by mass of glycidyl methacrylate, 80 parts by mass of methyl methacrylate, 40 parts by mass of ethyl acrylate and tert-butyl peroxy-2-ethylhexanoate (Nippon Emulsifier Co., Ltd. "Perbutyl O") 5.5 parts by mass of the mixed solution, and then kept at 110°C for 15 hours. Next, the temperature was lowered to 90°C, and after loading 5 parts by mass of p-methoxyphenol and 130 parts by mass of acrylic acid, 2.6 parts by mass of triphenylphosphine was added, and the temperature was further raised to 100°C and kept for 8 hours to obtain acrylic acid acryloyl 997 parts by mass of m...

Synthetic example 2（

[0264] Synthesis Example 2 (Synthesis of Acryloyl Acrylate A2)

[0265] In a reaction device equipped with a stirring device, a condenser, a dropping funnel, and a nitrogen gas introduction pipe, 500 parts by mass of methyl isobutyl ketone was charged, and the temperature in the system was raised to 110° C. while stirring, and then, it was used for 2 hours from The dropping funnel was dripped with 180 parts by mass of glycidyl methacrylate, 230 parts by mass of methyl methacrylate, 10 parts by mass of n-butyl methacrylate and tert-butyl peroxy-2-ethylhexanoate (Nippon Emulsification Co., Ltd. "Perbutyl O") 17.2 parts by mass of the liquid mixture was then kept at 110° C. for 15 hours. Next, the temperature was lowered to 90°C, and after loading 5 parts by mass of p-methoxyphenol and 80 parts by mass of acrylic acid, 2.6 parts by mass of triphenylphosphine was added, and the temperature was further raised to 100°C and kept for 8 hours to obtain acrylic acid acryloyl 997 parts ...

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Abstract

Provided are: a process for producing a dispersion, whereby it becomes possible to perform the milling and dispersion of inorganic microparticles steadily and with good productivity while preventing the increase in viscosity or the occurrence of gelatinization of the dispersion; a dispersion which can provide a cured coating film having both high hardness and high transparency; a coating material prepared using the dispersion; a coating film; and a film produced by forming the coating film. The process is characterized in that a slurry containing an active-energy-curable compound (A), an active-energy-curable compound (B) and inorganic microparticles (C) as the essential components is introduced into a wet ball mill to mill and disperse the inorganic microparticles (C) in the slurry, wherein the wet ball mill comprises a vessel (p) in which a medium is filled, a rotating shaft (q), an impeller (r), a slurry inlet (s), a slurry outlet (t) and a shaft seal unit (u).

Description

technical field [0001] The present invention relates to a method for safely and stably producing a dispersion of inorganic fine particles in an active energy ray-curable compound, a dispersion obtained by the production method, a coating containing the dispersion, a coating film formed from the coating, and a coating having the coating. film layer of film. Background technique [0002] Inorganic microparticle-dispersed active energy ray-curable resin composition obtained by dispersing inorganic microparticles in the resin composition is attracting attention as a new material that can exhibit various properties such as improving the hardness of the coating film, adjusting the refractive index, and imparting electrical conductivity. . On the other hand, having such advantages, a coating film formed of an inorganic fine particle-dispersed resin composition has a disadvantage of inferior transparency compared to a coating film formed of an organic single-type resin composition....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F290/00B01F7/16C08F2/44C08J7/04C09D4/02C09D7/12C09D133/00C09D201/02C09D7/61C09D7/80
CPCB01F5/104B01F7/16G02B1/10B01F3/1221B02C23/18C08F2/44C09D133/08B02C17/16C09D133/068C09D7/1258C09D7/14C09D7/1216C09D5/028B01F13/1047G02B1/08B01F2013/1086B82Y40/00C09D4/00C08F265/06C09D151/003C09D7/61C09D7/66C09D7/80Y10T428/31935Y10T428/31891C08F220/325C08F222/106C08F220/1802B01F23/53B01F25/52B01F27/80B01F33/831B01F33/83613C08J3/02C08J7/04C08F220/26C08J2301/08C08F220/18
Inventor 杉山将志渡边泰之谷本洋一渡边英树大户清市水口良大渊宽之
Owner DIC CORP
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