Method for producing thermally expandable microspheres

A technology of heat-expandable microspheres and a manufacturing method, which can be used in the preparation of microspheres, microcapsule preparations, coatings, etc., can solve problems such as insufficient sufficiency, and achieve the effects of high solvent resistance and excellent stability over time

Active Publication Date: 2016-05-04
MATSUMOTO YUSHI SEIYAKU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in recent years, with the expansion of applications of heat-expandable microcapsules, the solvent resistance simply derived from nitrile-based monomers may not be sufficient.

Method used

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  • Method for producing thermally expandable microspheres
  • Method for producing thermally expandable microspheres
  • Method for producing thermally expandable microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0175] [Example 1; Thermally expandable microspheres]

[0176] To 600 g of ion-exchanged water, 150 g of sodium chloride, 70 g of colloidal silicon dioxide having an active ingredient of silicon dioxide of 20% by weight, 1.0 g of polyvinylpyrrolidone, and 0.5 g of tetrasodium ethylenediaminetetraacetic acid were added. The pH of the mixture was adjusted to 2.8 to 3.2 to prepare an aqueous dispersion medium.

[0177] In addition, 65 g of acrylonitrile, 30 g of methacrylonitrile, 5 g of methyl methacrylate, 0.3 g of trimethylolpropane trimethacrylate, 20 g of isopentane, and 1,1 - Di(tert-hexylperoxy)cyclohexane containing liquid 2.4g (active ingredient amount 2.0g) was mixed to prepare an oily mixture.

[0178] The aqueous dispersion medium and the oily mixture were mixed, and the obtained mixed solution was dispersed with a homomixer (manufactured by Primix Corporation) to prepare a suspension. This suspension was transferred to a pressurized reactor with a capacity ...

Embodiment 2～5 and comparative example 1～2

[0180] Except for changing the various components constituting the oily mixture used in Example 1, their amounts, and the polymerization temperature to those shown in Table 1, heat-expandable microspheres B to E were obtained in the same manner. Then, the solvent resistance and the residual monomer ratio were evaluated, and are shown in Table 1.

[0181] Furthermore, in Example 5, first, polymerization was carried out at 60°C for 10 hours (first stage), then the temperature was raised to 80°C in 30 minutes (second stage), and finally, polymerization was carried out at 80°C for 5 hours (third stage). ), under such reaction conditions, thermally expandable microspheres E are obtained.

[0182] [Table 1]

[0183]

[0184] *1 The first stage: 60°C x 10 hours, the second stage: heating from 60°C to 80°C in 30 minutes, the third stage: 80°C x 5 hours

[0185] In Table 1, monomer components, initiators, and crosslinking agents are represented by the following abbrev...

Embodiment A1

[0195] [Embodiment A1; Polyurethane coating film]

[0196] With the heat-expandable microsphere B of 10g and the polyurethane binder of 90g (polyurethane solid content 21%, mixed organic solvent 79%, the weight ratio of mixed organic solvent is methyl ethyl ketone / toluene / acetone / N, N-dimethylformamide =40 / 20 / 10 / 30) were mixed to prepare a polyurethane coating composition.

[0197] This polyurethane coating composition was coated on the base fabric with a coater so that the thickness of the coating film after drying would be 0.3 mm. Then, when the coating film thickness (T2) after drying at room temperature was measured with the film thickness meter, it was 0.3 mm. Then, it heat-processed for 2 minutes using the gear type oven previously heated to 180 degreeC, and obtained the polyurethane coating film which expanded.

[0198] When the thickness (T1) of this expanded polyurethane coating film was measured in the same manner as above, it was 1.8 mm. The expansion rat...

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Abstract

Provided is a method for producing thermally expandable microspheres having high solvent resistance with high efficiency. The method for producing thermally expandable microspheres is a method for producing thermally expandable microspheres each of which is composed of a shell part comprising a thermoplastic resin and a foaming agent included in the shell part and capable of being evaporated by heating. The method comprises the steps of: preparing an aqueous suspension in which an oily mixture is dispersed in an aqueous dispersion medium, wherein the oily mixture comprises a polymerizable component, the foaming agent and a polymerization initiator that is essentially composed of a peroxide (A) having an ideal active oxygen content of 7.8% or more; and polymerizing the polymerizable component in the oily mixture.

Description

technical field [0001] The invention relates to a method for manufacturing heat-expandable microspheres. Background technique [0002] Heat-expandable microspheres having a structure in which a thermoplastic resin is used as an outer shell and a blowing agent is sealed inside are generally called heat-expandable microcapsules. Vinylidene chloride, (meth)acrylonitrile-based monomers, (meth)acrylate-based monomers, and the like are generally used as raw material monomers for thermoplastic resins. Moreover, hydrocarbons, such as isobutane and isopentane, are mainly used as a foaming agent (refer patent document 1). [0003] As heat-expandable microcapsules having high solvent resistance, heat-expandable microcapsules obtained by polymerizing a nitrile-based monomer at a high proportion of 80% by weight or more are known (see Patent Document 2). However, in recent years, with the expansion of applications of heat-expandable microcapsules, the solvent resistance simply derived ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/32C09D7/65
CPCB01J13/185C08J9/0061C08J9/32C08J2323/06C08J2327/06C08J2375/04C08J2423/08C09D5/00C08K7/22C09D7/70C09D7/65C08J9/20C08J9/228C08K5/14C08J2203/22C08J2333/18C08J9/236C08J2300/22
Inventor 阪部晃一三木胜志野村贯通
Owner MATSUMOTO YUSHI SEIYAKU
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