Heat-expandable microsphere, method for producing same and use of same
A heat-expandable microsphere and microsphere technology, applied in the preparation of microspheres, chemical instruments and methods, microcapsule preparations, etc., can solve the problems of poor gas barrier properties and solvent resistance, reduce the crystallinity of copolymer resins, etc. The effect of excellent solvent resistance and excellent heat resistance
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preparation example Construction
[0066] The substrate microspheres and their preparation steps are described below, followed by a detailed description of the surface treatment step, and finally a wetting step.
[0067] (Substrate microspheres and their preparation steps)
[0068] The substrate microspheres include 1) a thermoplastic resin shell and 2) a thermally vaporizable foaming agent encapsulated in the shell. The thermoplastic resin is prepared by polymerizing a polymerizable component substantially comprising a carboxyl group-containing monomer (ie, a polymerizable component comprising a carboxyl group-containing monomer).
[0069] In the preparation step of the base material microspheres, the polymerizable component is polymerized in an aqueous dispersion medium in which an oily mixture containing the polymerizable component and a foaming agent is dispersed.
[0070] The foaming agent is not particularly limited as long as it is a thermally vaporizable substance; and includes, for example, C 3 -C 1...
Embodiment
[0274] The heat-expandable microspheres of the present invention are specifically explained using the following examples, although the present invention is not limited within the scope of the examples. In the following Examples and Comparative Examples, "%" means "% by weight" unless otherwise specified.
[0275] Properties and performances of the substrate microspheres and heat-expandable microspheres described in the following Preparation Examples, Examples and Comparative Examples were measured and evaluated in the methods described below. Hereinafter, the substrate microspheres and heat-expandable microspheres may sometimes be referred to as "microspheres" for convenience of description.
[0276] [Measurement of average particle size and particle size distribution]
[0277] A laser diffraction particle size analyzer (HEROS & RODOS, manufactured by SYMPATEC) was used as a device for the measurement. The microspheres were analyzed in a dry system with a dry dispers...
preparation Embodiment 1
[0325] An aqueous dispersion medium was prepared by adding 150 g of sodium chloride, 70 g of colloidal silica containing 20% by weight of silica, 1.0 g of polyvinylpyrrolidone, and 0.5 g of ethylenediamine tetramine to 600 g of deionized water tetrasodium acetate, and the pH of the mixture is controlled from 2.8 to 3.2.
[0326] On the other hand, by mixing 120 g of acrylonitrile, 115 g of methacrylonitrile, 65 g of methacrylic acid, 1.0 g of 1,9-nonanediol diacrylate, 90 g of isooctane and 8 g of 50% peroxide di-sec-butyl dicarbonate solution to prepare an oily mixture.
[0327] The aqueous dispersion medium and the oily mixture are mixed, and the mixed liquid is dispersed into a suspension with a homomixer (T.K. Homo-mixer, manufactured by Tokushu Kika Kogyou). The suspension was then transferred to a pressurized reactor with a capacity of 1.5 liters and purged with nitrogen, and the polymerization was carried out at 60 degrees Celsius for 20 hours by stirring the s...
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Abstract
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