Preparation method of thermal expansion microspheres
A heat-expandable microsphere and mixing technology, which is applied in the field of preparation of heat-expandable microspheres, can solve the problems of low operation safety, high environmental protection requirements, high toxicity and the like
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[0021] The invention provides a method for preparing heat-expandable microspheres, the heat-expandable microspheres include a thermoplastic resin shell and a foaming agent encapsulated in the shell with a boiling point not higher than the softening point of the thermoplastic resin, wherein the The method includes the following steps:
[0022] (1) Preparation of the oil phase: mixing 80-200 parts by weight of foaming agent, 100 parts by weight of polymerization combined monomer composition, 0.05-5 parts by weight of crosslinking agent and 0.01-10 parts by weight of initiator get oily phase;
[0023] (2) Preparation of the water phase: 0.001-2 parts by weight of a water-soluble composition, 100-800 parts by weight of an aqueous dispersion medium, 5-50 parts by weight of a dispersion stabilizer and 0.005-0.03 parts by weight of an alkali metal nitrite Salt inhibitors are mixed to obtain an aqueous phase;
[0024] (3) Preparation of heat-expandable microspheres: the oil phase in...
Embodiment 1
[0043] (1) Preparation of oil phase: 6g isopentane, 6g isooctane, 8g methyl methacrylate, 2.5g N, N dimethyl acrylamide, 0.2g poly(ethylene glycol) methyl methacrylate , 1g isobornyl methacrylate, 0.5g hexafluorobutyl methacrylate, 0.05g triallyl cyanurate and 0.05g azobisisobutyronitrile, mixed and stirred at 25°C for 10-15min to form a uniform the oil phase;
[0044] (2) Preparation of the water phase: 20g sodium chloride is dissolved in 100g deionized water, then the mass concentration of 20g added is 25% colloidal silicon dioxide solution, 1% polyvinylpyrrolidone aqueous solution and 0.1g dodecane Alkyl sodium sulfate, then add 1.8g of 1% sodium nitrite aqueous solution and stir evenly, then continue to add hydrochloric acid to adjust the pH to 3, and the formed solution is an aqueous phase;
[0045] (3) Homogenization of the water-oil phase: pour the above-mentioned oil phase into the above-mentioned water phase, and disperse the mixed liquid in a homogeneous mixer at 60...
Embodiment 2
[0048] (1) Preparation of oil phase: 6g isopentane, 7g isooctane, 8g methyl methacrylate, 3g N, N dimethyl acrylamide, 0.5g poly(ethylene glycol) methyl methacrylate, 1.2 1g of isobornyl methacrylate, 0.6g of hexafluorobutyl methacrylate, 0.06g of triallyl cyanurate and 0.04g of benzoyl peroxide were mixed and stirred at 25°C for 10min-15min to form a uniform oil phase ;
[0049] (2) Preparation of water phase: 20g sodium chloride is dissolved in 100g deionized water, then adding 20g mass concentration is 25% colloidal silicon dioxide solution, adding 5g 1% polyvinylpyrrolidone aqueous solution and 0.1g dodecane Alkyl sodium sulfate, then add 2g of 1% sodium nitrite aqueous solution and stir evenly, then continue to add hydrochloric acid to adjust the pH to 3, and the formed solution is an aqueous phase;
[0050] (3) Homogenization of the water-oil phase: pour the above-mentioned oil phase into the above-mentioned water phase, and disperse the mixed liquid in a homogeneous mi...
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