Graft copolymer, method for producing same and resin composition containing such graft copolymer
A technology of graft copolymer and resin composition, which is applied in the field of polyorganosiloxane graft copolymers, and can solve the problems that the physical properties cannot be fully expressed, the dispersion state of polyorganosiloxane components deteriorates, etc.
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[0168] Hereinafter, although the Example which showed this invention more concretely is demonstrated, this invention is not limited to these. In addition, the following measurement and test were performed as follows.
[0169] [polymerization conversion rate]
[0170] Take and accurately weigh a part of the obtained latex, and accurately weigh the solid content after drying in a hot air drier at 130° C. for 1 hour to obtain the solid content ratio in the latex. Ratio - total weight of raw materials other than monomers) / weight of added monomers × 100 (%) to calculate. In addition, chain transfer agents are treated as added monomers.
[0171] [Volume average particle size]
[0172] The volume average particle diameters of the seed polymer, polyorganosiloxane particles, and graft copolymers were measured in the latex state. The volume average particle diameter (µm) was measured using MICROTRAC UPA150 manufactured by Nikkiso Co., Ltd. as a measuring device.
[0173] [grafting ...
manufacture example 1
[0191] (Manufacture example 1) Manufacture of polybutylacrylate seed polymer (SD-1)
[0192] 400 parts by weight of water and 12 parts by weight (solid content) of a 15% by weight sodium dodecylbenzenesulfonate aqueous solution were mixed in a 5-neck flask equipped with a stirrer, a reflux cooler, a nitrogen blowing port, a monomer addition port, and a thermometer. (manufactured by Kao Corporation, Neopelex G15), the temperature was raised to 50°C, and after the liquid temperature reached 50°C, nitrogen substitution was performed. Then 10 parts by weight of butyl acrylate and 3 parts by weight of tert-dodecyl mercaptan were added. After 30 minutes, add 0.01 parts by weight (solid content) of Alkane hydroperoxide, 0.3 parts by weight of sodium formaldehyde sulfoxylate (SFS), 0.01 parts by weight of disodium ethylenediamine tetraacetate (EDTA), 0.0025 parts by weight of ferrous sulfate (FeSO 4 ·7H 2 O), stirred for 1 hour.
[0193] After 3 hours, 90 parts by weight of butyl...
manufacture example 2、3
[0194] (Production examples 2 and 3) Production of polyorganosiloxane particles (S-1 and 2)
[0195] With the composition shown in Table 1, a high-speed homomixer was used to stir at 7500 rpm for 5 minutes to prepare a silicone emulsion. In addition, the seed polymer (SD-1) latex corresponding to the solid content of the amount shown in Table 1 was put into a 5-necked flask equipped with a stirrer, a reflux cooler, a nitrogen blowing port, a monomer addition port, and a thermometer. The previous silicone emulsion was added to the flask in one portion. Under nitrogen flow, while stirring the system, the temperature was raised from 35° C. to 80° C. over 1 hour, and then 1 part by weight (solid content) of 10% by weight dodecylbenzenesulfonic acid (DBSA, manufactured by Kao Corporation, trade name: Neoperex GS) aqueous solution. After reacting for 15 hours, it was cooled to 25° C., and after standing for 20 hours, the pH of the system was adjusted to 6.5 with 3% by weight of so...
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Abstract
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