Method for manufacturing reactive polysiloxane solution
A polysiloxane solution and a technology for a manufacturing method are applied in the field of manufacturing reactive polysiloxane solutions, can solve problems such as different characteristics, and achieve the effects of less cost and time, and excellent storage stability
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[0118] The present invention will be specifically described by way of examples below. However, the present invention is not limited in any way by this Example.
[0119]It should be noted that Mn (number average molecular weight) was determined by gel permeation chromatography (GPC) using THF as the eluent at 40°C using GPC columns "TSK-GelG4000H" and "TSK-Gel G2000H" (model name, manufactured by Tosoh Corporation), and the molecular weight was calculated from the retention time using standard polystyrene.
[0120] Furthermore, the obtained reactive polysiloxane 1 In the H-NMR analysis, about 1 g of the measurement sample and about 100 mg of hexamethyldisiloxane (hereinafter referred to as "HMDSO") as an internal standard substance were accurately weighed, dissolved in deuterated chloroform as an analysis solvent, and The proton signal intensity of HMDSO was analyzed as a benchmark.
[0121] Table 1 shows the physical properties of the organic solvents for water washing used...
reference example 1
[0127] In order to exchange a part of the methoxy group of tetramethoxysilane (TMOS) with 1-propoxy group, put 43.39 g of 1-propanol and 38.06 g (250 mmol) of tetramethoxysilane into a beaker, and While stirring, 12.76 g of a 25% by mass methanol solution of tetramethylammonium hydroxide (299 mmol of methanol, 35 mmol of tetramethylammonium hydroxide) was gradually added, and the reaction was carried out for at least 15 minutes at a liquid temperature of 25°C. After 15 minutes, gas chromatography analysis (FID detector) was carried out on the reaction solution, and as a result, tetraalkoxysilane containing n-propoxy group was detected, that is, a compound in which the methoxy group of TMOS was replaced by n-propoxy group (1 substitution body, 2 substitution body, 3 substitution body and 4 substitution body) and unreacted TMOS. Based on the peak area of the product in gas chromatography, the substitution number of 1-propanol (the average number of n-propoxyl groups per molecu...
Embodiment 1
[0129] Put 0.003 g of N-nitrosophenylhydroxylamine aluminum salt (trade name "Q-1301", manufactured by Wako Pure Chemical Industries, Ltd.) as a polymerization inhibitor in a beaker, and add 3-methanol as a T monomer 62.09 g (250 mmol) of acryloyloxypropyltrimethoxysilane was added, and 75.13 g of 1-propanol and 31.53 g of water were further added. The liquid temperature was set at 60°C, and 94.21 g of the tetramethylammonium hydroxide-containing TMOS alcohol exchange liquid prepared in Reference Example 1 was added dropwise over 1 hour while stirring. Then, stirring was continued at 60° C., and the reaction was terminated after 2 hours. It should be noted that the alcohol exchange solution of TMOS was dripped at a constant speed as much as possible using a liquid delivery pump.
[0130] Next, with the temperature of the reaction liquid at 60°C, 8.27 g of a 20% by mass methyl ethyl ketone (MEK) solution of oxalic acid (18.38 mmol of oxalic acid) was added, and tetramethylammo...
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