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Composite-grade polycarbosilane and preparation method thereof
The invention discloses a preparation method of composite-grade polycarbosilane. The method comprises the following steps: taking 100 parts of sodium chloride, carrying out electrolysis and oil-bath heating, carrying out purification molding, adding 113 parts of dimethyldichlorosilane into the molten metal sodium for reacting, and carrying out stirring curing at high temperature; adding 104 partsof absolute ethyl alcohol into the reactant, controlling the temperature, continuously stirring, extracting sodium chloride for recycling, and performing vacuum filtration on the reacted mixture; adding 705 parts of purified water and 222 parts of absolute ethyl alcohol into the mixture for multiple times of cleaning so as to obtain pure polydimethylsilane; performing vacuum drying on the pure polydimethylsilane obtained in the previous step; carrying out pressure maintaining, vacuumizing, heat preservation, heating and cracking on the polydimethylsilane subjected to vacuum drying to obtain aliquid low-molecular cracking product; and synthesizing and desolventizing the liquid low-molecular cracking product at high temperature and high pressure to obtain the composite-grade polycarbosilane.
本发明公开了一种复合级聚碳硅烷的制备方法，制备步骤如下：取100份氯化钠进行电解并油浴加热，经过提纯成型，后再往熔融的金属钠中加入113份二甲基二氯硅烷进行反应，高温下搅拌熟化；在反应物中加入104份无水乙醇，控制温度并持续搅拌，提取氯化钠进行重新回收利用，对反应后的混合物进行真空抽滤；在混合物中分别加入705份纯净水和222份无水乙醇进行多次清洗，以获得纯净的聚二甲基硅烷；将步纯净的聚二甲基硅烷进行真空干燥；将真空干燥后的聚二甲基硅烷进行保压、抽真空、保温、升温和裂解，即得液态低分子裂解产物；再将液态低分子裂解产物在高温高压下进行合成、脱溶，以得到复合级聚碳硅烷。
Composite-grade polycarbosilane and preparation method thereof
The invention discloses a preparation method of composite-grade polycarbosilane. The method comprises the following steps: taking 100 parts of sodium chloride, carrying out electrolysis and oil-bath heating, carrying out purification molding, adding 113 parts of dimethyldichlorosilane into the molten metal sodium for reacting, and carrying out stirring curing at high temperature; adding 104 partsof absolute ethyl alcohol into the reactant, controlling the temperature, continuously stirring, extracting sodium chloride for recycling, and performing vacuum filtration on the reacted mixture; adding 705 parts of purified water and 222 parts of absolute ethyl alcohol into the mixture for multiple times of cleaning so as to obtain pure polydimethylsilane; performing vacuum drying on the pure polydimethylsilane obtained in the previous step; carrying out pressure maintaining, vacuumizing, heat preservation, heating and cracking on the polydimethylsilane subjected to vacuum drying to obtain aliquid low-molecular cracking product; and synthesizing and desolventizing the liquid low-molecular cracking product at high temperature and high pressure to obtain the composite-grade polycarbosilane.
本发明公开了一种复合级聚碳硅烷的制备方法，制备步骤如下：取100份氯化钠进行电解并油浴加热，经过提纯成型，后再往熔融的金属钠中加入113份二甲基二氯硅烷进行反应，高温下搅拌熟化；在反应物中加入104份无水乙醇，控制温度并持续搅拌，提取氯化钠进行重新回收利用，对反应后的混合物进行真空抽滤；在混合物中分别加入705份纯净水和222份无水乙醇进行多次清洗，以获得纯净的聚二甲基硅烷；将步纯净的聚二甲基硅烷进行真空干燥；将真空干燥后的聚二甲基硅烷进行保压、抽真空、保温、升温和裂解，即得液态低分子裂解产物；再将液态低分子裂解产物在高温高压下进行合成、脱溶，以得到复合级聚碳硅烷。
Composite-grade polycarbosilane and preparation method thereof
一种复合级聚碳硅烷及其制备方法
HUANG QINGQIAN (author) / HUANG LIFENG (author) / CHEN FULAI (author) / CHEN BOLIN (author) / LIAN XIAOPING (author) / CHEN JIAHUANG (author)
2021-03-19
Patent
Electronic Resource
Chinese
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