三(羟甲基)硝基甲烷的合成工艺研究摘 要：到目前为止，国内外生产三(羟甲基)硝基甲烷(TN)的工艺条件还不够好，存在杂质多、生产时间长、产量低、副反应、质量不稳定等问题。本文对三(羟甲基)硝基甲烷(TN)的生产工艺条件进行优化，使用甲醛溶液滴入到硝基甲烷溶液中的方法，把氢氧化钙做为催化剂。综合考察了亲核加成反应的反应时间、物料比、反应温度、催化剂、pH 值等五个因素对产率的影响。得到最新的工艺条件：反应原料滴加顺序为甲醛滴入硝基甲烷中，甲醛溶液与硝基甲烷溶液物质的量之比为3.2：1、溶剂为水、反应时间 5 小时、反应催化剂为氢氧化钙、反应温度 40℃、用硫酸除去钙离子、产率高达 89.1 %。关键词：三(羟甲基)硝基甲烷；合成；工艺条件；亲核加成Study on synthesis technology of trimethylolnitromethaneAbstract: Up to now, the process conditions for the production of trimethylolnitromethane (TN) at home and abroad are not good enough. There are many problems such as many impurities, long production time, low yield, side reactions and unstable quality. In this paper, the production conditions of trimethylolnitromethane (TN) were optimized. The method of dropping formaldehyde solution into nitromethane solution was used. Calcium hydroxide was used as the catalyst. The effects of reaction time, material ratio, reaction temperature, catalyst and pH value on yield were investigated. Get the newest technological conditions: reaction raw material add order for formaldehyde drops into the nitromethane, molar ratio of formaldehyde solution and nitromethane solution ratio of 3.2:1, the solvent is water, the reaction time 5 hours, reaction of calcium hydroxide catalyst, reaction temperature 40 ℃, with sulfuric acid to remove calcium and production rate as high as 89.1 %.Keywords:Trimethylolnitromethane; Synthesis; Process conditions; Nucleophilic addition目 录1 引言...........................................................................................
