浙江化工
浙江化工
절강화공
ZHEJIANG CHEMICAL INDUSTRY
2012年
5期
3-6
,共4页
染料中间体%硝基苯胺%溴代%绿色制备工艺
染料中間體%硝基苯胺%溴代%綠色製備工藝
염료중간체%초기분알%추대%록색제비공예
dye intermediates%nitroaniline%bromination%green technology
研究了一种利用回收的溴化物、硫酸或盐酸水溶液制备溴代硝基苯胺染料中间体的绿色制备工艺,即向回收的溴化物水溶液中加入无机酸水溶液,搅拌,加入硝基苯胺化合物,升温至35℃~55℃,搅拌30min,滴加氯酸钠或氯酸钾水溶液,滴加时间控制在2.5~3.5h,搅拌,升温至65℃~75℃,反应完成后过滤,滤饼水洗至pH=5~8,烘干得到溴代硝基苯胺染料中间体。采用该方法所得产品质量和收率高,生产成本大幅度降低,工艺简单,同时大大削减含溴化氢废气和含溴化盐废水对环境的污染.符合绿色化工要求,适合于大规模工业生产。
研究瞭一種利用迴收的溴化物、硫痠或鹽痠水溶液製備溴代硝基苯胺染料中間體的綠色製備工藝,即嚮迴收的溴化物水溶液中加入無機痠水溶液,攪拌,加入硝基苯胺化閤物,升溫至35℃~55℃,攪拌30min,滴加氯痠鈉或氯痠鉀水溶液,滴加時間控製在2.5~3.5h,攪拌,升溫至65℃~75℃,反應完成後過濾,濾餅水洗至pH=5~8,烘榦得到溴代硝基苯胺染料中間體。採用該方法所得產品質量和收率高,生產成本大幅度降低,工藝簡單,同時大大削減含溴化氫廢氣和含溴化鹽廢水對環境的汙染.符閤綠色化工要求,適閤于大規模工業生產。
연구료일충이용회수적추화물、류산혹염산수용액제비추대초기분알염료중간체적록색제비공예,즉향회수적추화물수용액중가입무궤산수용액,교반,가입초기분알화합물,승온지35℃~55℃,교반30min,적가록산납혹록산갑수용액,적가시간공제재2.5~3.5h,교반,승온지65℃~75℃,반응완성후과려,려병수세지pH=5~8,홍간득도추대초기분알염료중간체。채용해방법소득산품질량화수솔고,생산성본대폭도강저,공예간단,동시대대삭감함추화경폐기화함추화염폐수대배경적오염.부합록색화공요구,괄합우대규모공업생산。
A green bromination technology of dye intermediates was developed for preparing brominated nitroanilines via using the recycled bromide and sulfuric acid or hydrochloric acid. The inorganic acid solution and nitroaniline were dropped into the recycled bromide solution with stirring. When heated to 35 ~C- 55 ~C, the solution of sodium or potassium chlorate was dropped into the mixture, and stirred for 30 rain, the dropping time was controlled in 2.5 - 3.5 h. Then the temperature was heated to 65 ~C- 75 ~C. When the reaction was completed, the product was tittered, washed with water to pH = 5 - 8, dried to produce bromominated uitroaniline (dye intermediates). With this process, the quality and yield of product are high, decreasing the production cost by a large margin. The technology can make full use of the waste gas of hydrogen bromide and the waste water of bromide salt, which meets the green requirement of chemical industry with the large-scale industry production, and greatly eliminates the environment pollution.