水相清洁合成硬脂酸钙的研究及其产业化
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摘要
本文以硬脂酸和氢氧化钙为原料,双氧水和乙醇为复合催化剂,实现了在水介质中绿色清洁合成硬脂酸钙.考察了双氧水用量、乙醇用量、反应温度、固液比和反应时间等因素对反应的影响.结果表明,在双氧水用量24%、乙醇用量10%、反应温度60℃、固液比1∶15、反应时间3 h的优化条件下,产品的游离酸含量为0.28%.生产后的滤液可进行重复使用,避免了废水的排放.工业放大实验结果表明,此方法可沿用现有复分解法设备进行工业化生产.
In this paper,calcium stearate was environmentally synthesized from stearic acid and calcium hydroxide using hydrogen peroxide and ethanol as composite catalyst in aqueous media. Effects of hydrogen peroxide dosage,ethanol dosage,temperature,solid-liquid ratio and time on the reaction were investigated. The results showed that free acid of product was 0. 28% under the optimal conditions of 24% hydrogen peroxide,10% ethanol and solid-liquid ratio 1: 15 at 60 oC within 3 h. This route realized sewage zero emissions since the filtrate can be reused. According to the results of industrial scale-up,calcium stearate could be industrially prepared by this method using the original production equipment in the double decomposition.
In this paper,calcium stearate was environmentally synthesized from stearic acid and calcium hydroxide using hydrogen peroxide and ethanol as composite catalyst in aqueous media. Effects of hydrogen peroxide dosage,ethanol dosage,temperature,solid-liquid ratio and time on the reaction were investigated. The results showed that free acid of product was 0. 28% under the optimal conditions of 24% hydrogen peroxide,10% ethanol and solid-liquid ratio 1: 15 at 60 oC within 3 h. This route realized sewage zero emissions since the filtrate can be reused. According to the results of industrial scale-up,calcium stearate could be industrially prepared by this method using the original production equipment in the double decomposition.
引文
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[13]巫书刚,姜莉,肖锦平,等.水相清洁法合成硬脂酸钙工业化的研究[J].精细化工原料及中间体,2011,(09):3-6.
[14]吴茂英,陈妍.在水介质中直接制备硬脂酸钙[J].日用化学工业,2003,33(05):292-294.
[15]胡国华.硬脂酸钙一步法合成的工业化生产应用[J].广州化工,2013,41(09):199-201.
[16]郭立新,黄福星,谢斌,等.直接法工艺合成硬脂酸钙的研究及工业化生产[J].化工文摘,2006,(03):37-38.
[17]周泽广,周烈,黄在银.合成硬脂酸钙新工艺研究[J].日用化学工业,2005,35(05):331-333.
[2]沈刚,刘静敏.直接法合成硬脂酸盐工艺[J].辽宁化工,2009,38(12):850-851.
[3]冒圣华,周松涛,冒莹莹.一种硬脂酸钙的生产方法:中国,201210402005[P].2013-01-16.
[4]白浩,张安平,芮光超,等.一种硬脂酸盐的制作方法:中国,201010607259[P].2012-07-11.
[5]刘庆丰,严海彪,陈艳林.利用正交设计研究水热法合成硬脂酸钙[J].塑料助剂,2005,(05):27-29.
[6]吴茂英,陈妍.水介质直接法清洁合成金属皂的研究[J].塑料工业,2003,31(02):48-50.
[7]方银军,葛赞,史立文,等.一种低温干法连续化生产硬脂酸盐的工艺及装置:中国,201210421975[P].2013-02-13.
[8]周小群,阮文响.固相法生产硬脂酸盐的生产工艺及其生产系统:中国,201410173957[P].2014-07-16.
[9]鲍兴来,周松涛,周维宏.一种硬脂酸钙熔融法生产工艺及其硬脂酸钙反应釜:中国,201010246772[P].2012-02-08.
[10]李兰生,李翔元,夏长富,等.无排放一步合成法生产硬脂酸钙的方法:中国,200610109221[P].2008-02-06.
[11]冒圣华,冒莹莹.一种硬脂酸一步合成制备硬脂酸钙的方法:中国,200810022819[P].2009-01-28.
[12]郭立新,黄福星,谢斌,等.直接法工艺合成硬脂酸钙的工业化研究[J].塑料助剂,2006,(05):29-31.
[13]巫书刚,姜莉,肖锦平,等.水相清洁法合成硬脂酸钙工业化的研究[J].精细化工原料及中间体,2011,(09):3-6.
[14]吴茂英,陈妍.在水介质中直接制备硬脂酸钙[J].日用化学工业,2003,33(05):292-294.
[15]胡国华.硬脂酸钙一步法合成的工业化生产应用[J].广州化工,2013,41(09):199-201.
[16]郭立新,黄福星,谢斌,等.直接法工艺合成硬脂酸钙的研究及工业化生产[J].化工文摘,2006,(03):37-38.
[17]周泽广,周烈,黄在银.合成硬脂酸钙新工艺研究[J].日用化学工业,2005,35(05):331-333.