CN109369439B - 一种n-酰基氨基酸型表面活性剂的制备方法 - Google Patents
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Abstract
本发明涉及一种N‑酰基氨基酸型表面活性剂的制备方法,将0.11‑0.35g铜钨酸加入到50mL去离子水中,搅拌溶解,制得铜钨酸溶液,然后加入载体,超声浸渍12‑24小时,然后将所得固体依次进行干燥、焙烧,得到铜钨酸负载量为5‑15wt%的催化剂;将摩尔比为0.8~1.0:1的烷基胺脂肪酸盐和烷基酸加入到反应容器中,然后加入上述催化剂进行反应,反应结束后,过滤除去催化剂,将反应得到的溶液用去离子水进行萃取,收集上层液,即得。制备方法反应温度低,反应时间短,能耗低,收率高,制得的N‑酰基氨基酸型表面活性剂纯度高。
Description
技术领域
本发明涉及一种氨基酸型表面活性剂的制备方法,尤其是一种N-酰基氨基酸型表面活性剂的制备方法。
背景技术
表面活性剂可起洗涤、乳化、发泡、湿润、浸透和分散等多种作用,随着生活水平的不断提高,人们的环保意识、对自身健康的保护意识越来越强。LAS、AES、K12等传统的表面活性剂在生产和使用过程中,会产生硅油、二恶烷、致癌物质、生活污水的排放,且难生物降解,造成严重的环境污染问题。出于对环境保护和生物安全性的需要,开发和使用环境友好的表面活性剂日益受到世界各国的重视。
N-酰基氨基酸类表面活性剂是一种温和的且可降解的阴离子表面活性剂,其PH值与人体肌肤接近,温和无刺激、无毒无残留、易生物降解,是一种环境友好的表面活性剂,其具有良好的去污、发泡、乳化功能,对硬水稳定,生物降解性比烷基磺酸盐好。可用于人体清洁用品、洗涤剂、化妆品等。
N-酰基氨基酸类表面活性剂一般是通过氨基酸和脂肪酸发生直接脱水缩合反应制得,反应温度高(170-190℃),能耗大,且产品产率较低(约80%)。
发明内容
本发明的目的是解决现有技术的不足,提供提供一种制备高收率、高纯度的N-酰基氨基酸型表面活性剂的方法,该制备方法反应温度低,反应时间短,能耗低。
技术方案
一种N-酰基氨基酸型表面活性剂的制备方法,包括如下步骤:
(1)将0.11-0.35g铜钨酸加入到50mL去离子水中,搅拌溶解,制得铜钨酸溶液,然后加入载体,超声浸渍12-24小时,然后将所得固体依次进行干燥、焙烧,制得铜钨酸负载量为5-15wt%的催化剂;
(2)将摩尔比为0.8~1.0:1的烷基胺脂肪酸盐和烷基酸加入到反应容器中,然后加入步骤(1)制得的催化剂进行反应,反应结束后,过滤除去催化剂,将反应得到的溶液用去离子水进行萃取,收集上层液,即得。
进一步,步骤(1)中,所述载体选自MCM-41、ZSM-5、γ-Al2O3或SAPO分子筛中的任意一种。
进一步,步骤(1)中,所述干燥温度为100-120℃,时间为12-24小时。
进一步,步骤(1)中,所述焙烧温度为300-450℃,时间为3-5小时。
进一步,步骤(2)中,所述烷基胺脂肪酸盐选自N-甲基十二烷基酸钠、N-甲基十二烷基酸钾、N-乙基十二烷基酸钠、N-乙基十二烷基酸钾、N-丙基十烷基酸钠、N-丙基十烷基酸钾、N-壬烷基十一烷基酸钠或N-壬烷基十一烷基酸钾中任意一种。
进一步,步骤(2)中,所述烷基酸选自月桂酸、乙酸、十一烷基脂肪酸或辛烷基脂肪酸中任意一种。
进一步,步骤(2)中,反应温度为50~80℃,时间为3~6小时。
进一步,步骤(2)中,所述催化剂的用量为烷基胺脂肪酸盐和烷基酸总量的0.5~5.0wt%。
进一步,步骤(2)中,所述萃取次数为5-10。
反应方程式如下:
其中,R1和R3为C1~C11的直链烷基,R2为C1~C5的直链烷基。
本发明的有益效果:本发明提供了一种N-酰基氨基酸型表面活性剂的制备方法,该制备方法反应温度低,反应时间短,能耗低,收率高,制得的N-酰基氨基酸型表面活性剂纯度高。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
实施例1
一种N-酰基氨基酸型表面活性剂的制备方法,包括如下步骤:
(1)将0.11g铜钨酸(H6CuW2O10)加入到50mL去离子水中,搅拌溶解,制得铜钨酸溶液,然后加入2g的MCM-41载体,超声浸渍12小时,然后将所得固体依次进行干燥(120℃下干燥12小时)、焙烧(300℃下焙烧3小时),得到铜钨酸负载量为5wt%的H6CuW2O10/MCM-41催化剂;
(2)将摩尔比为0.8:1的N-甲基十二烷基酸钠和月桂酸加入到反应容器中,然后加入原料量0.5wt%的步骤(1)制得的催化剂进行反应,反应温度50℃,反应时间3小时,反应结束后,过滤除去催化剂,将反应得到的溶液用与溶液体积比为0.5:1去离子水进行10次萃取,收集上层液,得到纯度为98.5%,收率为95.3%的N-酰基氨基酸型表面活性剂。
实施例2
一种N-酰基氨基酸型表面活性剂的制备方法,包括如下步骤:
(1)将0.35g铜钨酸(H6CuW2O10)加入到50mL去离子水中,搅拌溶解,制得铜钨酸溶液,然后加入2g的ZSM-5载体,超声浸渍24小时,然后将所得固体依次进行干燥(120℃下干燥12小时)、焙烧(450℃下焙烧3小时),得到铜钨酸负载量为15wt%的H6CuW2O10/ZSM-5催化剂;
(2)将摩尔比为1.0:1的N-乙基十二烷基酸钠和乙酸加入到反应容器中,然后加入原料量1.5wt%的步骤(1)制得的催化剂进行反应,反应温度80℃,反应时间6小时,反应结束后,过滤除去催化剂,将反应得到的溶液用与溶液体积比为0.3:1的去离子水进行10次萃取,收集上层液,得到纯度为98.8%,收率为97.5%的N-酰基氨基酸型表面活性剂。
实施例3
一种N-酰基氨基酸型表面活性剂的制备方法,包括如下步骤:
(1)将0.35g铜钨酸(H6CuW2O10)加入到50mL去离子水中,搅拌溶解,制得铜钨酸溶液,然后加入2g的ZSM-5载体,超声浸渍24小时,然后将所得固体依次进行干燥(120℃下干燥12小时)、焙烧(450℃下焙烧3小时),得到铜钨酸负载量为15wt%的H6CuW2O10/ZSM-5催化剂;
(2)将摩尔比为0.9:1的N-丙基十烷基酸钠和十一烷基脂肪酸加入到反应容器中,然后加入原料量1.5wt%的步骤(1)制得的催化剂进行反应,反应温度80℃,反应时间6小时,反应结束后,过滤除去催化剂,将反应得到的溶液用与溶液体积比为0.4:1的去离子水进行8次萃取,收集上层液,得到纯度为99.1%,收率为92.6%的N-酰基氨基酸型表面活性剂。
实施例4
一种N-酰基氨基酸型表面活性剂的制备方法,包括如下步骤:
(1)将0.28g铜钨酸(H6CuW2O10)加入到50mL去离子水中,搅拌溶解,制得铜钨酸溶液,然后加入2g的SAPO载体,超声浸渍24小时,然后将所得固体依次进行干燥(120℃下干燥12小时)、焙烧(300℃下焙烧3小时),得到铜钨酸负载量为12.3wt%的H6CuW2O10/SAPO催化剂;
(2)将摩尔比为1.0:1的N-壬烷基十一烷基酸钠和辛烷基脂肪酸加入到反应容器中,然后加入原料量3.0wt%的步骤(1)制得的催化剂进行反应,反应温度70℃,反应时间5小时,反应结束后,过滤除去催化剂,将反应得到的溶液用与溶液体积比为0.5:1的去离子水进行10次萃取,收集上层液,得到纯度为99.0%,收率为93.8%的N-酰基氨基酸型表面活性剂。
实施例5
一种N-酰基氨基酸型表面活性剂的制备方法,包括如下步骤:
(1)将0.35g铜钨酸(H6CuW2O10)加入到50mL去离子水中,搅拌溶解,制得铜钨酸溶液,然后加入2g的γ-Al2O3载体,超声浸渍24小时,然后将所得固体依次进行干燥(120℃下干燥12小时)、焙烧(450℃下焙烧3小时),得到铜钨酸负载量为15wt%的H6CuW2O10/γ-Al2O3催化剂;
(2)将摩尔比为1.0:1的N-壬烷基十一烷基酸钠和辛烷基脂肪酸加入到反应容器中,然后加入原料量5.0wt%的步骤(1)制得的催化剂进行反应,反应温度80℃,反应时间3小时,反应结束后,过滤除去催化剂,将反应得到的溶液用与溶液体积比为0.5:1的去离子水进行10次萃取,收集上层液,得到纯度为98.5%,收率为95.3%的N-酰基氨基酸型表面活性剂。
实施例6
一种N-酰基氨基酸型表面活性剂的制备方法,包括如下步骤:
(1)将0.35g铜钨酸(H6CuW2O10)加入到50mL去离子水中,搅拌溶解,制得铜钨酸溶液,然后加入2g的ZSM-5载体,超声浸渍24小时,然后将所得固体依次进行干燥(120℃下干燥12小时)、焙烧(450℃下焙烧3小时),得到铜钨酸负载量为15wt%的H6CuW2O10/ZSM-5催化剂;
(2)将摩尔比为1.0:1的N-甲基十二烷基酸钠和月桂酸加入到反应容器中,然后加入原料量5.0wt%的步骤(1)制得的催化剂进行反应,反应温度80℃,反应时间6小时,反应结束后,过滤除去催化剂,将反应得到的溶液用与溶液体积比为0.5:1的去离子水进行10次萃取,收集上层液,得到纯度为99.5%,收率为97.1%的N-酰基氨基酸型表面活性剂。
Claims (7)
1.一种N-酰基氨基酸型表面活性剂的制备方法,其特征在于,包括如下步骤:
(1)将0.11-0.35g铜钨酸加入到50mL去离子水中,搅拌溶解,制得铜钨酸溶液,然后加入载体,超声浸渍12-24小时,然后将所得固体依次进行干燥、焙烧,得到铜钨酸负载量为5-15wt%的催化剂;
(2)将摩尔比为0.8~1.0:1的烷基胺脂肪酸盐和烷基酸加入到反应容器中,然后加入步骤(1)制得的催化剂进行反应,反应结束后,过滤除去催化剂,将反应得到的溶液用去离子水进行萃取,收集上层液,即得;
步骤(2)中,所述烷基胺脂肪酸盐选自N-甲基十二烷基酸钠、N-甲基十二烷基酸钾、N-乙基十二烷基酸钠、N-乙基十二烷基酸钾、N-丙基十烷基酸钠、N-丙基十烷基酸钾、N-壬烷基十一烷基酸钠或N-壬烷基十一烷基酸钾中任意一种;
步骤(2)中,所述烷基酸选自月桂酸、乙酸、十一烷基脂肪酸或辛烷基脂肪酸中任意一种。
2.如权利要求1所述N-酰基氨基酸型表面活性剂的制备方法,其特征在于,步骤(1)中,所述载体选自MCM-41、ZSM-5、γ-Al2O3或SAPO分子筛中的任意一种。
3.如权利要求1所述N-酰基氨基酸型表面活性剂的制备方法,其特征在于,步骤(1)中,所述干燥温度为100-120℃,时间为12-24小时。
4.如权利要求1所述N-酰基氨基酸型表面活性剂的制备方法,其特征在于,步骤(1)中,所述焙烧温度为300-450℃,时间为3-5小时。
5.如权利要求1所述N-酰基氨基酸型表面活性剂的制备方法,其特征在于,步骤(2)中,反应温度为50~80℃,时间为3~6小时。
6.如权利要求1所述N-酰基氨基酸型表面活性剂的制备方法,其特征在于,步骤(2)中,所述催化剂的用量为烷基胺脂肪酸盐和烷基酸总量的0.5~5.0wt%。
7.如权利要求1至6任一项所述N-酰基氨基酸型表面活性剂的制备方法,其特征在于,步骤(2)中,所述萃取次数为5-10。
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