CN112430317B - 一种表面活性剂的制备方法 - Google Patents

一种表面活性剂的制备方法 Download PDF

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CN112430317B
CN112430317B CN202011329069.0A CN202011329069A CN112430317B CN 112430317 B CN112430317 B CN 112430317B CN 202011329069 A CN202011329069 A CN 202011329069A CN 112430317 B CN112430317 B CN 112430317B
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潘龙
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Dalian Daping Oil Chemistry Co ltd
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Abstract

本发明涉及一种表面活性剂的制备方法，属于有机合成技术领域。本发明所述制备方法如下：在本发明制备的催化剂的存在下，以环氧乙烷、脂肪酸为原料，反应得到脂肪酸聚氧乙烯酯表面活性剂。本发明所述方法制备的脂肪酸聚氧乙烯酯表面活性剂收率高、杂质少。

Description

一种表面活性剂的制备方法
技术领域
本发明涉及一种表面活性剂的制备方法，属于有机合成技术领域。
背景技术
脂肪酸聚氧乙烯酯属于非离子表面活性剂，具有良好的乳化、增溶、润湿、分散、柔软及抗静电等表面活性，且无毒、无刺激性，因此，在化妆品、医药、食品、农药、造纸及纺织加工等行业中有着极为广泛的应用。例如，作为洗发水和染发剂的增稠剂、护肤霜和润肤霜的润湿剂、香精和香精油的增溶剂、化妆品用的遮光剂和珠光剂，同时亦可作为农药杀虫剂、除草剂的乳化剂、造纸行业中的柔软剂以及纺织油剂中的平滑剂和抗静电剂。
但是，在工业上，现有脂肪酸聚氧乙烯酯合成方法的缺陷为：杂质含量高，脂肪酸聚氧乙烯酯收率低。
发明内容
本发明通过改进表面活性剂的制备方法，解决了上述的问题。
本发明提供了一种用于制备表面活性剂的催化剂的制备方法，所述制备方法如下：将铁盐、钇盐和镁盐溶于水中，再向其加入活性碳，浸渍，干燥，热解炭化，得到用于制备表面活性剂的催化剂。
本发明优选为所述铁盐为可溶于水的盐，例如：硝酸铁。
本发明优选为所述钇盐为可溶于水的盐，例如：硝酸钇。
本发明优选为所述镁盐为可溶于水的盐，例如：硝酸镁。
本发明优选为所述铁盐、钇盐与镁盐中铁、钇、镁的摩尔比为1：0.5-0.8： 0.2-0.5，进一步优选为1：0.7-0.75：0.3-0.35，最优选为1：0.7：0.3。
本发明优选为所述活性碳在使用前，先将活性碳浸泡在酸中，浸泡后过滤、洗涤、干燥，再浸泡在碱中，浸泡后过滤、洗涤、干燥。
本发明优选为所述酸为硝酸或盐酸。
本发明优选为所述碱为氢氧化钠溶液。
本发明优选为所述浸渍的时间为8-10h。
本发明优选为所述热解炭化的条件为：在惰性气氛下，820-900℃热解炭化2- 3h。
本发明另一目的为提供一种上述方法制备的用于制备表面活性剂的催化剂。
本发明又一目的为提供一种表面活性剂的制备方法，所述制备方法如下：在上述催化剂的存在下，以环氧乙烷、脂肪酸为原料，反应得到脂肪酸聚氧乙烯酯表面活性剂。
本发明优选为上述催化剂加入量为理论产量的0.05-0.1％，进一步优选为 0.05-0.08％，最优选为0.08％。
本发明有益效果为：
本发明所述方法制备的脂肪酸聚氧乙烯酯表面活性剂收率高、杂质少。
具体实施方式
下述非限制性实施例可以使本领域的普通技术人员更全面地理解本发明，但不以任何方式限制本发明。
实施例1
一种用于制备表面活性剂的催化剂的制备方法，所述制备方法如下：
将活性碳颗粒浸泡在3mol/L盐酸中12h，浸泡后过滤、用去离子水洗涤活性碳、 90℃烘干，再浸泡在1mol/L氢氧化钠溶液中12h，浸泡后过滤、用去离子水洗涤活性碳、90℃烘干，得到预处理后活性碳；
将硝酸铁、硝酸钇和硝酸镁溶于去离子水中形成溶液，硝酸铁、硝酸钇与硝酸镁中铁、钇、镁的摩尔比为1：0.7：0.3，再向其加入预处理后活性碳，浸渍8h， 90℃烘干，在氩气气氛下，850℃热解炭化3h，冷却至室温，得到用于制备表面活性剂的催化剂。
对比例1
一种催化剂的制备方法，所述制备方法如下：
将活性碳颗粒浸泡在3mol/L盐酸中12h，浸泡后过滤、用去离子水洗涤活性碳、 90℃烘干，再浸泡在1mol/L氢氧化钠溶液中12h，浸泡后过滤、用去离子水洗涤活性碳、90℃烘干，得到预处理后活性碳；
将硝酸铁和硝酸钇溶于去离子水中形成溶液，硝酸铁与硝酸钇中铁、钇的摩尔比为1：0.7，再向其加入预处理后活性碳，浸渍8h，90℃烘干，在氩气气氛下， 850℃热解炭化3h，冷却至室温，得到催化剂。
对比例2
一种催化剂的制备方法，所述制备方法如下：
将活性碳颗粒浸泡在3mol/L盐酸中12h，浸泡后过滤、用去离子水洗涤活性碳、 90℃烘干，再浸泡在1mol/L氢氧化钠溶液中12h，浸泡后过滤、用去离子水洗涤活性碳、90℃烘干，得到预处理后活性碳；
将硝酸铁和硝酸镁溶于去离子水中形成溶液，硝酸铁与硝酸镁中铁、镁的摩尔比为1：0.3，再向其加入预处理后活性碳，浸渍8h，90℃烘干，在氩气气氛下， 850℃热解炭化3h，冷却至室温，得到催化剂。
对比例3
一种催化剂的制备方法，所述制备方法如下：
将活性碳颗粒浸泡在3mol/L盐酸中12h，浸泡后过滤、用去离子水洗涤活性碳、 90℃烘干，再浸泡在1mol/L氢氧化钠溶液中12h，浸泡后过滤、用去离子水洗涤活性碳、90℃烘干，得到预处理后活性碳；
将硝酸钇和硝酸镁溶于去离子水中形成溶液，硝酸钇与硝酸镁中钇、镁的摩尔比为0.7：0.3，再向其加入预处理后活性碳，浸渍8h，90℃烘干，在氩气气氛下，850℃热解炭化3h，冷却至室温，得到催化剂。
实施例2
一种脂肪酸聚氧乙烯酯表面活性剂的制备方法，所述制备方法如下：
在实施例1制备的催化剂的存在下，以油酸、环氧乙烷为原料，实施例1制备的催化剂加入量为理论产量的0.08％，140℃反应2.5h，得到脂肪酸聚氧乙烯酯表面活性剂，脂肪酸聚氧乙烯酯的收率见下表1。
对比例4
一种脂肪酸聚氧乙烯酯表面活性剂的制备方法，所述制备方法如下：
在对比例1制备的催化剂的存在下，以油酸、环氧乙烷为原料，对比例1制备的催化剂加入量为理论产量的0.08％，140℃反应2.5h，得到脂肪酸聚氧乙烯酯表面活性剂，脂肪酸聚氧乙烯酯的收率见下表1。
对比例5
一种脂肪酸聚氧乙烯酯表面活性剂的制备方法，所述制备方法如下：
在对比例2制备的催化剂的存在下，以油酸、环氧乙烷为原料，对比例2制备的催化剂加入量为理论产量的0.08％，140℃反应2.5h，得到脂肪酸聚氧乙烯酯表面活性剂，脂肪酸聚氧乙烯酯的收率见下表1。
对比例6
一种脂肪酸聚氧乙烯酯表面活性剂的制备方法，所述制备方法如下：
在对比例3制备的催化剂的存在下，以油酸、环氧乙烷为原料，对比例3制备的催化剂加入量为理论产量的0.08％，140℃反应2.5h，得到脂肪酸聚氧乙烯酯表面活性剂，脂肪酸聚氧乙烯酯的收率见下表1。
表1
脂肪酸聚氧乙烯酯的收率(％)
实施例2 95.8
对比例4 90.2
对比例5 91.1
对比例6 88.5

Claims (8)

1.一种用于制备脂肪酸聚氧乙烯酯表面活性剂的催化剂的制备方法，其特征在于：所述制备方法如下：
将铁盐、钇盐和镁盐溶于水中，再向其加入活性碳，浸渍，干燥，热解炭化，得到用于制备表面活性剂的催化剂；
所述铁盐为可溶于水的盐；
所述钇盐为可溶于水的盐；
所述镁盐为可溶于水的盐。
2.根据权利要求1所述用于制备脂肪酸聚氧乙烯酯表面活性剂的催化剂的制备方法，其特征在于：所述铁盐、钇盐与镁盐中铁、钇、镁的摩尔比为1：0.5-0.8：0.2-0.5。
3.根据权利要求1所述用于制备脂肪酸聚氧乙烯酯表面活性剂的催化剂的制备方法，其特征在于：所述活性碳在使用前，先将活性碳浸泡在酸中，浸泡后过滤、洗涤、干燥，再浸泡在碱中，浸泡后过滤、洗涤、干燥。
4.根据权利要求1所述用于制备脂肪酸聚氧乙烯酯表面活性剂的催化剂的制备方法，其特征在于：所述浸渍的时间为8-10h。
5.根据权利要求1所述用于制备脂肪酸聚氧乙烯酯表面活性剂的催化剂的制备方法，其特征在于：所述热解炭化的条件为：在惰性气氛下，820-900℃热解炭化2-3h。
6.权利要求1、2、3、4或5所述方法制备的用于制备脂肪酸聚氧乙烯酯表面活性剂的催化剂。
7.一种脂肪酸聚氧乙烯酯表面活性剂的制备方法，其特征在于：所述制备方法如下：
在权利要求6所述催化剂的存在下，以环氧乙烷、脂肪酸为原料，反应得到脂肪酸聚氧乙烯酯表面活性剂。
8.根据权利要求7所述脂肪酸聚氧乙烯酯表面活性剂的制备方法，其特征在于：权利要求6所述催化剂加入量为理论产量的0.05-0.1％。
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EP0478073A2 (en) * 1990-09-20 1992-04-01 Union Carbide Chemicals And Plastics Company, Inc. Processes for the preparation of carboxylated compounds
US5118650A (en) * 1988-09-30 1992-06-02 Union Carbide Chemicals & Plastics Technology Corporation Alkoxylation using modified group iiib metal-containing bimetallic or polymetallic catalysts
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Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5118650A (en) * 1988-09-30 1992-06-02 Union Carbide Chemicals & Plastics Technology Corporation Alkoxylation using modified group iiib metal-containing bimetallic or polymetallic catalysts
US5145602A (en) * 1989-02-01 1992-09-08 Union Oil Company Of California Sol/gels containing nonionic surfactants and preparation methods
EP0476786A2 (en) * 1990-09-20 1992-03-25 Union Carbide Chemicals And Plastics Company, Inc. Processes for the preparation of cyclic ethers
EP0478073A2 (en) * 1990-09-20 1992-04-01 Union Carbide Chemicals And Plastics Company, Inc. Processes for the preparation of carboxylated compounds
US5304662A (en) * 1992-01-11 1994-04-19 Ciba-Geigy Corporation Polyglycidyl compounds

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