基于差异硫酸化率的脂肪醇醚硫酸盐制备

doi:10.3969/j.issn.1001-1803.2021.08.004

摘要/Abstract

摘要：

以常规脂肪醇醚（AEO）和三氧化硫为原料,在降膜式磺化器中进行硫酸化反应,得到了不同硫酸化程度的脂肪醇醚硫酸盐（AES）产品。经测定阴离子活性物、游离油及无机酸含量,结合游离油的羟值与气质分析确定了产品中的组分及其随硫酸化率的变化,并通过顶空气相法分析了不同硫酸化率下产品中二噁烷的含量变化。结果表明：低氧乙烯基团加合数的AEO倾向于优先发生硫酸化反应;十二醇及十二烷基AEO相比十四醇及十四烷基AEO更易发生硫酸化反应;控制差异硫酸化率,可以调整氧乙烯基团的平均加合数,调控AEO的氧乙烯基团分布,实现AEO的窄分布;二噁烷含量随着硫酸化率的升高而升高。

关键词: 脂肪醇醚, 三氧化硫, 膜式磺化器, 硫酸化率, 二噁烷

Abstract:

The products of fatty alcohol ether sulfates （AES） with different sulfation degree were obtained by sulfation of fatty alcohol ethers （AEO） with sulfur trioxide in a falling film sulfonator. The components in the products and their changes with sulfation degree were determined by measuring the content of anionic active substance, AEO and inorganic acid, combined with the hydroxyl value of AEO and gas quality analysis. The content of 1,4-dioxane in the products with different sulfation degree was analyzed by headspace gas chromatography. The results show that the AEO with low addition number of oxyethylene group has the priority of sulfation. Dodecanol and dodecyl polyoxyethylene ether react with sulfur trioxide more easily than tetradecanol alcohol and tetradecyl polyoxyethylene ether. The average addition number of polyoxyethylene groups in AEO can be adjusted by controlling the different sulfation degree and thus the distribution of oxyethylene groups in AEO can also be further regulated and narrowed. The content of 1,4-dioxane increases with the increase of sulfation degree.

Key words: fatty alcohol polyoxyethylene ether, sulfur trioxide, falling film sulfonator, sulfation degree, 1;4-dioxane

中图分类号:

TQ423

李建波,李霁云,李萍,杨效益,郭朝华,任晓丹. 基于差异硫酸化率的脂肪醇醚硫酸盐制备[J]. 日用化学工业, 2021, 51(8): 719-724.

Li Jianbo,Li Jiyun,Li Ping,Yang Xiaoyi,Guo Chaohua,Ren Xiaodan. Preparation of fatty alcohol ether sulfates with different sulfation degree[J]. China Surfactant Detergent & Cosmetics, 2021, 51(8): 719-724.

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参考文献 13

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样品	硫酸化率/%	脂肪醇醚硫酸酯含量/%	游离AEO含量/%	无机酸含量/%
5-AES-9	4.5±0.03	5.1±0.03	96.5±0.12	0.1±0.05
15-AES-9	14.9±0.02	16.6±0.02	88.4±0.18	0.1±0.03
20-AES-9	18.6±0.04	20.6±0.04	83.3±0.16	0.1±0.03
25-AES-9	23.0±0.02	25.3±0.02	78.6±0.15	0.1±0.04
30-AES-9	27.4±0.04	29.9±0.04	74.4±0.13	0.2±0.04

样品	羟值/ （KOH mg·g^-1）	平均分子量	氧乙烯基团平均加合数
AEO9	96.2±0.08	583.2±0.5	8.9±0.01
5-AES-9	83.3±0.06	673.2±0.5	10.9±0.01
15-AES-9	79.6±0.08	704.8±0.7	11.7±0.02
20-AES-9	89.3±0.07	628.0±0.5	9.9±0.01
25-AES-9	87.0±0.06	644.8±0.4	10.3±0.01
30-AES-9	84.4±0.09	664.6±0.7	10.7±0.02

组分	样品
组分	5-AES-9	15-AES-9	20-AES-9	25-AES-9	30-AES-9
十二醇	58.0±0.12	22.9±0.13	31.6±0.09	28.9±0.11	30.9±0.13
十四醇	87.9±0.14	66.5±0.14	58.7±0.12	46.1±0.14	53.5±0.11
12-AEO1	76.3±0.11	67.6±0.11	57.2±0.11	58.1±0.11	67.1±0.13
14-AEO1	96.0±0.12	89.8±0.13	69.0±0.16	67.1±0.13	70.0±0.15
12-AEO2	82.2±0.13	68.9±0.09	53.7±0.12	55.9±0.15	69.9±0.12
14-AEO2	98.5±0.17	91.9±0.17	66.6±0.11	62.7±0.12	66.4±0.16
12-AEO3	73.3±0.11	64.0±0.12	49.9±0.16	52.2±0.12	63.3±0.12
14-AEO3	99.5±0.14	92.4±0.16	61.1±0.10	54.2±0.11	64.2±0.11
12-AEO4	79.2±0.12	63.3±0.13	47.7±0.12	50.5±0.17	60.7±0.15
14-AEO4	99.9±0.18	93.7±0.10	70.1±0.12	67.9±0.12	78.6±0.14
12-AEO5	79.8±0.14	65.6±0.11	48.0±0.15	60.2±0.16	71.2±0.10