烷基化壳聚糖硫酸盐的制备及性能研究

doi:10.3969/j.issn.1001-1803.2020.11.003

摘要/Abstract

摘要：

通过希夫碱反应并还原、硫酸化和中和反应,合成了两种壳聚糖表面活性剂:十二烷基壳聚糖硫酸盐（D₁₂CTS）和十烷基壳聚糖硫酸盐（D₁₀CTS）。通过红外光谱（FT-IR）、核磁共振氢谱（¹H NMR）、元素分析（EA）和热重分析（TGA）鉴定了它们的结构。结果表明,D₁₀CTS和D₁₂CTS的烷基化度分别为0.77和0.52,硫酸化度分别为1.35和1.79。通过表面张力和接触角测量表明D₁₀CTS和D₁₂CTS具有良好的表面活性和铺展性,临界胶束浓度（cmc）分别为0.69和0.49 g/L,最低表面张力（γ_cmc）分别为39.50和35.75 mN/m。目标产物具有一定的起泡性能和乳化能力,该表面活性剂为低泡型表面活性剂,有望在化妆品领域发挥潜在的应用。

关键词: 壳聚糖表面活性剂, 烷基化度, 硫酸化度, 低泡型表面活性剂

Abstract:

Two kinds of chitosan surfactants, dodecyl chitosan sulfate （D₁₀CTS） and decyl chitosan sulfate （D₁₂CTS） were synthesized by Schiff base reaction, reduction, sulfation and neutralization reaction. Their structures were identified by infrared spectroscopy （FT-IR）, H NMR spectroscopy（¹H NMR）, elemental analysis （EA）, and thermogravimetric analysis （TGA）. The results show that the degrees of alkylation are 0.77 and 0.52, and the degrees of sulfation are 1.35 and 1.79, respectively. Favourable surface activity and spreadability of D₁₀CTS and D₁₂CTS were evidenced by surface tension and contact angle measurements. The critical micelle concentrations （cmc） are 0.69 and 0.49 g/L, and the minimum surface tension γ_cmc are 39.50 and 35.75 mN/m, respectively. The target products possess certain foaming properties and emulsification performance. The surfactants are low-foaming and are expected to play a potential application in the field of cosmetics.

Key words: chitosan surfactant, degree of alkylation, degree of sulfation, low-foaming surfactant

中图分类号:

TQ423

贾振勇,李萍,杨效益,郭朝华,李建波. 烷基化壳聚糖硫酸盐的制备及性能研究[J]. 日用化学工业, 2020, 50(11): 749-755.

JIA Zhen-yong,LI Ping,YANG Xiao-yi,GUO Chao-hua,LI Jian-bo. Preparation and properties of alkylated chitosan sulfate[J]. China Surfactant Detergent & Cosmetics, 2020, 50(11): 749-755.

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样品	w（C）/%	w（N）/%	w（H）/%	w（S）/%	DS_alkyl/%	DS_sulfo/%	DA/%
CTS	41.51	7.61	6.36	—	—	—	71.0
D₁₀CTS	33.86	2.80	8.29	8.66	77.38	135.31	71.0
D₁₂CTS	30.83	2.85	6.97	11.65	52.08	178.84	71.0

样品	阶段	T₀	T_e	w_f/%	R/%
CTS	Ⅰ	50	248	8	92
	Ⅱ	248	336	39	53
	Ⅲ	336	657	53	0
	Ⅳ	657	800	0	0
D₁₀CTS	Ⅰ	50	202	8	92
	Ⅱ	202	318	38	54
	Ⅲ	318	599	18	36
	Ⅳ	599	761	21	15
	Ⅴ	761	800	0	15
D₁₂CTS	Ⅰ	50	238	11	89
	Ⅱ	238	322	29	60
	Ⅲ	322	574	17	43
	Ⅳ	574	772	23	20
	Ⅴ	772	800	1	19