双十八烷基二羟乙基溴化铵的微波合成及性能

doi:10.11949/j.issn.0438-1157.20190005

摘要/Abstract

摘要：

以十八烷基二乙醇胺和溴代十八烷通过微波合成技术制备了双十八烷基二羟基溴化铵季铵盐（DODAB）。确定最佳合成工艺条件为：反应物浓度为2.17 mol·L^-1、反应时间为158.61 min、微波功率为626.06 W，在此条件下转化率的预测值为93.71%。产品由IR和¹H NMR进行表征。测定产品的表面活性为：CMC=0.501 g·L^-1，表面张力为30.27 mN·m^-1，优于阳离子表面活性剂D1821。测定产品应用于织物的柔软性能，结果显示：DODAB的柔软效果与D1821相当，随着处理的次数增多，DODAB处理后的柔软效果虽比D1821稍微弱一些，但其手感上会更为自然，更为舒适。同时，DODAB较D1821有着更好的维持织物白度性能的效果，具有较好的抗黄变能力。

关键词: 微波, 合成, 表面活性剂, 双十八烷基二羟乙基溴化铵, 优化, 柔软剂

Abstract:

Dioctadecyldihydroxyethyl ammonium bromide (DODAB) was prepared by microwave synthesis of octadecyldiethanolamine and bromooctadecane. The optimum synthetic conditions were determined as follows: the concentration of reactant was 2.17 mol·L^-1, the reaction time was 158.61 min, and the microwave power was 626.06 W. Under these conditions, the predicted conversion was 93.71%. The product was characterized by IR and ¹H NMR. The surface activity of the product is determined as follows: CMC=0.501 g·L^-1, surface tension is 30.27 mN·m^-1, which is better than cationic surfactant D1821. The results show that the softening effect of DODAB is similar to that of D1821. With the increase of treatment times, the softening effect of DODAB treatment is slightly weaker than that of D1821, but its hand feel is more natural and comfortable. At the same time, DODAB is better than D1821 in maintaining fabric whiteness and yellowing resistance.

Key words: microwave, synthesis, surfactants, dioctadecyldihydroxyethyl ammonium bromide, optimization, softener

中图分类号:

TQ 423.12

陈燕饶, 毛桃嫣, 郑成. 双十八烷基二羟乙基溴化铵的微波合成及性能[J]. 化工学报, 2019, 70(S1): 226-234.

Yanrao CHEN, Taoyan MAO, Cheng ZHENG. Microwave synthesis and properties of dioctadecyldihydroxyethyl ammonium bromide[J]. CIESC Journal, 2019, 70(S1): 226-234.

图/表 15

表1 溶剂对转化率的影响

Table 1 Effect of different solvents on conversion rate

溶剂	转化率/%	产物颜色
正丁醇	12.4	淡黄色
正戊醇	30.77	浅黄色
正己醇	74.8	黄色

图1 反应时间对转化率的影响

Fig.1 Effect of time on conversion rate

图2 反应物浓度对转化率的影响

Fig.2 Effect of reactant concentration on conversion rate

图3 微波功率对转化率的影响

Fig.3 Effect of microwave power on conversion rate

表2 响应面实验的因素-水平

Table 2 Response surface experiment factors - level

水平	因素
水平	反应物浓度（A）/(mol·L^-1)	微波功率（B）/W	反应时间（C）/min
-1	2	500	120
0	2.2	600	150
1	2.4	700	180

表3 响应面分析方案与结果

No.	Reactant concentration（A）/ （mol·L^-1）	Power（B）/W	Time（C）/min	Conversion rate（response 1）/%
1	2.20	180.00	600.00	92.12
2	2.40	120.00	500.00	82.52
3	2.20	150.00	600.00	92.89
4	2.20	150.00	600.00	93.25
5	2.20	150.00	500.00	90.0
6	2.00	180.00	700.00	89.87
7	2.00	150.00	600.00	91.89
8	2.20	150.00	600.00	93.24
9	2.00	120.00	500.00	83.33
10	2.00	120.00	700.00	87.18
11	2.40	150.00	600.00	90.84
12	2.40	120.00	700.00	86.5
13	2.20	150.00	600.00	93.68
14	2.40	180.00	500.00	86.37
15	2.20	150.00	600.00	93.75
16	2.00	180.00	500.00	87.56
17	2.20	120.00	600.00	88.77
18	2.20	150.00	600.00	93.4
19	2.40	180.00	700.00	88.57
20	2.20	150.00	700.00	91.4

表4 二次方模型的方差分析

Table 4 Quadratic model variance analysis

Source	Squares	df	Square	F-value	Prob> F	Remar k
model	220.37	9	24.49	130.41	< 0.0001	significant
A(反应物浓度)	2.53	1	2.53	13.48	0.0043
B(时间)	26.21	1	26.21	139.60	< 0.0001
C(功率)	18.88	1	18.88	100.55	< 0.0001
AB	0.12	1	0.12	0.67	0.4335
AC	5.000×10^-5	1	5.000×10^-5	2.663×10^-4	0.9873
BC	1.38	1	1.38	7.34	0.0220
A²	8.36	1	8.36	44.53	< 0.0001
B²	19.51	1	19.51	103.92	< 0.0001
C²	15.95	1	15.95	84.97	< 0.0001
residual	1.88	10	0.19
lack of fit	1.37	5	0.27	2.73	0.1471	not significant
pure error	0.50	5	0.10
cor total	222.24	19

图4 微波功率和反应物浓度交互影响转化率的响应面图与等高线图

Fig.4 Response surface plotted and contour map on microwave power and concentration of reactants

图5 反应时间和反应物浓度交互影响转化率的响应面图与等高线图

Fig.5 Response surface plotted and contour map on react time and concentration of reactants

图6 微波功率和反应时间交互影响转化率的响应面图与等高线图

Fig.6 Response surface plotted and contour map on microwave power and react time

图7 产物的红外谱图

Fig.7 IR spectra of product

图8 合成产品的1H NMR谱图

Fig.8 1H NMR spectrum of synthesized product

图9 产物和D1821的γ-lgC的关系曲线

Fig.6 γ-lgC relation curve of product and D1821

图10 表面活性剂的柔软性能结果

Fig.10 Results of softening property

图11 柔软剂对织物抗黄变性能的影响

Fig.11 Softeners against yellowing properties of fabrics

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