微波辅助半干法合成阳离子瓜尔胶工艺条件的优化

doi:10.3969/j.issn.1001-1803.2019.09.004

摘要/Abstract

摘要：

以瓜尔胶为原料,2,3-环氧丙基三甲基氯化铵为醚化剂,氧氧化钠为催化剂,利用微波辅助半干法合成了阳离子瓜尔胶,并进行了红外和核磁表征。结果表明,在瓜尔胶醚化过程中使用微波辅助,反应时间是传统阳离子瓜尔胶合成方法的1/5,大大提高了反应效率。较佳反应条件为：微波功率640 W,微波辐射反应时间45 min,碱液与瓜尔胶的质量比为0.08∶1,微波温度60 ℃,在此条件下制备的阳离子瓜尔胶含氮量为1.23%。黏度实验表明：微波法合成的阳离子瓜尔胶水溶性好,黏度可达7 000 mpa·s。

关键词: 阳离子瓜尔胶, 微波辅助, 合成, 含氮量

Abstract:

Cationic guar gum（CGG） was synthesized with guar gum（GG） as raw materials, 2,3-epoxypr-opyltrimethylammonium chloride（GTA） as cationic etherifying agent and sodium hydroxide as catalyst by microwave-assisted semi-dry method, and characterized by IR and NMR . The results show that microwave-assisted etherification of guar gum shortens the reaction time to 1/5 of that in the traditional cationic guar gum synthesis method, which greatly improves the reaction efficiency. The optimum synthesis conditions were as follows:microwave power 640 W, microwave irradiation reaction time 45 min, mass ratio of alkali liquor to guar gum 0.08∶1, microwave temperature 60 ℃. Under these optimized conditions, the nitrogen content of cationic guar gum is 1.23%. Viscosity experiment shows that the cationic guar gum synthesized by microwave-assisted semi-dry method has good water solubility and its viscosity can reach up to 7 000 mpa·s.

Key words: cationic guar gum, microwave-assisted, synthesis, nitrogen content

中图分类号:

TQ423

张春晓,唐逸飞,王向鹏. 微波辅助半干法合成阳离子瓜尔胶工艺条件的优化[J]. 日用化学工业, 2019, 49(9): 579-584.

ZHANG Chun-xiao,TANG Yi-fei,WANG Xiang-peng. Optimization of process conditions for synthesis of cationic guar gum by microwave-assisted semi-dry method[J]. China Surfactant Detergent & Cosmetics, 2019, 49(9): 579-584.

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微波温度/℃	外观	η/（mpa·s）	X/%	DS	RE/%
40	浅黄色粉末	6 800	1.14	0.049	67.1
60	浅黄色粉末	6 500	1.23	0.061	83.6
80	深黄色粉末	5 600	1.16	0.052	71.2
100	褐色,部分碳化	–	–	–	–

水平	因素
水平	A 微波功率/W	B 反应时间/min	C 加碱量/g
1	400	30	0.4
2	640	45	0.8
3	800	75	1.2

序号	A	B	C	X/%
1	400	30	0.4	0.48
2	400	45	0.8	0.75
3	400	75	1.2	0.68
4	640	30	1.2	0.98
5	640	45	0.8	1.23
6	640	75	0.4	0.86
7	800	30	1.2	0.92
8	800	45	0.4	0.62
9	800	75	0.8	0.80
K₁	0.63	0.79	0.65
K₂	1.02	0.86	0.93
K₃	0.78	0.78	0.86
R	0.39	0.08	0.28

合成方法	指标
	t/min	η/（mpa·s）		X/%		DS	RE/%
	t/min	检测值	相对偏差/%	检测值	相对偏差/%	DS	RE/%
微波辅助半干法	45	6 500	1.04	1.23	1.65	0.061	83.6
		6 400	-0.51	1.21	0	0.059	80.8
		6 400	-0.51	1.19	-1.65	0.056	76.7
传统加热法	200	6 200	-0.53	1.18	1.71	0.055	75.3
		6 300	1.07	1.16	-1.71	0.052	71.5
		6 200	-0.53	1.17	0	0.054	74.0