新型树状大分子的制备及其破乳性能

doi:10.16085/j.issn.1000-6613.2020-1447

摘要/Abstract

摘要：

以自制双(2-邻苯二甲酰亚胺)胺（DETA-2PA）与烯丙基缩水甘油醚通过开环反应合成N-(3-烯丙氧基-2-羟丙基)-双［乙基-(2-邻苯二甲酰亚胺)］（AGE-DETA-2PA），将AGE-DETA-2PA在水合肼的作用下脱去邻苯二甲酰基得到活性中间体N-(3-烯丙氧基-2-羟丙基)-双(乙基胺)（AGE-DETA），再将AGE-DETA与丙烯酸甲酯和乙二胺通过迈克尔加成合成树状大分子AGE-PAMAM。并用红外光谱和核磁氢谱进行结构表征，通过特性黏度确定各整代分子特性黏度大于相邻半代分子，通过表面张力的测定确定破乳剂分子对水的表面张力最低为66.402mN/m。通过粒径分析、zeta电位测试、偏光显微镜分析得出乳液破乳的机理主要为电荷中和作用和吸附架桥作用。在破乳剂添加量为1.0g/L、破乳温度为40℃、沉降时间为60min的条件下，Turbiscan Lab稳定性分析仪光谱图和TSI值得出AGE-PAMAM破乳剂破乳效果优于市售SP169和HQ96-1破乳剂，并且该破乳剂在添加量为2.0g/L、破乳温度为45℃、沉降时间为120min的条件下，脱水率可达98.5%，脱出污水含油量为5.6mg/L，脱出污水透光率为98.47%。

关键词: 树状大分子, 迈克尔加成, 电荷中和, 吸附架桥

Abstract:

N-(3-allyloxy-2-hydroxypropyl) was synthesized by self-made bis(2-phthalimide)amine (DETA-2PA) and allyl glycidyl ether through ring-opening reaction bis[ethyl-(2-phthalimide)] (AGE-DETA-2PA), and AGE-DETA-2PA was removed under the action of hydrazine hydrate to get the active intermediate N-(3-allyloxy-2-hydroxypropyl)-bis(ethylamine) (AGE-DETA). Then, AGE-DETA was combined with methyl acrylate and ethylenediamine to synthesize dendrimers through Michael addition AGE-PAMAM. Infrared spectroscopy and hydrogen nuclear magnetic spectroscopy were used for structural characterization. The intrinsic viscosity of each generation of molecules was determined by intrinsic viscosity to be greater than that of adjacent half-generation molecules. The surface tension of the demulsifier molecules against water was determined to be 66.402mN/m minimum by the measurement of surface tension. Through particle size analysis, zeta potential test and polarization microscope analysis, it was concluded that the mechanism of emulsion breaking was mainly charge neutralization and adsorption bridging. Under the conditions of 1.0g/L of demulsifier, demulsifier temperature of 40℃, and sedimentation time of 1h, Turbiscan Lab stability analyzer spectrum and TSI value showed that the demulsifier effect of AGE-PAMAM demulsifier was better than that of the market sold SP169 and HQ96-1 demulsifiers. When the demulsifier was added at 2.0g/L, the demulsification temperature is 45℃, and the settling time was 120min, the dehydration rate can reach 98.5% with the oil content of the discharged sewage of 5.6mg/L and the light transmittance of the discharged sewage of 98.47%.

Key words: dendrimer, Michael addition, charge neutralization, adsorption bridging

中图分类号:

TQ423

郭睿, 徐康, 闫育蒙, 马丽娟, 张晓飞. 新型树状大分子的制备及其破乳性能[J]. 化工进展, 2021, 40(6): 3363-3373.

GUO Rui, XU Kang, YAN Yumeng, MA Lijuan, ZHANG Xiaofei. Preparation and demulsification performance of novel dendrimer[J]. Chemical Industry and Engineering Progress, 2021, 40(6): 3363-3373.

图/表 17

参考文献 21

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破乳剂AEG-PAMAM3.0G 添加量 /g·L^-1	脱水率/%	脱出污水含油量 /mg·L^-1	界面状况	水相清洁度	吸光度（550nm）	透光率/%
0.4	94.2	528.1	不齐	浑浊，偏黄	2.3278	<1
0.8	94.4	328.0	不齐	较浑浊，微黄	0.8620	13.74
1.2	95.3	147.8	较齐	较清	0.2840	52.00
1.6	95.9	74.6	齐	较清	0.1233	75.28
2.0	96.9	27.5	齐	清	0.0283	93.69
2.4	95.5	61.3	齐	清	0.0868	81.88
2.8	95.3	104.3	齐	较清	0.1146	76.81

破乳剂AEG-PAMAM3.0G 添加量 /g·L^-1	脱水率/%	脱出污水含油量 /mg·L^-1	界面状况	水相清洁度	吸光度（550nm）	透光率/%
0.4	94.2	528.1	不齐	浑浊，偏黄	2.3278	<1
0.8	94.4	328.0	不齐	较浑浊，微黄	0.8620	13.74
1.2	95.3	147.8	较齐	较清	0.2840	52.00
1.6	95.9	74.6	齐	较清	0.1233	75.28
2.0	96.9	27.5	齐	清	0.0283	93.69
2.4	95.5	61.3	齐	清	0.0868	81.88
2.8	95.3	104.3	齐	较清	0.1146	76.81

破乳温度 /℃	脱水率 /%	脱出污水含油量/mg·L^-1	界面状况	水相清洁度	吸光度（550nm）	透光率 /%
30	91.4	42.9	齐	较清，有挂壁	0.078	83.57
35	92.8	31.3	齐	较清，有挂壁	0.047	89.72
40	95.2	18.6	齐	清	0.019	95.76
45	97.4	7.2	齐	清	0.016	96.48
50	93.6	27.9	齐	清	0.025	94.48
55	91.4	44.3	齐	较清	0.090	81.19
60	90.5	49.5	齐	较清	0.122	75.50

破乳温度 /℃	脱水率 /%	脱出污水含油量/mg·L^-1	界面状况	水相清洁度	吸光度（550nm）	透光率 /%
30	91.4	42.9	齐	较清，有挂壁	0.078	83.57
35	92.8	31.3	齐	较清，有挂壁	0.047	89.72
40	95.2	18.6	齐	清	0.019	95.76
45	97.4	7.2	齐	清	0.016	96.48
50	93.6	27.9	齐	清	0.025	94.48
55	91.4	44.3	齐	较清	0.090	81.19
60	90.5	49.5	齐	较清	0.122	75.50

沉降时间 /min	脱水率 /%	脱出污水含油量 /mg·L^-1	界面状况	水相清洁度	吸光度（550nm）	透光率 /%
20	93.1	114.4	齐	较清	0.1358	73.15
40	95.3	69.8	齐	较清	0.0937	80.59
60	96.2	35.6	齐	清	0.0456	90.03
80	97.4	16.8	齐	清	0.0136	96.92
100	98.1	7.7	齐	清	0.0074	98.31
120	98.5	5.6	齐	清	0.0067	98.47
140	98.5	5.6	齐	清	0.0067	98.47