Synthesis of hyperbranched polymers and its demulsification properties

doi:10.19965/j.cnki.iwt.2024-0223

Industrial Water Treatment ›› 2025, Vol. 45 ›› Issue (4): 127-132. doi: 10.19965/j.cnki.iwt.2024-0223

• RESEARCH AND EXPERIMENT • Previous Articles

Synthesis of hyperbranched polymers and its demulsification properties

Heng ZHANG¹(), Cunchuan ZHENG²()

^1. Xinjiang Branch of China Oilfield Services Co. , Ltd. , Korla 841000, China
^2. School of Chemistry and Chemical Engineering, Southwest Petroleum University, Chengdu 610500, China

Received:2024-06-24 Online:2025-04-20 Published:2025-04-27
Contact: Cunchuan ZHENG

一种超支化聚合物的合成及其破乳性能

张恒¹(), 郑存川²()

^1. 中海油田服务股份有限公司新疆分公司，新疆库尔勒 841000
^2. 西南石油大学化学化工学院，四川成都 610500

通讯作者: 郑存川
作者简介:
张恒（1981— ），工程师，E-mail：zhangheng3@cosl.com.cn。
基金资助:
四川省重点研发项目(2021YFG0112)

Abstract

Abstract:

Hyperbranched polymer (h-PAMAM) with methyl acrylate and ethylenediamine as the backbone was synthesized using one pot method with 1,3-propanediamine as the core. Firstly, 30 mL of methanol was added to the three necked flask, 1,3-propanediamine (0.1 mol) was added with drop-wise of methyl acrylate (0.4 mol) while stirring. Then,the mixture was stirred at 25 ℃ for 24 hours. Ethylenediamine (0.28 mol) and methyl acrylate (0.24 mol) were sequentially added into the flask and continued the reaction for 24 hours. Finally, under vacuum conditions, light green and high viscosity sample was obtained by programmed heating method with reaction at 60 ℃ for 1 hour, reaction at 80 ℃ for 1 hour, reaction at 100 ℃ for 2 hours, reaction at 120 ℃ for 2 hours, and reaction at 140 ℃ for 2 hours. The structure of the polymer was characterized by FT-IR and ¹H NMR, and the demulsification performance of h-PAMAM on diesel oil lotion at different concentrations and temperatures was tested. The ability to reduce the interfacial tension was analyzed by surface tension meter and interfacial tension meter, and the mechanism of its action on the oil-water interface was discussed by microscopic observation. The results showed that when the concentration of h-PAMAM was 50 mg/L, the demulsification temperature was 60 ℃, and the demulsification time was 90 min, the demulsification efficiency could reach 80%, and the oil-water interface was neat. After demulsification, the water phase transmittance of lotion was 84.1%. The demulsifier had the characteristics of high efficiency and low dosage, and had great application potential in demulsification of oil in water lotion.

Key words: hyperbranched polymer, diesel emulsion, demulsification performance

摘要：

以1，3-丙二胺为核，采用“一锅法”合成了以丙烯酸甲酯和乙二胺为骨架的超支化聚合物（h-PAMAM）。首先将30 mL甲醇加入到三口烧瓶中，向其中加入1，3-丙二胺（0.1 mol），边搅拌边滴加丙烯酸甲酯（0.4 mol），随后混合物在25 ℃下继续搅拌反应24 h。然后依次将乙二胺（0.28 mol）和丙烯酸甲酯（0.24 mol）滴加入烧瓶中，继续反应24 h。最后，在真空状态下采用程序升温：60 ℃反应1 h，80 ℃反应1 h，100 ℃反应2 h，120 ℃反应2 h，140 ℃反应2 h，最终得到浅绿色、高黏度的样品。采用FT-IR和¹H NMR对聚合物的结构进行了表征，并测试了h-PAMAM在不同浓度和不同温度条件下对柴油乳液的破乳性能，采用表面张力仪和界面张力仪分析了其降低界面张力的能力以及采用显微观察探讨了其在油水界面上的作用机理。研究结果表明，在h-PAMAM质量浓度为50 mg/L，破乳温度为60 ℃，破乳时间为90 min时，破乳效率均能达到80%，且油水界面整齐，破乳后乳液水相透光率为84.1%。该破乳剂具有高效、低用量的特点，在水包油乳液的破乳中有着很大的应用潜力。

关键词: 超支化聚合物, 柴油乳液, 破乳性能

CLC Number:

TE39

Heng ZHANG, Cunchuan ZHENG. Synthesis of hyperbranched polymers and its demulsification properties[J]. Industrial Water Treatment, 2025, 45(4): 127-132.

张恒, 郑存川. 一种超支化聚合物的合成及其破乳性能[J]. 工业水处理, 2025, 45(4): 127-132.

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https://www.iwt.cn/EN/Y2025/V45/I4/127

Figures/Tables 9

Fig.1 Schematic diagram of h-PAMAM reaction

Fig.2 Infrared spectrum of h-PAMAM

Fig.3 Nuclear magnetic resonance hydrogen spectrum of h-PAMAM

Fig.4 Dynamic interfacial tension of h-PAMAM with different concentrations

Fig.5 Dynamic interfacial tension of h-PAMAM with different concentrations

Fig.6 Effect of demulsification time on the transmittance of aqueous phase

Fig.7 Effect of temperature on the transmittance of water phase

Fig.8 Dynamic demulsification process of diesel lotion observed under microscope

Fig.9 Possible demulsification mechanism of h-PAMAM

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