聚醚和含氟酯共改性苯基含氢硅油的制备及消泡性能

doi:10.3969/j.issn.1001-1803.2019.03.003

日用化学工业 ›› 2019, Vol. 49 ›› Issue (3): 150-155.doi: 10.3969/j.issn.1001-1803.2019.03.003

聚醚和含氟酯共改性苯基含氢硅油的制备及消泡性能

郭睿,韩双(),张瑶,王宁,高弯弯

陕西科技大学教育部轻化工助剂化学与技术重点实验室,陕西西安 710021

收稿日期:2018-06-20 修回日期:2019-01-25 出版日期:2019-03-22 发布日期:2019-04-04
通讯作者: 韩双
作者简介:郭睿（1959-）,教授,研究生导师,电话：13571007215,E-mail： gr304@163.com。
基金资助:
陕西省重点研发计划资助项目(2017ZDXM-GY-0872);陕西省重点研发计划资助项目(2017GY-185)

Preparation and defoaming performance of phenyl hydrogen-containing silicone oil co-modified with polyether and fluorine-containing ester

Rui GUO,Shuang HAN(),Yao ZHANG,Ning WANG,Wan-wan GAO

Key Laboratory of Auxiliary Chemistry & Technology for Chemical Engineering, Ministry of Education, Shaanxi University of Science & Technology, Xi’an, Shaanxi 710021, China

Received:2018-06-20 Revised:2019-01-25 Online:2019-03-22 Published:2019-04-04
Contact: Shuang HAN

摘要/Abstract

摘要：

以10-十一烯酸四氟丙酯（UATE）、聚醚（F-6）和苯基含氢硅油为原料,氯铂酸为催化剂,经硅氢加成反应合成了长链含氟烷基酯与聚醚共改性苯基含氢硅油（UAPFPS）。通过FT-IR和 ¹H NMR对UAPFPS的结构进行了表征,采用单因素试验对反应中各影响因素进行考察得到其较佳工艺参数为：反应温度110 ℃,反应时间5.5 h,n（Si-H） :n（C=C）=1:1.2,n（F-6） :n（UATE）=1:1,催化剂用量20 μg/g（相对于每克反应物）。在此条件下Si-H键转化率为95.30%。将UAPFPS、硅膏、乳化剂和增稠剂复配制得改性有机硅消泡剂,其性能测试结果表明,该消泡剂具有较好的消泡性、抑泡性与稳定性。

关键词: 长链含氟烷基酯, 苯基含氢硅油, 硅氢加成, 消泡剂

Abstract:

10-Undecenoic acid tetrafluoropropyl ester （UATE）, allyl polyether （F-6） and phenyl hydrogen-containing silicone oil were used as raw materials. Chloroplatinic acid was used as catalyst. The phenyl hydrogen-containing silicone oil co-modified with polyether and fluorine-containing ester （UAPFPS） was synthesized via hydrosilylation. The structure of UAPFPS was characterized by FT-IR and ¹H NMR. The optimum parameters were obtained by single factor experiment: the reaction temperature was 110 ℃; the reaction time was 5.5 h; n（Si-H） :n（C=C）=1:1.2; n（F-6） :n（UATE）=1:1; the amount of catalyst is 20 μg/g （relative to each gram of reactant）. Under this condition, the conversion of Si-H bonds was 95.30%. A modified silicone defoamer was prepared by compounding UAPFPS, silicone paste, emulsifiers and thickener. The results of performance test show that the defoamer has good defoaming properties, foam inhibition and stability.

Key words: long-chain fluorinated alkyl ester, phenyl hydrogen-containing silicone oil, hydrosilylation, defoamer

中图分类号:

TQ423.95

郭睿,韩双,张瑶,王宁,高弯弯. 聚醚和含氟酯共改性苯基含氢硅油的制备及消泡性能[J]. 日用化学工业, 2019, 49(3): 150-155.

Rui GUO,Shuang HAN,Yao ZHANG,Ning WANG,Wan-wan GAO. Preparation and defoaming performance of phenyl hydrogen-containing silicone oil co-modified with polyether and fluorine-containing ester[J]. China Surfactant Detergent & Cosmetics, 2019, 49(3): 150-155.

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n（Si-H）∶n（C=C）	γ/（mN·m^-1）
1∶1.0	26.9
1∶1.05	25.4
1∶1.1	24.1
1∶1.15	23.7
1∶1.2	23.2
1∶1.25	22.4
1∶1.3	23.6

θ/℃	冻融稳定性
0	未分层
-5	未分层
-10	未分层
-15	未分层
-20	未分层
-25	分层

转速/（r·min^-1）	离心稳定性
2 000	未分层
2 500	未分层
3 000	未分层
3 500	分层

聚醚和含氟酯共改性苯基含氢硅油的制备及消泡性能

Preparation and defoaming performance of phenyl hydrogen-containing silicone oil co-modified with polyether and fluorine-containing ester

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