支链型硅烷、聚醚烷基共改性硅油乳化剂的制备及性能研究

doi:10.3969/j.issn.1001-1803.2019.09.003

Abstract

Abstract:

The vinyltris（trimethylsiloxy）silane（branched-silicone）was synthesized by the hydrolytic condensation of triethoxyvinylsilane and ethoxytrimethylsilane. The modified silicone emulsifier was synthesized through hydrosilylation reactions, using hexachloroplatinic acid as catalyst, isopropanol as solvent, and polymethylhydrosiloxane, vinyltris（trimethylsiloxy）silane, allyl polyther and 1-dodecene as raw materials. The structure of the modified silicone was characterized by ¹H NMR and FT-IR. The effects of reaction temperature（T）, time（t）, catalyst dosage and material ratio on the conversion were investigated. The effects of the structure of modified silicone emulsifier on the stability of water-in-oil emulsion was also studied. The results show that the conversion is 94.97% when T=95 ℃, t=5 h, the catalyst dosage of 0.20% and n（Si-H）∶n（C=C content of the mixture）=1∶1.1. When the HLB value of the emulsifier is equal to 5 and n（branched-silicone）∶n（alkyl）=25∶75, stable water-in-oil emulsion can be prepared by using the mixed oil phase composed of silicone oil, ester oil and hydrocarbon oil.

Key words: silicone emulsifier, hydrosilylation, water-in-oil emulsion

CLC Number:

TQ423

HE Tong,YANG Cheng. Synthesis and properties of the modified silicone emulsifier with branched-silicone-polyether and alkyl group[J].China Surfactant Detergent & Cosmetics, 2019, 49(9): 572-578.

Figures/Tables 9

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References 14

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	原料	w/%
油相	硅油	7.67
	GTCC	7.67
	异十二烷	7.67
	改性硅油乳化剂	2.00
水相	去离子水	至100
	NaCl	0.50
	1,3-丁二醇	6.00

序号	反应温度/ ℃	时间/h	催化剂用量/%	n（Si-H）∶ n（C=C）	转化率/%
1	85	4	0.10	1∶1.05	77.84
2	85	5	0.15	1∶1.1	86.76
3	85	6	0.20	1∶2	83.73
4	90	4	0.15	1∶2	86.98
5	90	5	0.20	1∶1.05	88.98
6	90	6	0.10	1∶1.1	89.77
7	95	4	0.20	1∶1.1	92.29
8	95	5	0.10	1∶2	93.65
9	95	6	0.15	1∶1.05	89.29
均值K₁	85.75	85.70	87.08	85.37	-
均值K₂	88.58	89.80	87.68	89.61	-
均值K₃	91.74	87.60	88.34	88.12	-
极差R	5.99	4.10	1.25	4.24	-
主次顺序	A>D>B>C
最优方案	A₃B₂C₃D₂

物质	σ/cm^-1	红外峰归属
含氢硅油	2 950~2 873	-CH₃、-CH₂伸缩振动
	2 150	Si-H伸缩振动
	1 120~1 031	Si-O-Si伸缩振动
乙烯基三（三甲基硅氧烷基）硅烷	1 605	C=C伸缩振动
	1 250	Si-（CH₃） ₃非对称伸缩振动
	1 054~1 013	Si-O-Si伸缩振动
	794	Si-C伸缩振动
共改性硅油	3 492	-OH伸缩振动
	2 960~2 865	-CH₃、-CH₂伸缩振动
	1 090~1 013	C-O-C、Si-O-Si伸缩振动
	757	-CH₂面内摇摆

HLB值	粒径/μm	PDI
4	5.3±0.9	1.17±0.08
5	4.8±0.7	1.06±0.01
6	5.5±1.1	1.09±0.04
7	7.7±1.5	1.33±0.13

n（支链硅）∶n（烷基）	油相
	硅油			异十二烷
	外观	粒径/μm	PDI	外观	粒径/μm	PDI
100/0	稳定	5.4±0.4	1.04±0.01	分水	-	-
75/25	稳定	6.2±0.9	1.09±0.03	分油	8.6±2.1	1.31±0.11
50/50	稳定	6.7±0.9	1.13±0.07	稳定	7.1±1.1	1.18±0.06
25/75	稳定	6.8±1.0	1.15±0.07	稳定	5.5±0.9	1.07±0.03
0/100	分油	8.9±1.8	1.32±0.12	稳定	5.1±0.7	1.06±0.02

Synthesis and properties of the modified silicone emulsifier with branched-silicone-polyether and alkyl group

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