增稠定型二合一流变改性剂的合成及应用研究

doi:10.3969/j.issn.1001-1803.2022.09.007

摘要/Abstract

摘要：

通过沉淀聚合法分别合成了丙烯酸（AA）/N-乙烯基吡咯烷酮（NVP）、AA/NVP/N-叔丁基丙烯酰胺（BAA）、AA/NVP/N-叔辛基丙烯酰胺（OAA）的交联共聚物,并对其进行了结构及性能表征。通过DSC测定其玻璃化转变温度（T_g）,发现随着BAA和OAA的引入,T_g依次升高。润湿分散性能及聚合物水凝胶测试结果表明,AA/NVP/OAA交联共聚物的润湿分散性能、增稠性能、水凝胶透光率和头发定型能力均较为理想。选取该聚合物进一步考察其流变学性能和发胶应用性能,并对其流变特性和定型机理进行了探讨。水凝胶的流变测试结果表明,该聚合物表现出与传统卡波树脂和市售AA/NVP共聚物流变改性剂不同的流变特性,且其可黏取性能与市售成品发胶接近。发胶应用实验结果表明,该聚合物用于发胶配方中,能同时起到增稠剂和定型剂的作用,其发胶透光率、定型能力优于市售AA/NVP共聚物流变改性剂。

关键词: 沉淀聚合, 流变改性剂, 头发定型

Abstract:

Acrylic acid （AA）/N-vinyl-2-pyrrolidinone （NVP） crosspolymer, AA/NVP/N-tert-butyl acrylamide （BAA） crosspolymer and AA/NVP/N-tert-octyl acrylamide （OAA） crosspolymer were synthesized via precipitation polymerization. The polymers were characterized by FT-IR, ¹H NMR and differential scanning calorimetry （DSC）. Glass transition temperature （T_g） of the polymers were measured by DSC. As the introduction of BAA and OAA, polymers’ T_g rise from 120.50 ℃ to 123.66 ℃ and 129.23 ℃, respectively, while the neutralized polymers’ T_g rise from 97.99 ℃ to 111.76 ℃ and 112.74 ℃, respectively. The viscosity, transmittance, hair curl retention, wetting time and dispersing performance of these samples were characterized to determine their thickening, fixing and dispersing performances. The AA/NVP/OAA crosspolymer shows the best parameters. This polymer sample was selected for further study, such as rheological test and hair gel application. Commercial hair gels usually can stick to the user’s fingers so that it can be picked up easily. The G' （0.1 rad/s）and G'' （100 rad/s） of various samples were determined by rotary rheometer so that rheological properties and pick up performance can be characterized. The G' （0.1 rad/s）and G'' （100 rad/s） of AA/NVP/OAA crosspolymer’s aquogel are comparable with the commercial hair gels, while the commercial carbomers and commercial AA/NVP copolymer show the opposite. These results indicate that AA/NVP/OAA crosspolymer’s aquogel can be easily picked up by users as the commercial hair gels. Hair gel formulation study was also carried out. Formula A is the hair gel prepared by AA/NVP/OAA crosspolymer, which shows comparable performance with the hair gel prepared by carbomer and PVP-K90 （Formula D）. The transmittance of Formula A is 93.82%, viscosity is 59 000 mPa·s and the curl retention is 96.5%. Hair bending strength of Formula A is also comparable with Formula D. These results indicate that AA/NVP/OAA crosspolymer can act as both rheology modifier and hair fixing agent in the formula. Even though commercial AA/NVP polymer can also provide thickening and fixing functions, it shows poorer transmittance, lower curl retention and weaker bending strength in formula. The introduction of NVP and OAA can also improve the compatibility with PVP-K90.

Key words: precipitation polymerization, rheology modifier, hair fixing

中图分类号:

TQ658

麦景璋,李琳,何金清,李泽勇. 增稠定型二合一流变改性剂的合成及应用研究[J]. 日用化学工业, 2022, 52(9): 960-968.

Mai Jingzhang,Li Lin,He Jinqing,Li Zeyong. Study on the synthesis and application of thickening-fixing hybrid rheology modifier[J]. China Surfactant Detergent & Cosmetics, 2022, 52(9): 960-968.

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	x/%
编号	AA	NVP	BAA	OAA
P（AA/NVP）	93.5	6.5	0	0
P（AA/NVP/BAA）	93.5	5	1.5	0
P（AA/NVP/OAA）	93.5	5	0	1.5

	w/%
编号	AA	NVP	BAA或OAA残留
P（AA/NVP）	0.038	0.026	0
P（AA/NVP/BAA）	0.025	0.033	0.062
P（AA/NVP/OAA）	0.030	0.029	0.059

编号	T_g/℃	中和后T_g/℃
市售产品A	168.78	141.20
P（AA/NVP）	120.50	97.99
P（AA/NVP/BAA）	123.66	111.76
P（AA/NVP/OAA）	129.23	112.74

	1.5%水凝胶黏度/（mPa·s）	1.5%水凝胶透光率/%	卷曲保持率/%
P（AA/NVP）	76 000	87.9	91.0
P（AA/NVP/BAA）	70 000	89.1	94.6
P（AA/NVP/OAA）	58 000	92.5	96.8
市售产品A	59 000	90.5	91.3

	A	B	C	D	E
去离子水	余量	余量	余量	余量	余量
P（AA/NVP/OAA）	1.5	1.5	0	0	0
市售产品B	0	0	0.5	0.5	0
市售产品A	0	0	0	0	1.5
甘油	2	2	2	2	2
PVP K90	0	1	0	1	0
TEA	适量	适量	适量	适量	适量
DMDMH	0.3	0.3	0.3	0.3	0.3
CO-40（含10%香精）	0.1	0.1	0.1	0.1	0.1
pH	7.01	6.92	6.80	7.08	6.88
黏度/（mPa·s）	59 000	60 000	47 000	54 000	61 000
透光率/%	93.82	90.98	93.34	86.08	89.25
卷曲保持率/%	96.5	98.1	48.2	96.7	90.1