化工学报
化工學報
화공학보
JOURNAL OF CHEMICAL INDUSY AND ENGINEERING (CHINA)
2015年
6期
2181-2188
,共8页
龚红升%胡文斌%廖列文%张蔚欣%刘其海%胡国栋
龔紅升%鬍文斌%廖列文%張蔚訢%劉其海%鬍國棟
공홍승%호문빈%료렬문%장위흔%류기해%호국동
非离子%表面活性剂%有机硅%硅氢加成%水解性能%响应面法
非離子%錶麵活性劑%有機硅%硅氫加成%水解性能%響應麵法
비리자%표면활성제%유궤규%규경가성%수해성능%향응면법
non-ionic%surfactant%silicone%hydrosilylation%hydrolysis performance%response surface methodology
选用EO(环氧乙烷ethylene oxide)链长为7~8,平均相对分子质量为380的烯丙醇聚氧烷羟基醚(PE-38)和1,1,1,3,5,5,5-七甲基三硅氧烷(MDHM)为原料,通过无溶剂聚合,在氮气保护下经Karstedt催化剂催化硅氢加成反应制备了非离子型聚醚改性三硅氧烷表面活性剂(NTS),并通过傅里叶红外光谱仪和质子核磁共振仪验证了其结构。采用响应面法对合成工艺进行了优化,确定了 NTS 的最佳合成条件为:n(C C):n(Si—H)=0.93,反应温度为94℃,催化剂用量为6.4 mg·kg?1,在反应时间为2 h下,经3次重复试验所得产品的平均表面张力为18.417 mN·m?1,与理论预测值基本相符。测试了产物NTS 0.1%(质量分数)的水溶液在pH为4、7和10的水溶液中的水解性能,发现该产物在酸性和碱性条件下可稳定存放30 d左右,在中性条件下可稳定存放60 d左右。
選用EO(環氧乙烷ethylene oxide)鏈長為7~8,平均相對分子質量為380的烯丙醇聚氧烷羥基醚(PE-38)和1,1,1,3,5,5,5-七甲基三硅氧烷(MDHM)為原料,通過無溶劑聚閤,在氮氣保護下經Karstedt催化劑催化硅氫加成反應製備瞭非離子型聚醚改性三硅氧烷錶麵活性劑(NTS),併通過傅裏葉紅外光譜儀和質子覈磁共振儀驗證瞭其結構。採用響應麵法對閤成工藝進行瞭優化,確定瞭 NTS 的最佳閤成條件為:n(C C):n(Si—H)=0.93,反應溫度為94℃,催化劑用量為6.4 mg·kg?1,在反應時間為2 h下,經3次重複試驗所得產品的平均錶麵張力為18.417 mN·m?1,與理論預測值基本相符。測試瞭產物NTS 0.1%(質量分數)的水溶液在pH為4、7和10的水溶液中的水解性能,髮現該產物在痠性和堿性條件下可穩定存放30 d左右,在中性條件下可穩定存放60 d左右。
선용EO(배양을완ethylene oxide)련장위7~8,평균상대분자질량위380적희병순취양완간기미(PE-38)화1,1,1,3,5,5,5-칠갑기삼규양완(MDHM)위원료,통과무용제취합,재담기보호하경Karstedt최화제최화규경가성반응제비료비리자형취미개성삼규양완표면활성제(NTS),병통과부리협홍외광보의화질자핵자공진의험증료기결구。채용향응면법대합성공예진행료우화,학정료 NTS 적최가합성조건위:n(C C):n(Si—H)=0.93,반응온도위94℃,최화제용량위6.4 mg·kg?1,재반응시간위2 h하,경3차중복시험소득산품적평균표면장력위18.417 mN·m?1,여이론예측치기본상부。측시료산물NTS 0.1%(질량분수)적수용액재pH위4、7화10적수용액중적수해성능,발현해산물재산성화감성조건하가은정존방30 d좌우,재중성조건하가은정존방60 d좌우。
Synthesis of non-ionic polyether modified trisiloxanes surfactant (NTS) from MDHM and polyoxyethylene alkyl allyl ethers (PE-38) with average EO (ethylene oxide) chain length of 7—8 and average molecular weight of 380, was catalyzed by Karstedt catalyst under N2 with no solvent. Its structure was verified by Fourier transform infrared spectroscopy and proton nuclear magnetic resonance. Synthesis of NTS was optimized by using the response surface methodology (RSM). The optimal conditions at which average surface tension (18.417 mN·m?1) repeated three times was obtained, being in agreement with the predicted value (18.177 mN·m?1), were as follows:reaction mass ratio of n(C C):n(Si—H)=0.93, amount of catalyst 6.4 mg·kg?1, and reaction temperature and time 94℃ and 2 h, respectively. Hydrolysis of the aqueous solution of NTS at pH 4, 7 and 10 also was studied, and the product under acidic and alkaline conditions was stable for about 30 d, while under neutral condition was stable for about 60 d.