化工学报 ›› 2021, Vol. 72 ›› Issue (5): 2837-2848.DOI: 10.11949/0438-1157.20201235
程文静1(),余林1(),程高1,钟远红1,郑成2,毛桃嫣2
收稿日期:
2020-08-28
修回日期:
2020-12-28
出版日期:
2021-05-05
发布日期:
2021-05-05
通讯作者:
余林
作者简介:
程文静(1984—),女,博士研究生,基金资助:
CHENG Wenjing1(),YU Lin1(),CHENG Gao1,ZHONG Yuanhong1,ZHENG Cheng2,MAO Taoyan2
Received:
2020-08-28
Revised:
2020-12-28
Online:
2021-05-05
Published:
2021-05-05
Contact:
YU Lin
摘要:
以1,3-二(3-缩水甘油醚丙基)-1,1,3,3-四甲基二硅氧烷(EDH)和八甲基环四硅氧烷(D4)为原料合成了端环氧硅油(ETSO),以ETSO为原料与葡甲胺胺化得到中间体有机硅嵌段硅油(PTSO),然后用γ-氯丙基三甲氧基硅烷(CPTSO)季铵化改性制备了Bola有机硅季铵盐(BPTSO)。BPTSO的季铵化过程最优合成工艺条件为:反应温度为80℃,物料摩尔比为n(PTSO)∶n(CPTSO)=1∶1.2,反应时间为3 h,PTSO转化率达98.60%。通过FT-IR、1H NMR、TGA、TEM对BPTSO的结构及BPTSO乳液整理后织物的微观形貌进行了表征。测试结果表明:BPTSO乳液的表面张力γ 为29.4 mN/m,临界胶束浓度CMC为0.036 mmol/L,具有囊泡结构和优越的稳定性,经BPTSO乳液整理后的棉织物具有优异的柔软度、白度及亲水性,当BPTSO乳液的用量为60 g/L时,对棉织物的增深率可达到46.5%。
中图分类号:
程文静, 余林, 程高, 钟远红, 郑成, 毛桃嫣. 多羟基Bola有机硅季铵盐的合成、表征及其应用性能[J]. 化工学报, 2021, 72(5): 2837-2848.
CHENG Wenjing, YU Lin, CHENG Gao, ZHONG Yuanhong, ZHENG Cheng, MAO Taoyan. Synthesis characterization and application of Bola silicone quaternary ammonium salt[J]. CIESC Journal, 2021, 72(5): 2837-2848.
季铵化试剂 | 转化率/% |
---|---|
γ-氯丙基三甲氧基硅烷 | 97.6 |
硫酸二甲酯 | 95.5 |
硫酸二乙酯 | 76.3 |
氯化苄 | 92.1 |
三甲基氯化铵盐酸盐 | 95.2 |
表1 不同季铵化试剂对PTSO的转化率
Table 1 Conversion rates of PTSO with different quaternary ammonium reagents
季铵化试剂 | 转化率/% |
---|---|
γ-氯丙基三甲氧基硅烷 | 97.6 |
硫酸二甲酯 | 95.5 |
硫酸二乙酯 | 76.3 |
氯化苄 | 92.1 |
三甲基氯化铵盐酸盐 | 95.2 |
水平 | A(反应温度)/℃ | B(反应物摩尔比) | C(反应时间)/h |
---|---|---|---|
1 | 60 | 1∶1 | 2 |
2 | 70 | 1∶1.1 | 3 |
3 | 80 | 1∶1.2 | 4 |
表2 正交实验因素水平表
Table 2 Factors and levels of orthogonal experiments
水平 | A(反应温度)/℃ | B(反应物摩尔比) | C(反应时间)/h |
---|---|---|---|
1 | 60 | 1∶1 | 2 |
2 | 70 | 1∶1.1 | 3 |
3 | 80 | 1∶1.2 | 4 |
实验号 | A | B | C | 转化率/% |
---|---|---|---|---|
1 | 60 | 1∶1.0 | 2 | 96.11 |
2 | 60 | 1∶1.1 | 3 | 97.83 |
3 | 60 | 1∶1.2 | 4 | 96.72 |
4 | 70 | 1∶1.0 | 3 | 98.03 |
5 | 70 | 1∶1.1 | 4 | 96.74 |
6 | 70 | 1∶1.2 | 2 | 98.04 |
7 | 80 | 1∶1.0 | 4 | 98.27 |
8 | 80 | 1∶1.1 | 2 | 98.00 |
9 | 80 | 1∶1.2 | 3 | 98.22 |
K1 | 290.66 | 292.15 | 292.41 | — |
K2 | 292.81 | 292.57 | 294.08 | — |
K3 | 294.49 | 292.98 | 291.73 | — |
k1 | 96.89 | 97.47 | 97.38 | — |
k2 | 97.60 | 97.52 | 97.03 | — |
k3 | 97.16 | 97.66 | 97.24 | — |
极差R | 3.83 | 0.57 | 2.35 | — |
因素主次 | A>C>B | |||
最优方案 | A 80℃、B (1∶1.2),C 3 h | |||
重复实验 | 平均转化率98.60% |
表3 正交实验方案与结果
Table 3 Result of orthogonal experiments
实验号 | A | B | C | 转化率/% |
---|---|---|---|---|
1 | 60 | 1∶1.0 | 2 | 96.11 |
2 | 60 | 1∶1.1 | 3 | 97.83 |
3 | 60 | 1∶1.2 | 4 | 96.72 |
4 | 70 | 1∶1.0 | 3 | 98.03 |
5 | 70 | 1∶1.1 | 4 | 96.74 |
6 | 70 | 1∶1.2 | 2 | 98.04 |
7 | 80 | 1∶1.0 | 4 | 98.27 |
8 | 80 | 1∶1.1 | 2 | 98.00 |
9 | 80 | 1∶1.2 | 3 | 98.22 |
K1 | 290.66 | 292.15 | 292.41 | — |
K2 | 292.81 | 292.57 | 294.08 | — |
K3 | 294.49 | 292.98 | 291.73 | — |
k1 | 96.89 | 97.47 | 97.38 | — |
k2 | 97.60 | 97.52 | 97.03 | — |
k3 | 97.16 | 97.66 | 97.24 | — |
极差R | 3.83 | 0.57 | 2.35 | — |
因素主次 | A>C>B | |||
最优方案 | A 80℃、B (1∶1.2),C 3 h | |||
重复实验 | 平均转化率98.60% |
项目 | 指标 |
---|---|
含量/% | 15 |
成本(元/千克) | 6.35 |
用量(g/L) | 20 |
固色牢度 | 4.5级 |
摩擦牢度 | 4.5级 |
耐水洗效果 | 5级 |
手感 | 蓬松、软滑风格,5分 |
表4 BPTSO乳液放大产品指标
Table 4 Index of BPTSO emulsion after amplification
项目 | 指标 |
---|---|
含量/% | 15 |
成本(元/千克) | 6.35 |
用量(g/L) | 20 |
固色牢度 | 4.5级 |
摩擦牢度 | 4.5级 |
耐水洗效果 | 5级 |
手感 | 蓬松、软滑风格,5分 |
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