CN113788959A - 一种有机硅乳液的制备方法 - Google Patents
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Abstract
本发明公开了一种有机硅乳液的制备方法，包括以下步骤：a、将二甲基硅氧烷混合环体、封头剂、羧基硅烷偶联剂及催化剂在容器中混合缩聚，缩聚反应得到缩聚反应产物；b、将步骤a得到的缩聚产物进行减压蒸馏，质量恒定后结束蒸馏，降温得到羧基硅油原油；c、将步骤b得到的羧基硅油、乳化剂和水加入容器中，搅拌乳化，得到透明的羧基硅油乳液。本发明制备得到的应用于合成革人造革表面的水性有机硅乳液，与人造革表面附着力好，揉纹后手感保持度高；且制备工艺简单，制得的乳液粒径细，印刷过程中不漂油，稳定性好。
Description
本申请是申请日为2018年12月28日，申请号为2018116229752，发明名称为“用于合成革人造革表面滑爽处理的有机硅乳液及其制备方法”的分案申请。
技术领域
本发明涉及有机硅乳液及其制备方法，特别是涉及一种用于合成革人造革表面滑爽处理的有机硅乳液及其制备方法。
背景技术
目前大多采用羟基硅油、甲基硅油及氨基硅油乳液作为滑爽处理的表面处理剂，但是其主要缺陷在于：
(1)羟基、甲基硅油乳液粒径大，印刷性差；
(2)现有羟基硅油，甲基硅油及氨基硅油在印刷过程中由于刀片与辊筒的挤压会导致破乳，使最终的成品革面出现油斑；
(3)羟基硅油、甲基硅油乳液对皮革的附着力差，手感保持度弱。
因此，研发出一种制备工艺简单、印刷性好，附着力好的有机硅乳液对合成革人造革表面处理具有重要的意义。
发明内容
为了解决现有技术存在的问题，本发明提供了一种用于合成革人造革表面滑爽处理的有机硅乳液及其制备方法，以提高表面处理剂的印刷性以及附着力和稳定性。
为实现上述目的，本发明采取的技术方案是一种用于合成革人造革表面滑爽处理的有机硅乳液：
包括以下质量比的各组分：
羧基硅油原油：乳化剂：水为30-35：2-8：50-65；
其中，所述羧基硅油原油由以下重量份的各组分组成：
于本发明一实施例中，所述羧基硅烷偶联剂的结构式为Si-PEG-COOH。
于本发明一实施例中，所述羧基硅烷偶联剂的具体结构为(OMe)3Si(CH2)2NHCONH(CH2)2(EO)mCOOH或(OEt)3Si(CH2)2NHCONH(CH2)2(EO)mCOOH，其中m≥3。
于本发明一实施例中，所述封头剂为六甲基二硅氧烷。
于本发明一实施例中，所述催化剂为酸性阳离子交换树脂。
于本发明一实施例中，所述乳化剂为脂肪醇聚氧乙烯醚。
一种有机硅乳液的制备方法，其特征在于，包括以下步骤：
a、将二甲基硅氧烷混合环体、封头剂、羧基硅烷偶联剂及酸性阳离子交换树脂在容器中混合缩聚，缩聚反应得到缩聚反应产物；
b、将步骤a得到的缩聚产物进行减压蒸馏，质量恒定后结束蒸馏，降温得到羧基硅油原油；
c、将步骤b得到的羧基硅油、乳化剂和水加入容器中，搅拌乳化，得到透明的羧基硅油乳液。
于本发明一实施例中，步骤c中的搅拌为在常温下进行的机械搅拌。
于本发明一实施例中，缩聚的反应温度为100-200℃。
本技术方案具有以下有益效果：
本发明合成了一种羧基硅油乳液，先将羧基硅烷偶联剂，二甲基硅氧烷混合环体以及封头剂及催化剂在一定温度下进行缩聚反应，得到侧链为羧基的羧基硅油，再将该羧基硅油通过乳化剂乳化，得到本发明的羧基硅油乳液。本发明解决羟基硅油和甲基硅油通过大量乳化剂乳化复配所造成的不稳定性问题，得到的羧基硅油乳液稳定性好，附着力强，且粒径小，印刷性好，印刷过程中不产生油斑。
具体实施方式
下面结合实施例对本发明作进一步描述。
实施例1
羧基硅油原油制备：
将八甲基环四硅氧烷、六甲基二硅氧烷、羧基硅烷偶联剂及酸性阳离子交换树脂在容器中混合缩聚，其质量比分别为4000:15:250:1，缩聚的反应温度为120℃，反应时间4小时。经减压蒸馏后得到所需要的羧基硅油原油。本实施例中，所采用的羧基硅烷偶联剂的通式为Si-PEG-COOH，具体为(OMe)3Si(CH2)2NHCONH(CH2)2(EO)mCOOH，其中m≥3。
羧基硅油乳液制备：
将制备的羧基硅油原油、脂肪醇聚氧乙烯醚和水加入容器中，其质量比分别为32:4:64，常温下进行机械搅拌乳化，搅拌速度为1000r/min,搅拌时间为1小时，得到透明稳定的羧基硅油乳液，记乳液1。
应用测试：
将该羧基硅油乳液进行以下性能测试：(1)离心稳定性测试，测试条件为转速3000r/min，时间为30min；(2)印刷性测试，测试条件为300目辊筒印刷，时间为30min，观察刀口是否有油状物
(3)手感评估测试，测试条件为在合成革表面300目印刷该乳液，温度80℃干揉30分钟。测试结果：乳液1离心不分层，且印刷刀口无油斑，革面手感丰满油润感强。
实施例2
羧基硅油原油制备：
将八甲基环四硅氧烷、六甲基二硅氧烷、羧基硅烷偶联剂及酸性阳离子交换树脂在容器中混合缩聚，其质量比分别为3500:20:250:1，缩聚的反应温度为120℃，反应时间4小时。经减压蒸馏后得到所需要的羧基硅油原油。本实施例中，所采用的羧基硅烷偶联剂的通式为Si-PEG-COOH，具体为(OMe)3Si(CH2)2NHCONH(CH2)2(EO)mCOOH，其中m≥3。
羧基硅油乳液制备：
将制备的羧基硅油原油、脂肪醇聚氧乙烯醚和水加入容器中，其质量比分别为33:3:64，常温下进行机械搅拌乳化，搅拌速度为1000r/min,搅拌时间为1小时，得到透明稳定的羧基硅油乳液，记乳液2。
应用测试：
将该羧基硅油乳液进行以下性能测试：(1)离心稳定性测试，测试条件为转速3000r/min，时间为30min；(2)印刷性测试，测试条件为300目辊筒印刷，时间为30min，观察刀口是否有油状物
(3)手感评估测试，测试条件为在合成革表面300目印刷该乳液，温度80℃干揉30分钟。测试结果：乳液2离心不分层，且印刷刀口无油斑，但由于封头剂过多导致合成的羧基硅油分子量较低，因此革面手感比乳液1差，油润感不足。
实施例3
羧基硅油原油制备：
将八甲基环四硅氧烷、六甲基硅氧烷、羧基硅烷偶联剂及酸性阳离子交换树脂在容器中混合缩聚，其质量比分别为4500:10:150:1，缩聚的反应温度为120℃，反应时间4小时。经减压蒸馏后得到所需要的羧基硅油原油。本实施例中，所采用的羧基硅烷偶联剂的通式为Si-PEG-COOH，具体为(OEt)3Si(CH2)2NHCONH(CH2)2(EO)mCOOH，其中m≥3。
羧基硅油乳液制备：
将制备的羧基硅油原油、脂肪醇聚氧乙烯醚和水加入容器中，其质量比分别为35:7:58，常温下进行机械搅拌乳化，搅拌速度为1000r/min，搅拌时间为1小时，得到半透明稳定的羧基硅油乳液，记乳液3。
应用测试：
将该羧基硅油乳液进行以下性能测试：(1)离心稳定性测试，测试条件为转速3000r/min，时间为30min；(2)印刷性测试，测试条件为300目辊筒印刷，时间为30min，观察刀口是否有油状物
(3)手感评估测试，测试条件为在合成革表面300目印刷该乳液，温度80℃干揉30分钟。测试结果：乳液3离心有少量分层，离心稳定性差，这可能与羧基硅油合成时羧基硅烷偶联剂含量少，导致该硅油不易乳化。同时，印刷刀口有少量油斑析出，手感也有些油腻。
对比例
甲基硅油乳液制备：
将市售的甲基硅油粘度为5000cps、脂肪醇聚氧乙烯醚和水加入容器中，其质量比分别为35:7:58，常温下进行机械搅拌乳化，搅拌速度为1000r/min，搅拌时间为1小时，得到乳白色的甲基硅油乳液，记乳液4。
应用测试：
将甲基硅油乳液进行以下性能测试：(1)离心稳定性测试，测试条件为转速3000r/min，时间为30min；(2)印刷性测试，测试条件为300目辊筒印刷，时间为30min，观察刀口是否有油状物
(3)手感评估测试，测试条件为在合成革表面300目印刷该乳液，温度80℃干揉30分钟。测试结果：乳液4离心分层严重，离心稳定性差，印刷5分钟后刀口有大量油斑析出，用乳液4在合成革表面印刷，手感非常油腻，不舒服。
本发明创新性的选用羧基硅烷偶联剂、采用本体聚合法制备羧基硅油，与目前现有的羧基硅油制备方法相比，具有生产工艺简单，副反应少的优点。且羧基硅油中含有聚醚键，提高了亲水性，使乳化的硅油乳液更加稳定；乳液粒径细，印刷过程中不漂油。同时，与人造革表面附着力好，揉纹后手感保持度高。通过上述实施例和对比例也看出，本发明所制备的有机硅乳液稳定性有了很大提高，因此在工业应用中会具有更强的适用性。
上述具体实施例只是用来解释说明本发明，而非是对本发明进行限制，在本发明的宗旨和权利要求的保护范围内，对本发明做出的任何不付出创造性劳动的替换和改变，皆落入本发明专利的保护范围。
Claims (10)
1.一种有机硅乳液的制备方法，其特征在于，所述有机硅乳液用于合成革人造革表面滑爽处理，包括以下步骤：
a、将二甲基硅氧烷混合环体、封头剂、羧基硅烷偶联剂及催化剂在容器中混合缩聚，缩聚反应得到缩聚反应产物；
b、将步骤a得到的缩聚产物进行减压蒸馏，质量恒定后结束蒸馏，降温得到羧基硅油原油；
c、将步骤b得到的羧基硅油、乳化剂和水加入容器中，搅拌乳化，得到透明的羧基硅油乳液。
2.根据权利要求1所述的有机硅乳液的制备方法，其特征在于，步骤c中的搅拌为在常温下进行的机械搅拌。
3.根据权利要求1所述的有机硅乳液的制备方法，其特征在于，缩聚的反应温度为100-200℃。
4.根据权利要求1所述的有机硅乳液的制备方法，其特征在于，缩聚反应的时间为3.5-4.5h。
5.根据权利要求1所述的有机硅乳液的制备方法，其特征在于，步骤a中,各组分按照重量份数计分别为:二甲基硅氧烷混合环体3500-4500份，封头剂10-20份，羧基硅烷偶联剂150-280份和催化剂0.1-2份。
6.根据权利要求1或5所述的有机硅乳液的制备方法，其特征在于，其特征在于，所述羧基硅烷偶联剂的通式为Si-PEG-COOH。
7.根据权利要求6所述的有机硅乳液的制备方法，其特征在于，其特征在于，所述羧基硅烷偶联剂的具体结构为(OMe)3Si(CH2)2NHCONH(CH2)2(EO)mCOOH或(OEt)3Si(CH2)2NHCONH(CH2)2(EO)mCOOH，其中m≥3。
8.根据权利要求1或5所述的有机硅乳液的制备方法，其特征在于，其特征在于，所述封头剂为六甲基二硅氧烷。
9.根据权利要求1或5所述的有机硅乳液的制备方法，其特征在于，其特征在于，所述催化剂为酸性阳离子交换树脂。
10.根据权利要求1或5所述的有机硅乳液的制备方法，其特征在于，其特征在于，所述乳化剂为脂肪醇聚氧乙烯醚。
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