CN102505497B - 高耐久自洁防污pu流平剂的制备方法 - Google Patents
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Abstract
本发明公开了一种高耐久自洁防污PU流平剂的制备方法，包括以下步骤：(1)在干燥清洁的反应釜中加入计量的氨基硅烷偶联剂、酰化改性剂以及催化剂，升温反应1~3h，得到改性的氨基硅油乳液；(2)称取配比量的有机溶剂N,N-二甲基甲酰胺、MDI以及催化剂二月桂酸二异丁基锡，置于另一充满氮气的反应器中，搅拌下加热溶解，并往该溶液中缓慢滴加改性的氨基硅油乳液，控温反应1~5h得到预聚产物；(3)在获得的预聚产物中依次加入封端剂、中和剂后，再加入防霉剂、抗氧剂、紫外吸收剂，得到复配产品。本发明所获得高耐久自洁防污PU流平剂，具有优良交联固着性，以及耐久性，防污自洁性好，协同效果好。
Description
技术领域：
本发明涉及一种高耐久自洁防污PU流平剂，特别涉及高耐久自洁防污PU流平剂的制备方法。
背景技术：
流平剂在PU表面能形成单分子层，以提供均一的表面张力，以相容性受限制的长链硅材为主要组成。作用是改善基布表面的平整性，增加树脂与基布问的亲合性。常用的有二苯基聚硅氧烷、甲基苯基聚硅氧烷、聚醚改性硅氧烷、氟化硅氧烷等。随着功能性的强化，单组分单功能的PU助剂已经跟不上形势的发展。有机硅改性聚氨酯类高分子材料不仅具有聚氨酯材料的优异性能，还具有有机硅的各种特点。目前，国产皮革助剂在品种和质量以及在合成和应用技术方面与国际先进水平相比还有较大差距，专用和高档皮革助剂尚不得不依赖进口。特别是想让皮革具有例如高耐久、防污自洁等特殊特性能，则必须制备合适的皮革助剂。
发明内容：
发明目的：针对现有技术存在的缺陷，本发明提供了一种高耐久自洁防污PU流平剂的制备方法。
技术方案：为实现上述发明目的，本发明采用以下技术方案：
一种高耐久自洁防污PU流平剂的制备方法，包括以下步骤：(1)、在干燥清洁的反应釜中加入计量的氨基硅烷偶联剂、酰化改性剂以及催化剂浓硫酸，升温至40~60℃反应1~3h，得到改性的氨基硅油乳液；(2)、称取配比量的有机溶剂N,N-二甲基甲酰胺和4,4’-二苯甲烷二异氰酸酯MDI、催化剂量的二月桂酸二异丁基锡，并有机溶剂N,N-二甲基甲酰胺、二月桂酸二异丁基锡以及MDI依次加入另一充满氮气的反应器中，搅拌下加热溶解后，往该溶液中缓慢滴加改性的氨基硅油乳液，在60~85℃下控温反应1~5h即可得到预聚产物；(3)、在步骤(2)获得的预聚产物中加入由摩尔比为1-1.05:1的乙二醇乙醚和二乙醇胺复配的封端剂，继续在60~85℃下保温反应1~2h，得到封端的聚氨酯；(4)、加入乙醇酸中和剂，调节PH=6~8，得改性的有机硅聚氨酯产品；(5)、加入防霉剂、抗氧剂、紫外吸收剂，得到复配产品。
所述氨基硅烷偶联剂为KH-550；酰化改性剂为聚己内酯二元醇。
根据以上的技术方案，可以实现以下的有益效果：与现有技术相比，本发明具有以下优点：本发明所获得高耐久自洁防污PU流平剂，具有优良交联固着性，以及耐久性，防污自洁性好，协同效果好。
具体实施方式：
下面结合实施例对本发明做进一步地详细说明，但是本发明要求保护的范围并不局限于实施例表示的范围。
实施例1：
在干燥，清洁的反应釜中依次加入计算量的氨基硅烷偶联剂KH-550(1.0kmol)， 聚己内酯二元醇(1.1kmol)，催化剂量的浓硫酸（10.0ml），升温至40~60℃，反应1~3h，得到酰化改性的氨基硅油乳液，待用。
在另一干燥，清洁的反应釜中加入有机溶剂N,N-二甲基甲酰胺（100.0kg）和4,4’-二苯甲烷二异氰酸酯（300.0kg），催化剂二月桂酸二异丁基锡(1.8kg)，升温至40~60℃，高速搅拌，将上述酰化改性的氨基硅油乳液缓慢滴加入反应釜中，控制温度在60~85℃，滴毕，保温反应1~5h，向反应产物中加入封端剂乙二醇乙醚(1.0mol)和二乙醇胺(0.1mol)，保温反应1~2h，降温至60℃，加入乙醇酸中和剂，调节PH=7.0得改性的有机硅聚氨酯产品，再向反应物中加入防霉剂（8.5kg）、抗氧剂(10.0kg)、紫外吸收剂(10.5kg)，搅拌30分钟，得到复配产品。
Claims (1)
1.一种高耐久自洁防污PU流平剂的制备方法，其特征在于，包括以下步骤：(1)、在干燥清洁的反应釜中加入计量的氨基硅烷偶联剂、酰化改性剂以及催化剂浓硫酸，升温至40~60℃反应1~3h，得到改性的氨基硅油乳液；(2)、称取配比量的有机溶剂N,N-二甲基甲酰胺和4,4’-二苯甲烷二异氰酸酯MDI、催化剂量的二月桂酸二异丁基锡，并有机溶剂N,N-二甲基甲酰胺、二月桂酸二异丁基锡以及MDI依次加入另一充满氮气的反应器中，搅拌下加热溶解后，往该溶液中缓慢滴加改性的氨基硅油乳液，在60~85℃下控温反应1~5h即可得到预聚产物；(3)、在步骤(2)获得的预聚产物中加入由摩尔比为1-1.05:1的乙二醇乙醚和二乙醇胺复配的封端剂，继续在60~85℃下保温反应1~2h，得到封端的聚氨酯；(4)、加入乙醇酸中和剂，调节pH=6~8，得改性的有机硅聚氨酯产品；(5)、加入防霉剂、抗氧剂、紫外吸收剂，得到复配产品；所述氨基硅烷偶联剂为KH-550；酰化改性剂为聚己内酯二元醇。
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| CN1704523A (zh) * | 2004-05-27 | 2005-12-07 | 香港理工大学 | 反应型水性聚氨酯织物整理剂，其制备方法及应用 |
| CN101003945A (zh) * | 2006-01-18 | 2007-07-25 | 丹东恒星精细化工有限公司 | 热解闭聚氨酯抗皱整理剂及生产方法 |
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| CN1704523A (zh) * | 2004-05-27 | 2005-12-07 | 香港理工大学 | 反应型水性聚氨酯织物整理剂，其制备方法及应用 |
| CN101003945A (zh) * | 2006-01-18 | 2007-07-25 | 丹东恒星精细化工有限公司 | 热解闭聚氨酯抗皱整理剂及生产方法 |
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| Title |
|---|
| JP昭57-38813A 1982.03.03 |
| 康礼道等.硅烷偶联剂在密封胶中的应用.《化工进展》.2007,第24卷(第3期), |
| 硅烷偶联剂在密封胶中的应用;康礼道等;《化工进展》;20070430;第24卷(第3期);第260页-264页 * |
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Effective date of registration: 20141204 Address after: Song Ling Zhen Wujiang District of Suzhou City, Jiangsu province 215200 Suzhou River Road No. 18 Patentee after: Suzhou Xielv Network Technology Co., Ltd. Address before: 215200, Changan Road, Wujiang economic and Technological Development Zone, Jiangsu, Suzhou province (Science and Technology Pioneer Park) Patentee before: SUZHOU FANGYOU NEW MATERIAL CO., LTD. |
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Address after: 215200 Shengze, Jiangsu, China Town, Shengze, West No. two ring road, No. 1188, China Textile Science and Technology Park, Wujiang, building 10 Patentee after: Suzhou Xielv Network Technology Co., Ltd. Address before: Song Ling Zhen Wujiang District of Suzhou City, Jiangsu province 215200 Suzhou River Road No. 18 Patentee before: Suzhou Xielv Network Technology Co., Ltd. |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
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Granted publication date: 20130918 Termination date: 20171101 |