CN108276437B - 一种低泡润湿剂及其制备方法 - Google Patents
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Abstract
本发明公开了一种低泡润湿剂及其制备方法，它是由聚醚改性硅油马来酸酯依次经酯化、磺化得到，该低泡润湿剂的结构中引入了聚醚改性硅油侧链、磺酸根和羧酸根，具有低泡和消泡性能，能够降低水体系的表面张力，使体系具有较低的表面张力，使体系泡沫少，能够很好的分散于水中，便于生产和使用；本发明可以应用在农药可湿性粉剂、悬浮剂、水分散粒剂等制剂中。本发明适用于制备低泡润湿剂。
Description
技术领域
本发明属于高分子合成领域，具体涉及一种低泡润湿剂及其制备方法。
背景技术
润湿剂是一种能使固体物料更易被水浸湿的一种物质，主要是用来降低物质的表面张力，使水能够展开在固体物料表面上或透入其表面而将其润湿，以提高所要分散的物质的分散性能。现有的润湿剂主要是有机硅类润湿剂，是目前效果较好的使用范围较广的一类，但是，这种润湿剂起泡性较高，动态表面张力较高，给高速研磨分散或应用造成稳泡的负面作用。因此，因此，亟需开发一种倾点低、适用于低温季节使用的润湿剂。一种低泡沫的润湿剂。
发明内容
本发明的目的是，旨提供一种低泡润湿剂，以解决砂磨过程中的润湿和泡沫高等问题；
本发明的另外一个目的，是提供了上述低泡润湿剂的制备方法，过程简单，易于控制，制备周期短，适用于工业化生产中。
为实现上述目的，本发明的技术方案为：
一种低泡润湿剂，它的结构式如下：
式中，m是0～10的整数，例如，m可以为0、1、2、3、4、5、6、7、8、9或10；n是3～53的整数，例如，n可以为3、4、5、6、7、8、9、10、11、12、13、14、15、16、17、18、19、20、21、22、23、24、25、26、27、28、29、30、31、32、33、34、35、36、37、38、39、40、41、42、43、44、45、46、47、48、49、50、51、52或53；x为1～18的整数，例如1、2、3、4、5、6、7、8、9、10、11、12、13、14、15、16、17或18；y为碳数为1～18的直链醇、支链醇发生酯化反应后剩余H的个数。
本发明还提供了上述低泡润湿剂的制备方法，它是由聚醚改性硅油马来酸酯依次经酯化、磺化得到。
作为本发明制备方法的一种限定，所述聚醚改性硅油马来酸酯的分子量为500～3500。
作为本发明制备方法的进一步限定：
所述聚醚改性硅油马来酸酯的制备方法按照如下的步骤顺序依次进行：
在装有甲苯的四口烧瓶中，加入摩尔比为1：1.2的聚醚改性硅油和马来酸酐，待全部溶解后，于30℃～60℃下搅拌反应3～10h，停止加热，除去甲苯和残余的马来酸酐，降温出料，得到液体产物；
在此步骤中，所述的聚醚改性硅油为市场上现有化合物，也可以参照《聚醚改性硅油的制备及其在棉织物舒适性整理中的应用》(任新华等,浙江理工大学学报,26(2),2009:189-194.)进行合成，即0.16％～0.18％含氢硅油与烯丙基聚醚，在催化剂的作用下，通过加成反应而成。
所述低泡润湿剂按照如下的步骤顺序依次进行：
(1)在反应器中，加入聚醚改性硅油马来酸酯、酯化剂、酯化催化剂及酯化带水剂，其中：聚醚改性硅油马来酸酯、酯化剂及酯化带水剂的摩尔比为1：1～1.2：1～1.2；聚醚改性硅油马来酸酯与酯化催化剂的质量比为1:0.01～0.05，升温至100～150℃，反应3～24h；
(2)在上述反应物中加入亚硫酸氢钠、乙醇、快T和水，搅拌加热至90～100℃，其中：聚醚改性硅油马来酸酯与亚硫酸氢钠的摩尔比为1：1～1.5，聚醚改性硅油马来酸酯、乙醇、快T和水的质量比为1：0.05～0.15：0.01～0.1：0.05～0.15，反应3～24h，得最终的低泡润湿剂。在本发明的低泡润湿剂的制备过程中，酯化反应和磺化反应的控制是非常关键的，具体为酯化剂种类和磺化剂种类的选择、以及酯化剂和磺化剂比例的选择。作为本发明制备方法的更进一步限定：
所述的酯化剂为碳数1～18的直链醇、支链醇，例如为乙醇、丙醇或戊醇；
所述的酯化带水剂为甲苯。
所述的酯化催化剂为浓硫酸、氨基磺酸、甲苯磺酸中的一种。
与现有技术相比，本发明的低泡润湿剂具有以下优点：
(1)本发明的低泡润湿剂由于引入了聚醚改性硅油侧链，具有低泡和消泡性能，使体系泡沫少，便于生产和使用；
(2)本发明的低泡润湿剂由于引入了聚醚改性硅油侧链，能够降低水体系的表面张力，使体系具有较低的表面张力，润湿性能好；
(3)本发明的低泡润湿剂由于引入了磺酸根和羧酸根，能够很好的分散于水中；
(4)本发明的低泡润湿剂由于引入了聚醚改性硅油侧链，具有一定的乳化性，制备的悬浮剂入水呈雾状分散，分散均匀；
(5)由于本发明的低泡润湿剂，可以应用在农药可湿性粉剂、悬浮剂、水分散粒剂等制剂中。
本发明制备的低泡润湿剂，配成1000mg/L的溶液，其表面张力可低至19.5mN/m；在35％吡虫啉WP中的应用中，悬浮率可达97.1％；在50％莠去津SC中的应用中本发明低泡润湿剂能够砂磨正常，物料稀；具有一定的乳化性能，入水成雾状分散，具有较好的低泡和消泡性能。
具体实施方式
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，进一步阐述本发明。除无特殊说明，下述实施例中的“％”代表“质量分数”。
实施例1一种低泡润湿剂的制备方法
本实施例为一种低泡润湿剂的制备方法，它为聚醚改性硅油马来酸酯依次经酯化、磺化得到，具体按照如下的步骤顺序依次进行：
(1Ⅰ)聚醚改性硅油马来酸酯的制备
在装有甲苯的四口烧瓶中，加入摩尔比为1：1.2的聚醚改性硅油和马来酸酐，待全部溶解后，于30℃下搅拌反应10h，停止加热，除去甲苯和残余的马来酸酐，降温出料，得到液体产物聚醚改性硅油马来酸酯，它的分子量为500～3500；
(1Ⅱ)低泡润湿剂的制备
(11)在反应器中，加入上步制备的聚醚改性硅油马来酸酯、丙醇、浓硫酸及甲苯，其中：聚醚改性硅油马来酸酯、丙醇及甲苯的摩尔比为1：1：：1，聚醚改性硅油马来酸酯与浓硫酸的质量比为1:0.03，升温至1300℃，反应10h；
(12)在步骤(11)所得反应物中加入亚硫酸氢钠、乙醇、快T和水，搅拌加热至100℃，其中：聚醚改性硅油马来酸酯与亚硫酸氢钠的摩尔比为1:1.2、聚醚改性硅油马来酸酯、乙醇、快T和水的质量比为1：0.1:0.05：0.1，反应24h，得最终的低泡润湿剂，它的结构式符合如下通式：
实施例2-5低泡润湿剂的制备方法
实施例2-5分别为一种低泡润湿剂的制备方法，过程与实施例1相似，不同之处仅在于，制备过程中相应的参数不同，具体如下：
本实施例所制备的低泡润湿剂，它的结构式符合如下通式
实施例6对比试验
为了更好的评价本发明实施例1-5所制备的低泡润湿剂的性能，做以下测试：
对比例1润湿剂为JFC；
对比例2的润湿剂为十二烷基苯磺酸钠；
对比例3的润湿剂为十二烷基硫酸钠；对比例4的润湿剂为NP-10；
对比例5的润湿剂为本发明实施例1-5所提供的润湿剂。
1.起泡性试验
选择润湿剂与常见的润湿剂AOS混合，取0.07g放入盛有250mL标准硬水的量筒中，按GB/T 28137-2011农药持久起泡性测试方法进行测试，结果如下：
| 组别 | 泡沫/mL |
| 对比例1 | 50 |
| 对比例2 | 40 |
| 对比例3 | 50 |
| 对比例4 | 50 |
| 对比例5 | 0 |
可见，本发明低泡润湿剂具有很好的低泡和消泡性能。
2.润湿性能测试
将对比例1-对比例5中的润湿剂配成1000mg/L的溶液，用表面张力仪进行测试静态表面张力，结果如下：
| 组别 | 表面张力/(mN/m) |
| 对比例1 | 40.1 |
| 对比例2 | 38.5 |
| 对比例3 | 41.0 |
| 对比例4 | 35.6 |
| 对比例5 | 19.5 |
可见，本发明低泡润湿剂具有很好的降低表面张力性能，具有很好的润湿性。
3.在农药制剂配方中的应用试验
(1)在35％吡虫啉WP中的应用
由于本发明合成的低泡润湿剂具有润湿性能，在对比例5中加入本发明实施例1-5制备的润湿剂，配方为：97％吡虫啉TC 36.1％，润湿剂5％，硫酸钠20％，高岭土补足至100％。
在对比例1-对比例4与对比例5中所加的原料相同，不同之处仅在于：润湿剂种类不同，评价结果如下：
| 润湿剂 | 入水状态 | 持久起泡性/mL | 悬浮率/％ |
| 对比例1 | 润湿差，块状下沉 | 0 | 69.1 |
| 对比例2 | 润湿差，块状下沉 | 0 | 70.1 |
| 对比例3 | 润湿差，块状下沉 | 0 | 71.5 |
| 对比例4 | 润湿差，块状下沉 | 0 | 70 |
| 对比例5 | 云雾状均匀分散 | 0 | 97.1 |
| 对比例1+AOS | 润湿一般，小块状下沉 | 50 | 72.5 |
| 对比例2+AOS | 润湿一般，小块状下沉 | 50 | 72.8 |
| 对比例3+AOS | 润湿一般，小块状下沉 | 50 | 73.5 |
| 对比例4+AOS | 润湿一般，小块状下沉 | 50 | 71.5 |
可见，本发明的低泡润湿剂使制剂能够均匀的润湿分散，而且分散悬浮性能好，具有较好的低泡和消泡性能。
(2)在50％莠去津SC中的应用
由于合成的低泡润湿剂具有润湿性能，在对比例5配方中加入本发明实施例制备的润湿剂，评价配方为：97％莠去津TC 51.6％，润湿剂5％，尿素4％，黄原胶0.16％，水补足至100％。
另外，在对比例1-对比例4与对比例5中所加的原料相同，不同之处仅在于：润湿剂种类不同，评价结果如下：
可见，本发明的低泡润湿剂能够砂磨正常，物料稀；具有一定的乳化性能，入水成雾状分散，具有较好的低泡和消泡性能。
Claims (4)
1.一种低泡润湿剂，其特征在于它的结构式如下：
式中，m是0～10的整数，n是3～53的整数，x为1～18的整数，y为碳数为1～18的直链醇、支链醇发生酯化反应后剩余H的个数；所述聚醚改性硅油马来酸酯的分子量为500～3500；它是由聚醚改性硅油马来酸酯依次经酯化、磺化得到；
制备方法按照如下的步骤顺序依次进行：
(1)在反应器中，加入聚醚改性硅油马来酸酯、酯化剂、酯化催化剂及酯化带水剂，其中：聚醚改性硅油马来酸酯、酯化剂及酯化带水剂的摩尔比为1：1～1.2：1～1.2；聚醚改性硅油马来酸酯与酯化催化剂的质量比为1:0.01～0.05，升温至100～150℃，反应3～24h；
(2)在上述反应物中加入亚硫酸氢钠、乙醇、快T和水，搅拌加热至90～100℃，其中：聚醚改性硅油马来酸酯与亚硫酸氢钠的摩尔比为1：1～1.5，聚醚改性硅油马来酸酯、乙醇、快T和水的质量比为1：0.05～0.15：0.01～0.1：0.05～0.15，反应3～24h，得最终的低泡润湿剂；
酯化催化剂为浓硫酸、氨基磺酸、甲苯磺酸中的一种。
2.根据权利要求1所述的低泡润湿剂，其特征在于：所述聚醚改性硅油马来酸酯的制备方法按照如下的步骤顺序依次进行：
在装有甲苯的四口烧瓶中，加入摩尔比为1：1.2的聚醚改性硅油和马来酸酐，待全部溶解后，于30～60℃下搅拌反应3～10h，停止加热，除去甲苯和残余的马来酸酐，降温出料，得到液体产物。
3.根据权利要求1所述的低泡润湿剂，其特征在于：所述的酯化剂为碳数1～18的直链醇或支链醇。
4.根据权利要求1所述的低泡润湿剂，其特征在于：所述的酯化带水剂为甲苯。
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