CN110746607B - 一种应用于氨纶纺丝油剂中的起到隔离和调节摩擦作用的助剂产品 - Google Patents
一种应用于氨纶纺丝油剂中的起到隔离和调节摩擦作用的助剂产品 Download PDFInfo
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Abstract
本发明公开了一种应用于氨纶纺丝油剂中的起到隔离和调节摩擦作用的助剂产品,涉及功能性有机硅材料技术领域,该助剂产品的结构为(A3SiO0.5)a(BMe2SiO0.5)b(CMe2SiO0.5)c(DMe2SiO0.5)d(Me2SiO)e(SiO2)f,其中,A指代甲基与羟基混合体结构,B指代长链烷基,C指代缩水甘油醚基,D指代聚醚基团,Me指代甲基。本发明提供的助剂通过在传统MQ硅树脂结构基础上引入二甲基硅氧烷链节、长链烷基链节、环氧烃基链节、聚醚链节并保留部分活性羟基,使之与氨纶纤维产生化学结合力,既提供持久相溶性、贮存稳定性又提供抗静电性和恰当解束张力。
Description
技术领域
本发明涉及功能性有机硅材料技术领域,具体涉及一种应用于氨纶纺丝油剂中的起到隔离和调节摩擦作用的助剂产品。
背景技术
中国氨纶纺丝行业,近年来以其迅猛的发展势头,一举成为全世界的产丝大国。而与之配套的高端氨纶纺丝用油剂,却一直是由日本“松本”、“竹本”、美国“高尔斯顿”油剂主宰。其原因主要是日、美油剂在产品质量、产量、性能方面一枝独秀。
而国产油剂在氨纶纤维上油后,一方面,纤维与纤维之间的隔离性不好,随着时间的推移,致使纤维之间发生化学反应型的粘连,而无法解束使用,浪费了大量氨纶丝。另一个方面,纤维之间的摩擦力太小,致纺丝松套,难以成型。轻则出现“轨道丝”、“凸肚丝”,重则出现乱丝致不可纺,针对市场上油剂存在的问题,本发明提供一种助剂产品用于复配生产氨纶纺丝油剂。
发明内容
本发明的目的在于提供一种应用于氨纶纺丝油剂中的起到隔离和调节摩擦作用的助剂产品,以解决上述技术问题。
一种应用于氨纶纺丝油剂中的起到隔离和调节摩擦作用的助剂产品,所述助剂产品的结构为(A3SiO0.5)a(BMe2SiO0.5)b(CMe2SiO0.5)c(DMe2SiO0.5)d(Me2SiO)e(SiO2)f,其中,A指代甲基与羟基混合体结构,B指代长链烷基,C指代缩水甘油醚基,D指代聚醚基团,Me指代甲基;其中,a、b、c、d、e、f表示链节数或聚合度,a为3-10,b为2-5,c为2-5,d为2-5,e为1-5,f为5-8。
其中,助剂产品制备过程如下:
步骤一、先将硅酸酯、二甲基硅氧烷四聚体和含氢双封头溶解于混合溶剂中,然后滴加盐酸作催化剂于70-80℃水解缩合30-90min合成硅树酯基础材料;
步骤二、分离步骤一中得到的含有硅树脂基础材料的混合液中的油相得到硅树脂粗制品,粗制品依次经过中和、过滤、洗涤和干燥得到硅树脂基础材料;
步骤三、将硅树脂基础材料、不饱和烯烃、烯丙基缩水甘油醚和不饱和聚醚按一定比例和顺序进行硅氢加成反应,最后分离溶剂及低沸物。
作为一种优选方案,上述步骤一中混合溶剂为水、醇类和苯类物质混合制备而成,上述醇类为乙醇或者丙醇,上述苯类物质为甲苯、乙苯或者对二甲苯中的一种。
作为一种优选方案,上述步骤一中硅酸酯、水、醇类、苯类、二甲基硅氧烷四聚体、含氢双封头和盐酸中有效成分质量比为35-42:10-13:9-11:8-10:8.5-9.2:4-7:2.2-2.8。
作为一种优选方案,上述步骤一中含氢双封头为四甲基二氢二硅氧烷。
作为一种优选方案,上述步骤一中硅酸酯为正硅酸甲酯。
作为一种优选方案,上述步骤二中采用氢氧化钠将过滤物质中和至中性,采用蒸馏水对过滤物质进行洗涤,上述步骤二中减压蒸除溶剂操作在150℃条件下进行,蒸至无液体蒸出即可。
作为一种优选方案,上述步骤二中减压蒸除溶剂操作在150℃条件下进行,蒸至无液体蒸出即可。
作为一种优选方案,上述步骤三中具体操作为采用二甲苯作为溶剂,依次将硅树脂基础材料、不饱和烯烃、烯丙基缩水甘油醚以及不饱和聚醚溶解于二甲苯中,采用高活性铂催化剂在常温下催化反应6-18h,制备得到粗制的氨纶油剂中间体
作为一种优选方案,上述二甲苯、硅树脂基础材料、不饱和烯烃、烯丙基缩水甘油醚和不饱和聚醚和铂催化剂质量比为9-11:18-22:1-3:1-3:1-3:1,其中,上述不饱和烯烃、烯丙基缩水甘油醚和不饱和聚醚质量比为1:1:1。。
作为一种优选方案,上述步骤三中分离溶剂及低沸物具体操作为硅氢加成反应结束后,在80-90℃下,压力为0.10-0.15Mpa下蒸馏溶剂和小分子醇。
本发明的有益效果:
1、通过在传统MQ硅树脂结构基础上引入二甲基硅氧烷链节、长链烷基链节、环氧烃基链节、聚醚链节并保留部分活性羟基,使之与氨纶纤维产生化学结合力,既提供持久相溶性、贮存稳定性又提供抗静电性和恰当解束张力。
2、在传统MQ硅树脂结构基础上,引入二甲基硅氧烷链节、长链烷基链节、环氧烃基链节、聚醚链节,保留活性羟基,通过调整M、D、Q之间的比例得到不同摩尔质量、密度、粘度、软化点、韧性、增粘性的产物,使硅树脂韧性调节成为可能。
3、通过在传统MQ硅树脂结构基础上引入长链烷基结构使中间体助剂与矿物油及其他助剂具有更好的的相溶性,从而体现在纤维上油在长时间贮存过程中,表面油剂不会游离分离而发生迁移,防止因表面油剂析出而导致氨纶丝不是丝饼变形就是粘连的情况出现。
4、通过在传统MQ硅树脂结构基础上引入环氧烃基有利于增加丝与丝间的抱合力,使丝饼不至于因长时间存放而变形和泛黄。
附图说明
图1为本发明结构流程示意图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例一
称量35mg正硅酸甲酯、10mg水、9mg乙醇、8mg甲苯、8.5mg二甲基硅氧烷四聚体、4mg四甲基二氢二硅氧烷和220mg质量分数为1%的盐酸备用;
将水、乙醇、甲苯混合溶解,制备成混合溶剂,然后将硅酸酯、二甲基硅氧烷四聚体和含氢双封头溶解于混合溶剂中,然后滴加加盐酸作催化剂于70℃水解缩合50min合成硅树脂基础材料;
过滤步骤一中得到的含有硅树脂基础材料的混合液中的油相,得到硅树脂粗制品,粗制品依次滴加质量分数为1%的氢氧化钠溶液中和至中性,然后再次过滤,对所得固体采用蒸馏水洗涤三次,每次5ml,然后将固体放在烘箱中,调整压力为1.5Mpa,调整温度为150℃进行加压蒸馏,蒸至无液体蒸出即可得到硅树脂基础材料。
称取9mg二甲苯、18mg硅树脂基础材料、1mg不饱和烯烃、1mg烯丙基缩水甘油醚和1mg不饱和聚醚和1mg铂催化剂备用。
依次将硅树脂基础材料、不饱和烯烃、烯丙基缩水甘油醚以及不饱和聚醚溶解于二甲苯中,采用高活性铂催化剂在常温下催化反应6-18h,制备得到粗制的氨纶油剂中间体,反应结束后在80℃下,压力为0.10Mpa下蒸馏二甲苯和小分子醇,得到硅树脂固体材料。
实施例二
称量42mg正硅酸甲酯、13mg水、11mg丙醇、10mg乙苯、9.2mg二甲基硅氧烷四聚体、7mg四甲基二氢二硅氧烷和280mg质量分数为1%的盐酸备用;
将水、丙醇和乙苯混合溶解,制备成混合溶剂,然后将硅酸酯、二甲基硅氧烷四聚体和含氢双封头溶解于混合溶剂中,然后滴加加盐酸作催化剂于80℃水解缩合90min合成硅树脂基础材料;
过滤步骤一中得到的含有硅树脂基础材料的混合液中的油相,得到硅树脂粗制品,粗制品依次经过质量分数为1%的氢氧化钠溶液中和至中性,然后再次过滤,对所得固体采用蒸馏水洗涤三次,每次5ml,然后将固体放在烘箱中,调整压力为1.5Mpa,调整温度为150℃进行加压蒸馏,蒸至无液体蒸出即可得到硅树脂基础材料。
称取11mg二甲苯、22mg硅树脂基础材料、3mg不饱和烯烃、3mg烯丙基缩水甘油醚和3mg不饱和聚醚和1mg铂催化剂备用。
依次将硅树脂基础材料、不饱和烯烃、烯丙基缩水甘油醚以及不饱和聚醚溶解于二甲苯中,采用高活性铂催化剂在常温下催化反应8h,制备得到粗制的氨纶油剂中间体,反应结束后在85℃下,压力为0.15Mpa下蒸馏二甲苯和小分子醇,得到硅树脂固体材料。
实施例三
称量37mg正硅酸甲酯、11mg水、10mg乙醇、9mg对二甲苯、8.6mg二甲基硅氧烷四聚体、4.5mg四甲基二氢二硅氧烷和230mg质量分数为1%的盐酸备用;
将水、乙醇和对二甲苯混合溶解,制备成混合溶剂,然后将硅酸酯、二甲基硅氧烷四聚体和含氢双封头溶解于混合溶剂中,然后滴加加盐酸作催化剂于72℃水解缩合45min合成硅树脂基础材料;
过滤步骤一中得到的含有硅树脂基础材料的混合液中的油相,得到硅树脂粗制品,粗制品依次经过质量分数为1%的氢氧化钠溶液中和至中性,然后再次过滤,对所得固体采用蒸馏水洗涤三次,每次5ml,然后将固体放在烘箱中,调整压力为1.5Mpa,调整温度为150℃进行加压蒸馏,蒸至无液体蒸出即可得到硅树脂基础材料。
称取10mg二甲苯、20mg硅树脂基础材料、2mg不饱和烯烃、2mg烯丙基缩水甘油醚和2mg不饱和聚醚和1mg铂催化剂备用。
依次将硅树脂基础材料、不饱和烯烃、烯丙基缩水甘油醚以及不饱和聚醚溶解于二甲苯中,采用高活性铂催化剂在常温下催化反应6-18h,制备得到粗制的氨纶油剂中间体,反应结束后在85℃下,压力为0.13Mpa下蒸馏二甲苯和小分子醇,得到硅树脂固体材料。
实施例四
称量38mg正硅酸甲酯、12mg水、10mg丙醇、9mg对二甲苯、8.7mg二甲基硅氧烷四聚体、5.6mg四甲基二氢二硅氧烷和260mg质量分数为1%的盐酸备用;
将水、丙醇、对二甲苯混合溶解,制备成混合溶剂,然后将硅酸酯、二甲基硅氧烷四聚体和含氢双封头溶解于混合溶剂中,然后滴加加盐酸作催化剂于75℃水解缩合40min合成硅树脂基础材料;
过滤步骤一中得到的含有硅树脂基础材料的混合液中的油相,得到硅树脂粗制品,粗制品依次经过质量分数为1%的氢氧化钠溶液中和至中性,然后再次过滤,对所得固体采用蒸馏水洗涤三次,每次5ml,然后将固体放在烘箱中,调整压力为1.5Mpa,调整温度为150℃进行加压蒸馏,蒸至无液体蒸出即可得到硅树脂基础材料。
称取10mg二甲苯、20mg硅树脂基础材料、2mg不饱和烯烃、2mg烯丙基缩水甘油醚和2mg不饱和聚醚和1mg铂催化剂备用。
依次将硅树脂基础材料、不饱和烯烃、烯丙基缩水甘油醚以及不饱和聚醚溶解于二甲苯中,采用高活性铂催化剂在常温下催化反应16h,制备得到粗制的氨纶油剂中间体,反应结束后在88℃下,压力为0.14Mpa下蒸馏二甲苯和小分子醇,得到硅树脂固体材料。
实施例五
称量40mg正硅酸甲酯、12mg水、10mg丙醇、9mg乙苯、9.1mg二甲基硅氧烷四聚体、6mg四甲基二氢二硅氧烷和270mg质量分数为1%的盐酸备用;
将水、丙醇、乙苯混合溶解,制备成混合溶剂,然后将硅酸酯、二甲基硅氧烷四聚体和含氢双封头溶解于混合溶剂中,然后滴加加盐酸作催化剂于78℃水解缩合88min合成硅树脂基础材料;
过滤步骤一中得到的含有硅树脂基础材料的混合液中的油相,得到硅树脂粗制品,粗制品依次经过质量分数为1%的氢氧化钠溶液中和至中性,然后再次过滤,对所得固体采用蒸馏水洗涤三次,每次5ml,然后将固体放在烘箱中,调整压力为1.5Mpa,调整温度为150℃进行加压蒸馏,蒸至无液体蒸出即可得到硅树脂基础材料。
称取10mg二甲苯、20mg硅树脂基础材料、2mg不饱和烯烃、2mg烯丙基缩水甘油醚和2mg不饱和聚醚和1mg铂催化剂备用。
依次将硅树脂基础材料、不饱和烯烃、烯丙基缩水甘油醚以及不饱和聚醚溶解于二甲苯中,采用高活性铂催化剂在常温下催化反应16h,制备得到粗制的氨纶油剂中间体,反应结束后在87℃下,压力为0.14Mpa下蒸馏二甲苯和小分子醇,得到硅树脂固体材料。
实施例六
称量41mg正硅酸甲酯、12mg水、10mg乙醇、8mg对二甲苯、8.6mg二甲基硅氧烷四聚体、4.5mg四甲基二氢二硅氧烷和275mg质量分数为1%的盐酸备用;
将水、乙醇、对二甲苯混合溶解,制备成混合溶剂,然后将硅酸酯、二甲基硅氧烷四聚体和含氢双封头溶解于混合溶剂中,然后滴加加盐酸作催化剂于78℃水解缩合85min合成硅树脂基础材料;
过滤步骤一中得到的含有硅树脂基础材料的混合液中的油相,得到硅树脂粗制品,粗制品依次经过质量分数为1%的氢氧化钠溶液中和至中性,然后再次过滤,对所得固体采用蒸馏水洗涤三次,每次5ml,然后将固体放在烘箱中,调整压力为1.5Mpa,调整温度为150℃进行加压蒸馏,蒸至无液体蒸出即可得到硅树脂基础材料。
称取10mg二甲苯、21mg硅树脂基础材料、2mg不饱和烯烃、2mg烯丙基缩水甘油醚和2mg不饱和聚醚和1mg铂催化剂备用。
依次将硅树脂基础材料、不饱和烯烃、烯丙基缩水甘油醚以及不饱和聚醚溶解于二甲苯中,采用高活性铂催化剂在常温下催化反应17h,制备得到粗制的氨纶油剂中间体,反应结束后在88℃下,压力为0.14Mpa下蒸馏二甲苯和小分子醇,得到硅树脂固体材料。
将实施例一、实施例二、实施例三、实施例四、实施例五和实施例六制备的助剂产品添加到氨纶产品中,分别作为实验组一、实验组二、实验组三、实验组四、实验组五、实验组六,再采用一组氨纶不添加助剂,作为对比例一,分别测量实验组一、实验组二、实验组三、实验组四、实验组五、实验组六和对比例一在常温下的退绕张力、电阻率以及高温恶化后退让张力,结果如表1、表2和表3所示,由表1、表2和表3可知,添加本发明提供的助剂,能够有效减小氨纶退绕张力,降低氨纶的比电阻,降低氨纶高温恶化后的退让张力。
表1 助剂对氨纶退绕张力的影响
表层退绕张力(N) | 中层退绕张力(N) | 内层退绕张力(N) | |
实施例一 | 1.87 | 2.07 | 2.55 |
实施例二 | 1.88 | 2.09 | 2.56 |
实施例三 | 1.84 | 2.03 | 2.52 |
实施例四 | 1.86 | 2.06 | 2.54 |
实施例五 | 1.83 | 2.02 | 2.51 |
实施例六 | 1.89 | 2.11 | 2.57 |
对比例一 | 2.01 | 2.26 | 2.97 |
表2助剂对氨纶电阻率的影响
比电阻(欧姆) | |
实施例1 | 1.09*10<sup>11</sup> |
实施例2 | 1.11*10<sup>11</sup> |
实施例3 | 1.10*10<sup>11</sup> |
实施例4 | 1.08*10<sup>11</sup> |
实施例5 | 1.06*10<sup>11</sup> |
实施例6 | 1.07*10<sup>11</sup> |
对比例一 | 1.8*10<sup>11</sup> |
表3助剂对氨纶高温恶化后退让张力的影响
表层高温恶化后退绕张力(N) | 中层高温恶化后退绕张力(N) | 内层高温恶化后退绕张力(N) | |
实施例一 | 2.37 | 3.21 | 3.97 |
实施例二 | 2.38 | 3.22 | 3.96 |
实施例三 | 2.35 | 3.23 | 3.93 |
实施例四 | 2.33 | 3.2 | 3.94 |
实施例五 | 2.39 | 3.22 | 3.99 |
实施例六 | 2.40 | 3.24 | 3.91 |
对比例一 | 3.01 | 4.11 | 4.79 |
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (10)
1.一种应用于氨纶纺丝油剂中的起到隔离和调节摩擦作用的助剂产品,其特征在于,所述助剂产品的结构为(A3SiO0.5)a(BMe2SiO0.5)b(CMe2SiO0.5)c(DMe2SiO0.5)d(Me2SiO)e(SiO2)f,其中,A指代甲基与羟基混合体结构,B指代长链烷基,C指代缩水甘油醚基,D指代聚醚基团,Me指代甲基;其中,a、b、c、d、e、f表示链节数或聚合度,a为3-10,b为2-5,c为2-5,d为2-5,e为1-5,f为5-8。
2.根据权利要求1所述的应用于氨纶纺丝油剂中的起到隔离和调节摩擦作用的助剂产品,其特征在于,所述助剂产品制备过程如下:
步骤一、先将硅酸酯、二甲基硅氧烷四聚体和含氢双封头溶解于混合溶剂中,然后滴加盐酸作催化剂于70-80℃水解缩合30-90min合成硅树脂基础材料;
步骤二、分离步骤一中得到的含有硅树脂基础材料的混合液中的油相得到硅树脂粗制品,粗制品依次经过中和、过滤、洗涤和干燥得到硅树脂基础材料;
步骤三、将硅树脂基础材料、不饱和烯烃、烯丙基缩水甘油醚和不饱和聚醚按一定比例和顺序进行硅氢加成反应,最后分离溶剂及低沸物。
3.根据权利要求2所述的应用于氨纶纺丝油剂中的起到隔离和调节摩擦作用的助剂产品,其特征在于,所述步骤一中混合溶剂为水、醇类和苯类物质混合制备而成,所述醇类为乙醇或者丙醇,所述苯类物质为甲苯、乙苯或者对二甲苯中的一种。
4.根据权利要求2所述的应用于氨纶纺丝油剂中的起到隔离和调节摩擦作用的助剂产品,其特征在于,所述步骤一中硅酸酯、水、醇类、苯类、二甲基硅氧烷四聚体、含氢双封头和盐酸中有效成分质量比为35-42:10-13:9-11:8-10:8.5-9.2:4-7:2.2-2.8。
5.根据权利要求2所述的应用于氨纶纺丝油剂中的起到隔离和调节摩擦作用的助剂产品,其特征在于,所述步骤一中含氢双封头为四甲基二氢二硅氧烷。
6.根据权利要求2所述的应用于氨纶纺丝油剂中的起到隔离和调节摩擦作用的助剂产品,其特征在于,所述步骤一中硅酸酯为正硅酸甲酯。
7.根据权利要求2所述的应用于氨纶纺丝油剂中的起到隔离和调节摩擦作用的助剂产品,其特征在于,所述步骤二中采用氢氧化钠将过滤物质中和至中性,采用蒸馏水对过滤物质进行洗涤,所述步骤二中减压蒸除溶剂操作在150℃条件下进行,蒸至无液体蒸出即可。
8.根据权利要求2所述的应用于氨纶纺丝油剂中的起到隔离和调节摩擦作用的助剂产品,其特征在于,所述步骤三中具体操作为采用二甲苯作为溶剂,依次将硅树脂基础材料、不饱和烯烃、烯丙基缩水甘油醚以及不饱和聚醚溶解于二甲苯中,采用高活性铂催化剂在常温下催化反应6-18h,制备得到粗制的氨纶油剂中间体。
9.根据权利要求8所述的应用于氨纶纺丝油剂中的起到隔离和调节摩擦作用的助剂产品,其特征在于,所述二甲苯、硅树脂基础材料、不饱和烯烃、烯丙基缩水甘油醚和不饱和聚醚和铂催化剂质量比为9-11:18-22:1-3:1-3:1-3:1,其中,所述不饱和烯烃、烯丙基缩水甘油醚和不饱和聚醚质量比为1:1:1。
10.根据权利要求2所述的应用于氨纶纺丝油剂中的起到隔离和调节摩擦作用的助剂产品,其特征在于,所述步骤三中分离溶剂及低沸物具体操作为硅氢加成反应结束后,在80-90℃下,压力为0.10-0.15Mpa下蒸馏溶剂和小分子醇。
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CN101440574A (zh) * | 2008-12-18 | 2009-05-27 | 宁波经济技术开发区希科新材料有限公司 | 一种干法氨纶纺丝用油剂及其制备方法和应用 |
CN101597377A (zh) * | 2009-06-29 | 2009-12-09 | 山东大易化工有限公司 | 一种甲基封端烷基聚醚环氧基苯基共改性聚硅氧烷的化合物及其制备方法和应用 |
KR20110079299A (ko) * | 2009-12-31 | 2011-07-07 | 주식회사 효성 | 비이온 계면활성제를 포함하는 스판덱스 방사유제, 이의 제조방법 및 이를 이용한 생산된 스판덱스 섬유 |
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