CN107501520A - 一种抗静电处理剂及其制备方法 - Google Patents

一种抗静电处理剂及其制备方法 Download PDF

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Publication number
CN107501520A
CN107501520A CN201710864093.6A CN201710864093A CN107501520A CN 107501520 A CN107501520 A CN 107501520A CN 201710864093 A CN201710864093 A CN 201710864093A CN 107501520 A CN107501520 A CN 107501520A
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treatment agent
antistatic treatment
parts
glycol
alcohol
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何子健
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Jiangsu Duosen Chemical Co Ltd
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Jiangsu Duosen Chemical Co Ltd
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Priority to CN201710864093.6A priority Critical patent/CN107501520A/zh
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Abstract

本发明提供一种抗静电处理剂及其制备方法，涉及材料制备技术领域。一种抗静电处理剂，该抗静电处理剂的原料包括按重量份数计的以下组分：聚合物多元醇20‑30份，多异氰酸酯5‑22份，导电剂0.1‑1份。聚合物多元醇主要采用多种常用的二元醇。多异氰酸酯包括二异氰酸酯、三异氰酸酯中的一种或两种。导电剂包括氧化石墨和/或氧化石墨烯。多异氰酸酯上的异氰酸根将与氧化石墨或氧化石墨烯上的羟基进行反应，同时异氰酸根也将与聚合物多元醇的羟基进行反应。因此，以多异氰酸酯为桥梁将氧化石墨接入到了聚氨酯的分子链中，从根本上解决了氧化石墨在聚氨酯树脂中的聚集和沉降问题，从而提高聚氨酯合成革表面的抗静电能力。

Description

一种抗静电处理剂及其制备方法
技术领域
本发明涉及材料制备技术领域，具体而言，涉及一种抗静电处理剂及其制备方法。
背景技术
随着聚氨酯原材料及相关配方工艺的不断优化，聚氨酯合成革已经深入到人们生活的方方面面。聚氨酯处理剂可以赋予聚氨酯合成革更为优异的性能，突出表现为提高合成革的表面机械性能，如耐磨耐刮性等。合成革由有机高分子化合物组成，本身不易导电，但在使用过程中不可避免的与身体等产生摩擦，极易产生静电。静电如果不能及时的从合成革表面导出，静电聚集过多很容易诱发一些事故，如静电在人体聚集到一定程度，极易诱发心脑血管疾病。
发明内容
本发明的目的在于提供一种抗静电处理剂，其具有优异的抗静电效果。
本发明的另一目的在于提供一种抗静电处理剂的制备方法，该方法简单易行，易于工业化生产。
本发明解决其技术问题是采用以下技术方案来实现的。
本发明提出一种抗静电处理剂，该抗静电处理剂的原料包括按重量份数计的以下组分：
聚合物多元醇20-30份，多异氰酸酯5-22份，导电剂0.1-1份。
聚合物多元醇包括聚四氢呋喃醚二醇、聚己二酸-1,4丁二醇酯二醇、聚己二酸乙二醇酯二醇、聚己二酸丙二醇酯二醇、聚己二酸-1,6己二醇酯二醇、聚己二酸新戊二醇酯二醇、聚己二酸乙二醇丁二醇酯二醇、聚己二酸乙二醇丙二醇酯二醇、聚己二酸己二醇新戊二醇酯二醇、聚己二酸丁二醇己二醇酯二醇、聚己二酸丁二醇新戊二醇酯二醇、聚己內酯二醇中的一种或多种。
多异氰酸酯包括二异氰酸酯、三异氰酸酯中的一种或两种。导电剂包括氧化石墨和/或氧化石墨烯。
本发明提出一种抗静电处理剂的制备方法，包括：将聚合物多元醇，二异氰酸酯，导电剂进行混合反应。
本发明实施例提供的抗静电处理剂及其制备方法的有益效果是：
传统的聚氨酯抗静电处理剂的主要做法是在聚氨酯树脂中添加一定量导电填料。这类直接添加的导电填料与有机的聚氨酯相容性较差，极易在聚氨酯体系中聚集或沉降，在后续加工应用中抗静电效果差。本发明实施例将氧化石墨(或氧化石墨烯)添加到聚氨酯的合成体系中，利用氧化石墨上的羟基、羧基与多异氰酸酯的反应，将氧化石墨接入到聚氨酯的分子链中，使得氧化石墨在聚氨酯体系中不易团聚，具有更好的分散性。从根本上解决了氧化石墨在聚氨酯树脂中的聚集和沉降问题，使聚氨酯合成革表面的抗静电能力大幅度提高，从而进一步拓宽该抗静电处理剂在合成革中的应用领域。
本发明实施例还提出一种抗静电处理剂的制备方法，将聚合物多元醇，二异氰酸酯，氧化石墨进行混合反应。该方法简便易行，便于批量生产。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将对本发明实施例中的技术方案进行清楚、完整地描述。实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。
下面对本发明实施例的抗静电处理剂和制备方法进行具体说明。
一种抗静电处理剂，抗静电处理剂的原料包括按重量份数计的以下组分：聚合物多元醇20-30份，多异氰酸酯5-22份，导电剂0.1-1份。导电剂包括氧化石墨和/或氧化石墨烯。氧化石墨与氧化石墨烯在化学组成上相同，但氧化石墨烯的厚度较氧化石墨更小。氧化石墨上带有大量含氧官能团，其中主要包括羟基和羧基。多异氰酸酯上的异氰酸根将与氧化石墨上的羟基进行反应，同时异氰酸根也将与聚合物多元醇的羟基进行反应。因此，以多异氰酸酯为桥梁将氧化石墨接入到了聚氨酯的分子链中，从根本上解决了氧化石墨在聚氨酯树脂中的聚集和沉降问题，从而提高聚氨酯合成革表面的抗静电能力。传统工艺上，主要是将导电物料直接作为填料添加到聚氨酯中，因此多存在导电物料分散不均匀、团聚，甚至是导电物料的脱落，最终导致聚氨酯合成革表面的抗静电能力较差。本发明可以有效解决上述问题。
聚合物多元醇包括聚四氢呋喃醚二醇、聚己二酸-1,4丁二醇酯二醇、聚己二酸乙二醇酯二醇、聚己二酸丙二醇酯二醇、聚己二酸-1,6己二醇酯二醇、聚己二酸新戊二醇酯二醇、聚己二酸乙二醇丁二醇酯二醇、聚己二酸乙二醇丙二醇酯二醇、聚己二酸己二醇新戊二醇酯二醇、聚己二酸丁二醇己二醇酯二醇、聚己二酸丁二醇新戊二醇酯二醇、聚己內酯二醇中的一种或多种。其中，上述每一种二元醇均可以选用数均分子量为1000-3000的二元醇。
多异氰酸酯包括二异氰酸酯、三异氰酸酯中的一种或两种。多异氰酸酯是聚氨酯胶黏剂的主要原料之一，制造聚氨酯胶黏剂用的多异氰酸酯主要有二异氰酸酯、三异氰酸酯以及它们的改性体，其中最常见的是二异氰酸酯。
二异氰酸酯可以进一步包括常用的4,4-二苯甲烷二异氰酸酯(MDI)、甲苯二异氰酸酯(TDI)、苯亚甲基二异氰酸酯(XDI)、1,5-奈二异氰酸酯(NDI)、对苯二异氰酸酯(PPDI)、六亚甲基二异氰酸酯(HDI)、氢化4,4-二苯甲烷二异氰酸酯(H12MDI)中的一种或多种。
上述原料还可以进一步包括按重量份数计的以下组分：小分子多元醇0.5-1份，亲水性二元醇1-12份，水50-70份(化学反应中一般使用去离子水或蒸馏水)。聚氨酯主要包括油性聚氨酯和水性聚氨酯，目前由于水性聚氨酯的环保性，因此水性聚氨酯受到了更多的重视。亲水性二元醇主要用于制备水性聚氨酯。
小分子多元醇包括脂肪族二元醇，该脂肪族二元醇的烃基上可以含有2-6个碳原子，例如乙二醇、1，6己二醇、1，4丁二醇。脂肪族化合物是指烃基是直链结构，但烃基可以是饱和的和不饱和的。该小分子多元醇可以选用一种或多种脂肪族二元醇。
亲水性二元醇包括二羟甲基丁酸、二羟甲基丙酸、含磺酸钠基团的二元醇、含羧基的聚醚或聚酯中一种或多种。
在聚氨酯合成原料中使用多种不同多元醇，有利于提高聚氨酯产品的综合力学性能，力学性能的提高有利于保持聚氨酯的抗静电能力。
上述原料还可以进一步包括按重量份数计的以下组分：催化剂0.01-0.2份，助剂0.1-1.5份。
催化剂包括二丁基二月桂酸锡、辛酸亚锡或者有机铋催化剂中的一种或多种。催化剂可以提高混合物的反应速率，加快生产速率。助剂包括抗氧剂、流平剂、消泡剂、润湿剂中的一种或多种。助剂的使用可以提高聚氨酯终产品的综合力学性能。
本发明实施例还提供一种抗静电处理剂的制备方法，主要包括以下步骤：
先将氧化石墨进行超声处理，由于氧化石墨层间插入了大量含氧官能团(例如羟基和羧基)，经过超声处理后的氧化石墨很容易被剥离开来，使氧化石墨剥离为氧化石墨烯。因此，氧化石墨与氧化石墨烯在化学组成上相同，但氧化石墨烯的厚度较氧化石墨更小。因此，相较于氧化石墨，氧化石墨烯的导电能力更为优异。当然，也可以直接购买氧化石墨烯。
再将氧化石墨烯与聚合物多元醇加入反应釜中进行搅拌混合，搅拌混合在45-55℃下进行。期间，还可以将亲水性二元醇、小分子多元醇加入进行搅拌混合。混合完成后，再向其中缓慢加入多异氰酸酯，滴加多异氰酸酯的速率可以是20-50ul/min。缓慢加入多异氰酸酯有利于提高其与多元醇以及氧化石墨烯的反应均匀性，尤其可以进一步提高氧化石墨烯在聚氨酯中的分散性，从而保证聚氨酯合成革的抗静电能力。
多异氰酸酯加入完毕后，60-100℃下将混合反应保持1-5小时。反应完毕后，还可以进一步加入催化剂。加入催化剂后，当混合反应的溶液达到要求的粘度，即可对其进行中和(一般加入三乙胺进行中和)并加入去离子水进行乳化。最后再进一步添加助剂并搅拌均匀，即得到上述的抗静电处理剂。
以下结合实施例对本发明的特征和性能作进一步的详细描述。
实施例1
本实施例所用原料及质量如下：
聚己二酸丁二醇新戊二醇酯二醇(数均分子量1000)15g；聚己二酸-1,4丁二醇酯二醇(数均分子量1000)5g；三苯甲烷三异氰酸酯5g；氧化石墨0.1g。
本实施例的抗静电处理剂的制备方法如下：
将上述原料全部进行混合，混合后在50℃下保持反应的进行，根据观察反应溶液的变化判断反应的进行程度，最终得到抗静电处理剂。
实施例2
本实施例所用原料及质量如下：
聚己二酸乙二醇酯二醇(数均分子量3000)10g；聚己二酸丙二醇酯二醇(数均分子量1000)5g；聚己二酸丁二醇己二醇酯二醇(数均分子量2000)13g；三苯甲烷三异氰酸酯8g；PPDI 14g；氧化石墨1g；丙三醇0.3g；戊二醇0.5g；含磺酸钠基团的二元醇5g；含羧基的聚酯5g；去离子水50g。
本实施例的抗静电处理剂的制备方法如下：
聚己二酸乙二醇酯二醇、聚己二酸丙二醇酯二醇、聚己二酸丁二醇己二醇酯二醇、含磺酸钠基团的二元醇、含羧基的聚酯、丙三醇、戊二醇、氧化石墨一起投入反应釜中，45℃搅拌均匀。再缓慢的加入三苯甲烷三异氰酸酯和PPDI的混合物(滴加速度不限)，在60℃下保温反应，3h达到要求粘度后，中和并加去离子水乳化，即得到抗静电处理剂。
实施例3
本实施例所用原料及质量如下：
聚己二酸乙二醇丁二醇酯二醇(数均分子量3000)4g；聚己二酸乙二醇丙二醇酯二醇(数均分子量2000)7g；聚己二酸己二醇新戊二醇酯二醇(数均分子量2000)13g；聚四氢呋喃醚二醇(数均分子量1000)6g；H12MDI9g；XDI 9g；氧化石墨0.15g；氧化石墨烯0.15g；丙三醇0.3g；戊二醇0.2g；1，6己二醇0.4g；二羟甲基丁酸3g；二羟甲基丙酸4g；含磺酸钠基团的二元醇1g；蒸馏水70g；有机铋0.1g；辛酸亚锡0.1g；抗氧剂1g；流平剂5g。
本实施例的抗静电处理剂的制备方法如下：
先将氧化石墨超声处理，剥离为氧化石墨烯。将聚合物多元醇、亲水性二元醇、小分子多元醇、氧化石墨烯一起投入反应釜中，55℃搅拌均匀。再缓慢的加入H12MDI和XDI的混合物(滴加速率为50ul/min)，在100℃下保温反应。4h后滴加有机铋和辛酸亚锡的混合物，达到要求粘度后，中和并加蒸馏水乳化。最后添加BHT抗氧剂和流平剂并搅拌均匀，即得到抗静电处理剂。
实施例4
本实施例所用原料及质量如下：
聚己二酸-1,4丁二醇酯二醇(数均分子量2000)6g；聚己二酸乙二醇酯二醇(数均分子量1000)4g；聚己二酸丙二醇酯二醇(数均分子量1000)3g；聚己二酸-1,6己二醇酯二醇(数均分子量3000)8g；聚己二酸新戊二醇酯二醇(数均分子量1000)5g；NDI 5g；MDI 5g；HDI10g；氧化石墨0.8g；乙二醇0.1g；1，6己二醇0.2g；1，4丁二醇0.2g；丙三醇0.1g；二羟甲基丁酸2g；二羟甲基丙酸1g；含磺酸钠基团的二元醇1g；含羧基的聚醚2g；蒸馏水60g；二丁基二月桂酸锡0.02g；辛酸亚锡0.05g；有机铋0.03g；流平剂0.2g；消泡剂0.3g；润湿剂0.5g。
本实施例的抗静电处理剂的制备方法如下：
先将氧化石墨超声处理，剥离为氧化石墨烯。将聚合物多元醇、亲水性二元醇、小分子多元醇、氧化石墨烯一起投入反应釜中，52℃搅拌均匀。再缓慢的加入NDI、MDI和HDI的混合物(滴加速率为45ul/min)，在80℃下保温反应。3h后滴加上述催化剂的混合物，达到要求粘度后，中和并加蒸馏水乳化。最后添加上述助剂的混合物并搅拌均匀，即得到抗静电处理剂。
实施例5
本实施例所用原料及质量如下：
聚四氢呋喃醚二醇(数均分子量2000)20g；1，4丁二醇0.5g；二羟甲基丙酸1g；MDI4g；PPDI 8g；H12MDI 5g；TDI 5g；氧化石墨烯0.1g；去离子水54.7g；二丁基二月桂酸锡0.2g；抗氧剂BHT 1.5g。
本实施例的抗静电处理剂的制备方法如下：
将聚四氢呋喃醚二醇、二羟甲基丙酸、1，4丁二醇、石墨烯一起投入反应釜中，45℃搅拌均匀。再缓慢的加入上述多异氰酸酯的混合物(滴加速率为20ul/min)，在70℃下保温反应。2h后滴加二丁基二月桂酸锡催化剂，达到要求粘度后，中和并加去离子水乳化。最后添加BHT抗氧剂并搅拌均匀，即得到抗静电处理剂。
实施例6
本实施例所用原料及质量如下：
聚己二酸-1,6己二醇酯二醇(数均分子量2000)30g；1，4丁二醇1g；二羟甲基丁酸10g；MDI 5g；氧化石墨烯1g；去离子水52.89g；二丁基二月桂酸锡0.01g，流平剂0.1g。
本实施例的抗静电处理剂的制备方法如下：
将聚己二酸-1,6己二醇酯二醇(数均分子量2000)、二羟甲基丁酸、1，4丁二醇、石墨烯一起投入反应釜中，45℃搅拌均匀。再缓慢的加入MDI(滴加速率为50ul/min)，在70℃下保温反应。2h后滴加二丁基二月桂酸锡催化剂，达到要求粘度后，中和并加去离子水乳化。最后添加流平剂并搅拌均匀，即得到抗静电处理剂。
实施例7
本实施例所用原料及质量如下：
聚己內酯二醇(数均分子量2000)25g；1，6己二醇0.75g；二羟甲基丁酸12g；TDI8g；氧化石墨烯0.5g；去离子水53.45g；二丁基二月桂酸锡0.2g；流平剂0.1g。
本实施例的抗静电处理剂的制备方法如下：
将聚己內酯二醇(数均分子量2000)、二羟甲基丁酸、1，6己二醇、石墨烯一起投入反应釜中，55℃搅拌均匀。再缓慢的加入TDI(滴加速率为30ul/min)，在60℃下保温反应，2h后滴加二丁基二月桂酸锡催化剂。达到要求粘度后，中和并加去离子水乳化。最后添加流平剂并搅拌均匀，即得到抗静电处理剂。
实施例8
本实施例所用原料及质量如下：
聚己內酯二醇(数均分子量2000)26.8g；1，6己二醇1g；二羟甲基丁酸11g；HDI 2g；MDI 1g；TDI 2g；XDI 3g；NDI 2g；氧化石墨烯0.1g；去离子水50g；辛酸亚锡0.1g；消泡剂1g。
本实施例的抗静电处理剂的制备方法如下：
将聚己內酯二醇(数均分子量2000)、二羟甲基丁酸、1，6己二醇、石墨烯一起投入反应釜中，50℃搅拌均匀。再缓慢的加入上述多异氰酸酯的混合物(滴加速率为40ul/min)，在100℃下保温反应，5h后滴加辛酸亚锡催化剂。达到要求粘度后，中和并加去离子水乳化。最后添加消泡剂并搅拌均匀，即得到抗静电处理剂。
实施例9
本实施例所用原料及质量如下：
聚己二酸新戊二醇酯二醇(数均分子量2000)21.4g；乙二醇1g；含羧基的聚醚(数均分子量1000)1g；HDI 5g；氧化石墨烯0.5g；去离子水70g；辛酸亚锡0.1g；润湿剂0.2g；抗氧剂0.3g；流平剂0.4g；消泡剂0.1g；
本实施例的抗静电处理剂的制备方法如下：
聚己二酸新戊二醇酯二醇(数均分子量2000)、含羧基的聚醚(数均分子量1000)、乙二醇、石墨烯一起投入反应釜中，45℃搅拌均匀。再缓慢的加入HDI(滴加速率为45ul/min)，在70℃下保温反应，1h后滴加辛酸亚锡催化剂。达到要求粘度后，中和并加去离子水乳化。最后添加上述助剂并搅拌均匀，即得到抗静电处理剂。
试验例
将实施例1-9提供的抗静电处理剂和市售抗静电处理剂分别以20丝的厚度刮涂在汽车革专用离型纸上，并在130℃条件下烘干10min，分离后通过万用表测试膜上相隔2cm两点间的电阻值。实施例1-9与市售抗静电处理剂表面电阻测试结果见表1。
表1.实施例1-9与市售抗静电处理剂的表面电阻
从表1可知，本发明实施例1-9制备的抗静电处理剂具有优异的抗静电效果，其抗静电能力均优于市售抗静电处理剂。另外，加入氧化石墨烯制得的抗静电处理剂其抗静电能力较加入氧化石墨制得的抗静电处理剂强。
以上所描述的实施例是本发明一部分实施例，而不是全部的实施例。本发明的实施例的详细描述并非旨在限制要求保护的本发明的范围，而是仅仅表示本发明的选定实施例。基于本发明中的实施例，本领域普通技术人员在没有作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。

Claims (10)

1.一种抗静电处理剂，其特征在于，所述抗静电处理剂主要由以下按重量份数计的原料混合反应制成：
聚合物多元醇20-30份，多异氰酸酯5-22份，导电剂0.1-1份，
所述聚合物多元醇包括聚四氢呋喃醚二醇、聚己二酸-1,4丁二醇酯二醇、聚己二酸乙二醇酯二醇、聚己二酸丙二醇酯二醇、聚己二酸-1,6己二醇酯二醇、聚己二酸新戊二醇酯二醇、聚己二酸乙二醇丁二醇酯二醇、聚己二酸乙二醇丙二醇酯二醇、聚己二酸己二醇新戊二醇酯二醇、聚己二酸丁二醇己二醇酯二醇、聚己二酸丁二醇新戊二醇酯二醇、聚己內酯二醇中的一种或多种，
所述多异氰酸酯包括二异氰酸酯、三异氰酸酯中的一种或两种，所述导电剂包括氧化石墨和/或氧化石墨烯。
2.根据权利要求1所述的抗静电处理剂，其特征在于，所述二异氰酸酯包括4,4-二苯甲烷二异氰酸酯、甲苯二异氰酸酯、苯亚甲基二异氰酸酯、1,5-奈二异氰酸酯、对苯二异氰酸酯、六亚甲基二异氰酸酯、氢化4,4-二苯甲烷二异氰酸酯中的一种或多种。
3.根据权利要求1所述的抗静电处理剂，其特征在于，所述抗静电处理剂的原料还包括按重量份数计的以下组分：
小分子多元醇0.5-1份，亲水性二元醇1-12份，水50-70份，
所述小分子多元醇包括脂肪族二元醇，所述脂肪族二元醇的烃基上含有2-6个碳原子，
所述亲水性二元醇包括二羟甲基丁酸、二羟甲基丙酸、含磺酸钠基团的二元醇、含羧基的聚醚或聚酯中一种或多种。
4.根据权利要求1-3任一项所述的抗静电处理剂，其特征在于，所述抗静电处理剂的原料还包括按重量份数计的以下组分：
催化剂0.01-0.2份，助剂0.1-1.5份，
所述催化剂包括二丁基二月桂酸锡、辛酸亚锡或者有机铋催化剂中的一种或多种，所述助剂包括抗氧剂、流平剂、消泡剂、润湿剂中的一种或多种。
5.一种如权利要求1-4任一项所述的抗静电处理剂的制备方法，其特征在于，包括：将所述聚合物多元醇，所述多异氰酸酯，所述导电剂进行混合反应。
6.根据权利要求5所述的抗静电处理剂的制备方法，其特征在于，混合反应的温度为60-100℃。
7.根据权利要求5所述的抗静电处理剂的制备方法，其特征在于，混合所述聚合物多元醇，所述多异氰酸酯，所述氧化石墨之前，还包括对所述氧化石墨进行超声处理。
8.根据权利要求5所述的抗静电处理剂的制备方法，其特征在于，将所述聚合物多元醇与所述导电剂混合，并于45-55℃下搅拌，再与所述多异氰酸酯进行混合反应。
9.根据权利要求8所述的抗静电处理剂的制备方法，其特征在于，向所述聚合物多元醇与所述导电剂的混合溶液中滴加所述多异氰酸酯的速率为20-50ul/min。
10.根据权利要求5所述的抗静电处理剂的制备方法，其特征在于，混合反应1-5小时后，对混合反应后的反应溶液进行中和、乳化。
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