CN106188477A - 一种高弹医用聚氨酯手套材料的制备方法 - Google Patents

一种高弹医用聚氨酯手套材料的制备方法 Download PDF

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CN106188477A
CN106188477A CN201610594885.1A CN201610594885A CN106188477A CN 106188477 A CN106188477 A CN 106188477A CN 201610594885 A CN201610594885 A CN 201610594885A CN 106188477 A CN106188477 A CN 106188477A
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李成文
赵世图
李民刚
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Hongpulin (beijing) Medical Supplies High-Tech Research Institute Co Ltd
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Abstract

本发明涉及一种高弹医用聚氨酯手套材料的制备方法，先合成出特殊高分子量回弹剂，然后用这种高分子量回弹剂改性整个聚氨酯合成材料的性能，从而得到高弹医用聚氨酯手套材料，其综合性能是优于天然乳胶手套和丁腈手套材料。

Description

一种高弹医用聚氨酯手套材料的制备方法
技术领域
本发明涉及一种高弹医用聚氨酯手套材料的制备方法，属于高分子材料领域。
背景技术
目前，在医疗卫生、食品保健、电子等多个行业，对薄手套的防护性能要求越来越高，而传统的手套种类只有天然橡胶手套、聚氯乙烯手套、丁腈手套、聚乙烯手套等，其中聚乙烯手套没有弹性使用领域很小，聚氯乙烯手套强度和弹性略好，能适用于简单手部保护，弹性最好的手套只有天然乳胶手套和丁腈手套，而丁腈手套由于不含有天然乳胶手套中的蛋白质，不会引起穿戴手套过敏，因此逐渐代替天然乳胶手套。但是就是综合性能最好的丁腈手套，也因为含有硫磺、易破等缺陷限制了使用。因此，开发一种不含硫磺，同时具有天然乳胶手套和丁腈手套的所有优点的手套，在成本相当的情况下，就必将引起医用手套行业的革命。本发明高弹医用聚氨酯手套材料就是在这样的背景下开始研究的。
中国现有关于手套相关专利如CN103549686A、CN1759778A、CN101036535A、CN103564892A、CN102599660A、CN101028742A、CN201414445U和CN1513903A都是从手套防护功能和用途，以及生产工艺方面进行研究的，很少有从制作手套胶乳原料本身进行改性研究的。
本发明的目的是提供一种高弹医用聚氨酯手套材料的制备方法。
本发明是通过在聚氨酯合成的过程中引入一种高分子量回弹剂，增大聚氨酯材料的回弹性，可以与橡胶材料媲美，因此，称之为高弹医用聚氨酯手套材料。因为传统聚氨酯材料基本都是有伸长，没回弹，而高弹医用聚氨酯手套材料则完全改变了聚氨酯材料没有回弹的缺点，并且其弹性与橡胶材料相近。
本发明通过先合成出特殊高分子量回弹剂，然后用这种高分子量回弹剂改性整个聚氨酯合成材料的性能，从而得到高弹医用聚氨酯手套材料。由于聚氨酯材料具有极好的生物相容性，广泛用于医疗领域，因此用这种高弹医用聚氨酯手套材料制备的手套就可以作为医用手套，其综合性能是优于天然乳胶手套和丁腈手套的，必将引起医用手套更新换代。
发明内容
本发明通过先合成出特殊高分子量回弹剂，然后用这种高分子量回弹剂改性整个聚氨酯合成材料的性能，从而得到高弹医用聚氨酯手套材料。然后用这种高弹医用聚氨酯手套材料制成医用聚氨酯手套。
本发明采用的技术方案是：先制备高分子量回弹剂，制备出高弹医用聚氨酯手套材料后，再通过浸渍成型工艺，制得手套。
本发明详述如下：
1.高分子量回弹剂的合成。
回弹剂以聚醚多元醇为原料，常用聚醚多元醇的数均分子量一般在400～8000之间，其中以分子量为2000、3000、4800、6000和8000应用最为广泛，鲜有数均分子量超过20000的多元醇商品。所述的高分子量回弹剂采用聚醚二元醇与多异氰酸酯加成聚合制备大分子聚氨酯预聚体，再通过多官能度聚醚多元醇封端该大分子聚氨酯预聚体，从而得到多官能度超高分子量多元醇。制备的多官能度高分子量多元醇具有Am-Bp-An型分子结构，数均分子量在35 000～100 000之间，分子链两端羟基封端且羟基平均官能度不小于4。
具体步骤如下：
将聚醚二元醇起始剂抽真空加热至110℃～120℃进行除水1.5h～2h，降温至40℃～50℃；
将异氰酸酯按计量比例加入二元醇中；
在催化剂作用下，80℃～85℃下搅拌反应3～5h得到预聚物；
按配比加入封端剂终止反应，得到一种多官能度高分子量多元醇，即高分子量回弹剂。
所述封端剂为高官能度聚醚多元醇，如聚醚四元醇、聚醚五元醇、聚醚六元醇等，分子量200-10000。
化学反应方程式如下：
2.高弹医用聚氨酯手套材料的制备。先将聚醚二元醇与高分子量回弹剂混合，再和含有亲水基团的二元醇组成聚氨酯链段中的软段成分；二异氰酸酯选用脂肪族二异氰酸酯作为硬段成分；上述软段成分、硬段成分、扩链剂充分混合搅拌后，即得高弹医用聚氨酯手套材料。
聚醚二元醇与高分子量回弹剂按10：0到5：5比例混合，优选按7：3到5：5比例混合，特别优选按3：2到1：1比例混合。
自乳化阴离子型聚氨酯乳液由于分子链中引入离子基团羧基、磺酸或硫酸根，所以通常选用含羧基的二元醇，如二羟甲基丙酸(DMPA)，其含量为0.5-20％，理想含量为2-12％。
扩链剂通常选用二元胺，如乙二胺，加入量为1-10％，最理想加入量为3-7％。
上述步骤中还可以加入润湿剂1-2％，消泡剂1-2％。
聚醚多元醇部分分子量为500-5000，理想分子量为500-3500。
二异氰酸酯的加入量为3-8％，优选为4-6％。上述脂肪族二异氰酸酯选择氢化4，4-亚甲基二苯基二异氰酸酯(HMDI)、六亚甲基二异氰酸酯(HDI)、异佛尔酮二异氰酸酯(IPDI)或其混合物，二异氰酸酯优选选取六亚甲基二异氰酸酯(HDI)、异佛尔酮二异氰酸酯(IPDI)或其混合物。
本发明还要求保护上述制备方法制备的高弹医用聚氨酯手套材料。
具体实施方式
1、高分子量回弹剂合成配方如下表。
表1高分子量回弹剂
名称 规格 加入量(份数)
1 起始剂聚醚二元醇 Mn＝3000 72～96
2 异佛尔酮二异氰酸酯 99％ 3～18
3 催化剂 T9 0.01～3
(1)将二元醇起始剂抽真空加热至110℃～120℃进行除水1.5h～2h，降温至40℃～50℃。
(2)将异氰酸酯按计量比例加入二元醇中。
(3)在催化剂作用下，80℃～85℃下搅拌反应3～5h得到预聚物。
(4)按配比加入封端剂终止反应，得到一种多官能度高分子量多元醇，即高分子量回弹剂。
实施例：
1.1高分子量回弹剂合成工艺
(1)称取聚氧化丙烯醚二元醇PPG(分子量3000)511.55g，置于带有搅拌装置的三口烧瓶中，体系加热升温；
(2)体系温度达到110℃时进行真空除水，真空度-0.095～-0.1MPa、110℃～120℃条件下抽真空脱水1.5h～2h；
(3)除去体系真空，降温至40℃～50℃，将20.84g异佛尔酮二异氰酸酯(IPDI)逐渐滴加至体系中；
(4)IPDI滴加完成后，85℃恒温计时反应1h；
(5)加入催化剂T9(辛酸亚锡)5.40g，在催化剂作用下，85℃继续恒温反应2～3h得大分子聚氨酯预聚物，反应过程中每隔15min少量取样测定反应体系的NCO基团质量分数，直到NCO基团质量分数达到设计的理论值(0.13％)为止；
(6)加入9.00gDD-380A(硬质聚醚多元醇，羟值360-400mgKOH/g，水份≤0.2％，pH为9-12，粘度9000-13000MPa/25℃)封端剂，搅拌0.5h～1h，反应过程中每隔15min少量取样测定反应体系羟值，直到羟值达到设计的理论值(8.69mgKOH/g)为止；
(7)停止反应，得到十官能度超高分子量多元醇，合成出高分子量回弹剂。
2、高弹医用聚氨酯手套材料的合成：
先将聚醚二元醇与上述高分子量回弹剂按10：0到5：5比例混合(具体参见下述实施例1-5)，再和含有亲水基团的二元醇共同组成聚氨酯链段中的软段部分。聚醚多元醇分子量为3000左右。二异氰酸酯选取六亚甲基二异氰酸酯(HDI)和异佛尔酮二异氰酸酯(IPDI)比例为1：1，二羟甲基丙酸(DMP)，其含量为6％。扩链剂通常选用乙二胺，加入量为5％。再加入润湿剂1％，消泡剂1％。充分混合搅拌后，即得高弹医用聚氨酯手套材料。
上述实施例中原料产地：
聚氧化丙烯醚二元醇PPG(分子量3000，山东蓝星东大工有限责任公司生产)
DD-380A(聚六醚醇，山东蓝星东大工有限责任公司生产)
表2性能测试

Claims (10)

1.一种高弹医用聚氨酯手套材料的制备方法，包括如下步骤：
(1)高分子量回弹剂的合成，采用聚醚二元醇与多异氰酸酯加成聚合制备大分子聚氨酯预聚体，再通过多官能度聚醚多元醇封端该大分子聚氨酯预聚体，从而得到多官能度超高分子量多元醇，即高分子量回弹剂；
(2)高弹医用聚氨酯手套材料的制备，将聚醚二元醇与上述高分子量回弹剂混合，再和含有亲水基团的二元醇组成聚氨酯链段中的软段成分；二异氰酸酯选用脂肪族二异氰酸酯作为硬段成分；上述软段成分、硬段成分、扩链剂充分混合搅拌后，即得高弹医用聚氨酯手套材料。
2.根据权利要求1所述的制备方法，其特征在于：制备的所述多官能度高分子量多元醇具有Am-Bp-An型分子结构，数均分子量在35 000～100 000之间，分子链两端羟基封端且羟基平均官能度不小于4。
3.根据权利要求1所述的制备方法，其特征在于：高分子量回弹剂合成的具体步骤为：
(1)将二元醇起始剂抽真空加热至110℃～120℃进行除水1.5h～2h，降温至40℃～50℃；
(2)将异氰酸酯加入二元醇中；
(3)在催化剂作用下，80℃～85℃下搅拌反应3～5h得到预聚物；
(4)加入封端剂终止反应，得到多官能度高分子量多元醇。
4.根据权利要求3所述的制备方法，其特征在于：所述催化剂为辛酸亚锡。
5.根据权利要求3所述的制备方法，其特征在于：所述封端剂为高官能度聚醚多元醇，如聚醚四元醇、聚醚五元醇、聚醚六元醇等。
6.根据权利要求1所述的制备方法，其特征在于：步骤(2)中，聚醚二元醇与高分子量回弹剂按10：0到5：5比例混合，优选按7：3到5：5比例混合，特别优选按3：2到1：1比例混合。
7.根据权利要求1所述的制备方法，其特征在于：含有亲水基团的二元醇通常选用含羧基的二元醇，如二羟甲基丙酸(DMP)，其含量为0.5-20％，理想含量为2-12％。
8.根据权利要求1所述的制备方法，其特征在于：扩链剂通常选用二元胺，如乙二胺，加入量为1-10％，最理想加入量为3-7％。
9.根据权利要求1所述的制备方法，其特征在于：步骤(2)中，二异氰酸酯的加入量为3-8％，优选为4-6％；二异氰酸酯为脂肪族二异氰酸酯，上述脂肪族二异氰酸酯选择氢化4，4-亚甲基二苯基二异氰酸酯(HMDI)、六亚甲基二异氰酸酯(HDI)、异佛尔酮二异氰酸酯(IPDI)或其混合物。
10.权利要求1-9任一项所述的制备方法制备的高弹医用聚氨酯手套材料。
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