CN112080035A - 一种水溶性泡沫及其制备方法 - Google Patents
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Abstract
本发明公开了一种水溶性泡沫及其制备方法，按照重量份数计，该泡沫由A、B两种水溶液按照质量比1～5:1混合后，经过浇注、快速冷冻和冷冻干燥等步骤制备而成。其中，A溶液由5～15份聚乙烯醇和100～200份水组成，B溶液由5～20份水性聚氨酯、1～3份增稠剂和1～10份吸水助剂组成。泡沫制备过程仅涉及机械混合和冷冻干燥，方法简单，易操作，成本低；所制备的水溶性泡沫具有可压缩、回弹性好和可降解特性。
Description
技术领域
本发明涉及一种水溶性泡沫及其制备方法，属于生物医用耗材领域。
背景技术
泡沫材料在日常生活和生产中应用非常广泛，例如软质泡沫材料由于具备缓冲、吸音、隔振、保温和过滤特性，被广泛应用于电子、汽车、家居、体育休闲等领域，硬质结构泡沫由于具备质轻高强和阻燃特性，被广泛应用于建筑、航空航天、轨道交通、风力发电等领域。然而，上述应用领域中的泡沫材料多为不能溶解和降解的，一方面不环保，另一方面不能很好满足特定领域的应用需求。
在医用止血材料领域，能够在手术后自行消融的泡沫材料能够方便医生观察伤口愈合情况或对伤口进行二次给药，同时能够极大限度减轻病人的痛苦，而且伤口完全愈合后无需特殊处理，仅通过水冲洗就可以去除止血泡沫材料，消除了病人术后止血材料去除过程中的恐惧感。
聚乙烯醇由于具有水溶性，常被用于亲水和高吸水泡沫。专利公开号为CN1289629 A、CN 1095075 A、CN 1557872 A和CN 1095387 A的中国专利所公开的基于聚乙烯醇制备的泡沫，均涉及到加入醛和酸，生产工艺不环保，产品不易作为医用止血材料使用。专利公开号为CN102827442 A的中国专利公开了一种聚乙烯醇-聚氨酯高吸水海绵的制备方法，是通过聚乙烯醇水溶液与聚氨酯共混发泡的方式得到高吸水海绵，涉及化学反应和有机锡催化剂的使用，工艺复杂，产品应用于医用止血领域存在一定的风险。专利公开号为CN 108587016 A的中国专利公开了一种聚乙烯醇水溶性泡沫塑料及其制备方法，是通过双螺杆挤出机挤出造粒得到可发性母粒，然后采用微波发泡工艺实现水溶性泡沫制备，该泡沫为闭孔结构，且制备工艺较复杂，尽管产品具备水溶性，但泡沫密度较大，不易作为医用止血材料使用。
发明内容
为了克服现有技术在医用止血领域应用的不足，本发明提供了一种生产工艺简单、且无需添加催化剂、醛和酸的水溶性泡沫及其制备方法。具体地，所述泡沫通过如下步骤制备得到：
S1、将5～15份聚乙烯醇在溶解于100～200份水中得到聚乙烯醇溶液，记为A；
S2、将5～20份聚氨酯分散体、1～3份增稠剂和1～10份吸水助剂混合，得到均匀分散液，记为B；
S3、将A、B按照体积比1～5:1进行混合，真空搅拌均匀后浇注于模具中，冷冻干燥得到聚氨酯水溶性泡沫。
在更优选的实施方式中，上述步骤S1是将5～15份聚乙烯醇在100～200份水中室温溶胀12-36h，然后在45～70℃、真空条件下搅拌3～4h得到稳定均匀溶液，记为A。
所述聚乙烯醇的醇解度70％～95％，聚合度1500～2000。
所述真空是在-0.090MPa～-0.098MPa的负压条件下，在优选的实施例中，是在-0.095MPa的真空条件下。
在更优选的实施方式中，所述步骤S2是将5～20份水性聚氨酯分散体、1～3份增稠剂和1～10份吸水助剂进行混合，室温条件下搅拌1～2h，然后在-0.095MPa真空搅拌条件下，继续搅拌0.5～1h得到均匀溶液，记为B。
在更优选的实施方式中，所述步骤S3是将A、B两种溶液按照体积比1～5:1进行混合，真空搅拌均匀后浇注于涂有脱模剂的模具中，在-25℃冷冻彻底后，将样品取出转移至冷冻干燥机中，在-80℃冷冻干燥24～36h得到水溶性泡沫。
在优选的实施方式中，所述水为纯净水。
所述水性聚氨酯为阴离子水性聚氨酯分散体，质量固含量29％～50％，固化后薄膜100％模量≤3MPa。
所述增稠剂为水性阴离子缔合型增稠剂。
所述吸水助剂为吸水率≥400％的高分子化合物。
所述吸水助剂包括但不限于淀粉、海藻酸钠、明胶、聚丙烯酸钠、聚乳酸、聚氧化烷烃中的一种或多种混合物。
制备得到的水溶性泡沫的25％压陷硬度为100-150N，平均孔径0.3-0.5mm，密度40-70kg/m3。
在本发明的水溶性泡沫应用于鼻腔止血棉的场景中，使用所述水溶性泡沫作为鼻腔止血棉材料。本发明通过吸水材料，特别是一种水溶性泡沫材料制备鼻腔止血棉。吸水材料以鼻腔作为受限空间，在鼻腔湿润的环境中，表面吸水后，形成柔软的凝胶，与伤口贴合，对伤口起到压迫止血作用。
当需要换药时，直接用大量水冲洗鼻腔，止血棉溶解发生结构塌陷，从而方便鼻腔棉的取出。
具体实施方式
为了更好理解本发明，下面结合具体实施例对本发明作进一步说明，但所举实施例不作为对本发明的限定。
压陷性能按照GB/T 10807-2006测试方法B法进行，密度按照GB6343-1995测试方法进行。
实施例1
将聚合度为1700、醇解度为88％聚乙烯醇粉末10份与200份纯净水混合，室温溶胀24h后，在60℃下真空搅拌1h后得到聚乙烯醇溶液，记为A；将AH-1618水性聚氨酯10份、AH-1509增稠剂2份、淀粉3份，搅拌1h后，在-0.095MPa真空条件下，继续搅拌1h得到均匀溶液，记为B；最后将A、B两种溶液按照质量比1:1真空混合均匀后，浇注于涂有涂膜剂的模具中，在-25℃冷冻6h后，将样品取出转移至冷冻干燥机中在-80℃冷冻干燥24h得到水溶性泡沫。
实施例2
将聚合度为1700、醇解度为88％聚乙烯醇粉末10份与150份纯净水混合，室温溶胀24h后，在60℃下真空搅拌1h后得到聚乙烯醇水溶液，记为A；将AH-1618水性聚氨酯10份、AH-1509增稠剂2份、淀粉3份混合，搅拌1h后，在-0.095MPa真空条件下，继续搅拌1h得到均匀溶液，记为B；最后将A、B两种溶液按照质量比1：1真空混合均匀后，浇注于涂有涂膜剂的模具中，在-25℃冷冻6h后，将样品取出转移至冷冻干燥机中在-80℃冷冻干燥24h得到水溶性泡沫。
实施例3
将聚合度为1700、醇解度为88％聚乙烯醇粉末10份与150份纯净水混合，室温溶胀24h后，在60℃下真空搅拌1h后得到聚乙烯醇水溶液，记为A；将Leasys 5218水性聚氨酯18份、Vesmody U905增稠剂1份、海藻酸钠3份混后，搅拌1h后，在-0.095MPa真空条件下，继续搅拌1h得到均匀溶液，记为B；最后将A、B两种溶液按照质量比1:1真空混合均匀后，浇注于涂有涂膜剂的模具中，在-25℃冷冻6h后，将样品取出转移至冷冻干燥机中在-80℃冷冻干燥24h得到水溶性泡沫。
实施例4
将聚合度为1700、醇解度为78％聚乙烯醇粉末15份与150份纯净水混合，室温溶胀24h后，在50℃下真空搅拌1h后得到聚乙烯醇水溶液，记为A；将Leasys 1258水性聚氨酯10份、Vesmody U505增稠剂2份、海藻酸钠5份混合，搅拌1h后，在-0.095MPa真空条件下，继续搅拌1h得到均匀溶液，记为B；最后将A、B两种溶液按照质量比1:1浇注于涂有涂膜剂的模具中，在-25℃冷冻6h后，将样品取出转移至冷冻干燥机中在-80℃冷冻干燥24h得到水溶性泡沫。
实施例5
将聚合度为1700、醇解度为78％聚乙烯醇粉末15份与200份纯净水混合，室温溶胀24h后，在50℃下真空搅拌1h后得到聚乙烯醇水溶液，记为A；将Leasys 1258水性聚氨酯10份、Vesmody U505增稠剂2份、聚丙烯酸钠5份混合，搅拌1h后，在-0.095MPa真空条件下，继续搅拌1h得到均匀溶液，记为B；最后将A、B两种溶液按照质量比2:1浇注于涂有涂膜剂的模具中，在-25℃冷冻6h后，将样品取出转移至冷冻干燥机中在-80℃冷冻干燥24h得到水溶性泡沫。
对比例1
将聚合度为2400、醇解度为88％聚乙烯醇粉末10份与200份纯净水混合，室温溶胀24h后，在60℃下真空搅拌1h后得到聚乙烯醇水溶液，记为A；将Leasys 1258水性聚氨酯10份、Vesmody U505增稠剂2份、淀粉3份混合，搅拌1h后，在-0.095MPa真空条件下，继续搅拌1h得到均匀溶液，记为B；最后将A、B两种溶液按照质量比2:1浇注于涂有涂膜剂的模具中，在-25℃冷冻6h后，将样品取出转移至冷冻干燥机中在-80℃冷冻干燥24h得到水溶性泡沫。
对比例2
将聚合度为1700、醇解度为88％聚乙烯醇粉末3份与200份纯净水混合，室温溶胀24h后，在50℃下搅拌1h后得到聚乙烯醇水溶液，记为A；将Leasys 5218水性聚氨酯20份、Vesmody U505增稠剂2份、海藻酸钠3份混合，搅拌1h后，在-0.095MPa真空条件下，继续搅拌1h得到均匀溶液，记为B；最后将A、B两种溶液按照质量比6:1浇注于涂有涂膜剂的模具中，在-25℃冷冻6h后，将样品取出转移至冷冻干燥机中在-80℃冷冻干燥24h得到水溶性泡沫。
表1实施例1-5、对比例1-2泡沫性能
| 性能实例 | 25％压陷硬度/N | 孔径/mm | 密度/kg/m<sup>3</sup> | 水溶解性 |
| 实例1 | 137 | 0.354 | 54 | 好 |
| 实例2 | 133 | 0.432 | 47 | 好 |
| 实例3 | 121 | 0.459 | 45 | 好 |
| 实例4 | 110 | 0.416 | 51 | 好 |
| 实例5 | 116 | 0.389 | 46 | 好 |
| 对比例1 | 370 | 0.504 | 52 | 差 |
| 对比例2 | 155 | 0.521 | 55 | 无 |
上述实施例为本发明较佳的实施方式，但本发明的实施方式不受上述实施例的限制，其他的任何未背离本发明精神实质和原理所做的改变、修饰、替代与简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (10)
1.一种水溶性泡沫的制备方法，其特征在于，包括以下步骤：
S1：将5～15份聚乙烯醇在溶解于100～200份水中得到聚乙烯醇溶液，记为A；
S2：将5～20份聚氨酯分散体、1～3份增稠剂和1～10份吸水助剂混合，得到均匀分散液，记为B；
S3：将A、B按照体积比1～5:1进行混合，真空搅拌均匀后浇注于模具中，冷冻干燥得到聚氨酯水溶性泡沫。
2.如权利要求1所述的水溶性泡沫的制备方法，其特征在于，步骤S1中，所述聚乙烯醇溶液是将5～15份聚乙烯醇在100～200份水中溶胀18～36小时，在45～70℃、真空条件下搅拌3～4h得到。
3.如权利要求1所述的水溶性泡沫的制备方法，其特征在于，步骤S1中，所述聚乙烯醇的醇解度70％～95％，聚合度1500～2000。
4.如权利要求1所述的水溶性泡沫的制备方法，其特征在于，步骤S2中，所述聚氨酯分散体为阴离子水性聚氨酯分散体，质量固含量29％～50％。
5.如权利要求4所述的水性泡沫的制备方法，其特征在于，所述阴离子水性聚氨酯分散体固化后薄膜100％模量≤3MPa。
6.如权利要求1所述的水溶性泡沫的制备方法，其特征在于，步骤S2中，所述增稠剂为水性阴离子缔合型增稠剂。
7.如权利要求1所述的水溶性泡沫的制备方法，其特征在于，步骤S2中，所述吸水助剂为吸水率≥400％的高分子化合物。
8.一种水溶性泡沫，其特征在于，根据权利要求1-7任一项所述的水溶性泡沫的制备方法制备得到的水溶性泡沫。
9.如权利要求8所述的水溶性泡沫，其特征在于，所述水溶性泡沫的25％压陷硬度为100-150N，平均孔径0.3-0.5mm，密度40-70kg/m3。
10.根据权利要求8所述的水溶性泡沫在止血类医用耗材中的应用。
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