CN107286669A - 一种表面亲水抗菌医用硅橡胶的制备方法 - Google Patents
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Abstract
本发明公开了一种表面亲水抗菌医用硅橡胶的制备方法,属于医用材料制备技术领域。本发明先将毛竹粉碎后加入酵母粉混合发酵后收集发酵物,浸泡在阳离子表面活性剂溶液中,再将甲基乙烯基硅橡胶加入混炼机中,并依次加入浸泡后的发酵物、硫化剂、硫化促进剂及乳酸进行混炼,出料得胶料,并将胶料压片后进行辐射硫化,制得改性甲基乙烯基硅橡胶,使用氩气对硅橡胶表面进行等离子体处理后用亲水性溶液浸泡,最后将硅橡胶取出自然风干,即可得表面亲水抗菌医用硅橡胶,本发明制得的医用硅橡胶生物相容性及环保性较好,同时抗菌能力强,与人体器官之间界面摩擦较小,能提高硅橡胶制品的使用安全性,延长其使用寿命,具有广阔的应用前景。
Description
技术领域
本发明公开了一种表面亲水抗菌医用硅橡胶的制备方法,属于医用材料制备技术领域。
背景技术
随着社会的发展,应用于医疗卫生领域的橡胶制品种类越来越多,如各种药剂瓶胶塞、无菌注射器用活塞、注射用密封胶封、软管、导管、医用气垫、灭菌橡胶医用手套、婴儿奶嘴、输血胶管等。在众多的合成橡胶中,硅橡胶是在其中的佼佼者。
硅橡胶是指主链由硅和氧原子交替构成,硅原子上通常连有两个有机基团的橡胶。其具有以下优点:(1)耐低温性能良好,一般在-55℃下仍能工作;(2)耐热性能突出,在180℃下可长期工作,稍高于200℃也能承受数周或更长时间仍有弹性,瞬时可耐300℃以上的高温;(3)透气性好,氧气透过率在合成聚合物中是最高的;(4)具有生理惰性、不会导致凝血的突出特性。由于具有了这些优异的性能,使得硅橡胶在现代医学中发挥了重要作用。
随着现代医学技术和生产的迅速发展,对医用硅橡胶产品的性能提出了更高的要求。而目前现有的医用硅橡胶制品,其生物相容性及产品环保性较差,使用寿命较短,且由于硅橡胶表面疏水,导致材料与人体器官之间界面摩擦较大,容易引起细菌繁殖,使用安全性不强。因此如何克服现有技术的不足,寻求一种综合性能优异的硅橡胶成为业内亟待解决的问题。
发明内容
本发明主要解决的技术问题:针对现有的医用硅橡胶生物相容性及环保性较差,使用寿命较短,且由于硅橡胶表面疏水,导致硅橡胶与人体器官之间界面摩擦较大,容易引起细菌繁殖,使用安全性不强的缺陷,提供了一种表面亲水抗菌医用硅橡胶的制备方法。
为了解决上述技术问题,本发明所采用的技术方案是:
(1)称取毛竹,晒干后破碎,过筛,得毛竹粉末,向毛竹粉末中加入水和酵母粉,搅拌厌氧发酵,发酵结束后收集发酵物;
(2)按质量比1:5将发酵物加入十二烷基三甲基氯化铵溶液中浸泡,浸泡后过滤得滤渣,干燥得干燥物;
(3)按重量份数计,分别选取100~120份甲基乙烯基硅橡胶生胶101、20~30份干燥物、3~5份过氧化二异丙苯、2~4份硬脂酸和3~5份乳酸,加入双辊混炼机中混炼得胶料;
(4)将胶料放置平板硫化机上,压制成胶料片,置于电子束辐照装置中,辐射硫化处理后得改性甲基乙烯基硅橡胶;
(5)按质量比1:10将改性甲基乙烯基硅橡胶加入无水乙醇中浸泡,浸泡后过滤得滤饼,将滤饼放置等离子体装置内,并通入氩气进行等离子体处理,得活化甲基乙烯基硅橡胶;
(6)按质量比1:5:3,分别称取脂肪酸蔗糖酯、无水乙醇中和丙三醇,混合20~30min后得亲水性溶液;
(7)按质量比1:5,将活化甲基乙烯基硅橡胶加入亲水性溶液中浸泡,浸泡后取出固体并风干,即可得表面亲水抗菌医用硅橡胶。
2.根据权利要求1所述的一种表面亲水抗菌医用硅橡胶的制备方法,其特征在于:步骤(1)中所述水的质量为毛竹粉末质量40~50%,酵母粉质量为毛竹粉末质量5~10%。
步骤(1)中所述的厌氧发酵温度为40~43℃,厌氧发酵时间为5~7天。
步骤(2)中十二烷基三甲基氯化铵溶液的质量分数为5%。
步骤(3)中混炼机的温度为100~120℃。
步骤(4)中平板硫化机的温度为100~120℃,压力为5~10MPa。
步骤(4)中所述的电子束辐照装置中的电子束能量为20~30keV,辐射硫化时间为20~30s。
步骤(5)中所述的等离子体装置的功率为200~300W,温度为100~120℃。
本发明的有益效果是:
(1)本发明将毛竹粉碎后发酵,并将发酵物浸泡在阳离子表面活性剂中,可以提高发酵物中的纤维素与硅橡胶间的相容性,接枝在硅橡胶后可以提高硅橡胶的表面亲水性;
(2)本发明利用等离子体对硅橡胶表面改性,目的是在硅橡胶表面引入各种极性基团,提高亲水性,并且等离子体处理对硅橡胶表面具有明显的杀菌作用;
(3)本发明将等离子体处理后的硅橡胶浸泡在亲水性溶液中,接枝亲水基团在硅橡胶表面,提高硅橡胶表面的亲水性,使硅橡胶与人体器官之间界面吻合度较高,可有效提高医用硅橡胶产品的使用安全性;
(4)本发明制得的医用硅橡胶不仅具有良好的力学性能、抗老化性,同时抗菌能力强,与人体器官之间界面摩擦较小,具有无毒、无刺激性、对生物体安全性高的特点。
具体实施方式
称取2~4kg毛竹,晒干后加入竹子破碎机中破碎,破碎后过70~80目筛,得毛竹粉末,向毛竹粉末中加入毛竹粉末质量40~50%水和毛竹粉末质量5~10%酵母粉,搅拌混合20~30min后加入发酵罐中并密封罐口,在40~43℃下厌氧发酵5~7天,发酵结束后收集发酵物,按质量比1:5将发酵物加入质量分数为5%十二烷基三甲基氯化铵溶液中浸泡,浸泡5~10h后过滤得滤渣,将滤渣放入烘箱中,在60~70℃温度下干燥8~10h,得干燥物,按重量份数计,分别选取100~120份甲基乙烯基硅橡胶生胶101、20~30份干燥物、3~5份过氧化二异丙苯、2~4份硬脂酸和3~5份乳酸,加入双辊混炼机中,在20~50r/min转速下混炼3~5min,随后设置混炼机的温度为100~120℃,在40~80r/min转速下混炼20~30min,混炼后出料得胶料,将胶料放置平板硫化机上,在100~120℃温度下以5~10MPa压力压制成3~5mm厚的胶料片,将胶料片置于电子束辐照装置中,在电子束能量为20~30keV的条件下进行辐射硫化处理20~30s,处理后得改性甲基乙烯基硅橡胶,按质量比1:10将改性甲基乙烯基硅橡胶加入无水乙醇中浸泡,浸泡40~60min后过滤得滤饼,将滤饼放置等离子体装置内,并向等离子体装置内通入氩气,通气速率为30~50mL/min,通入20~30min后停止通入氩气,并在功率为200~300W,温度为100~120℃的条件下对滤饼进行等离子体处理,处理60~90s后得活化甲基乙烯基硅橡胶,按质量比1:5:3,分别称取脂肪酸蔗糖酯、无水乙醇中和丙三醇,混合20~30min后得亲水性溶液,按质量比1:5,将活化甲基乙烯基硅橡胶加入亲水性溶液中浸泡,浸泡20~24h后取出固体并自然风干,即可得表面亲水抗菌医用硅橡胶。
实例1
称取2kg毛竹,晒干后加入竹子破碎机中破碎,破碎后过70目筛,得毛竹粉末,向毛竹粉末中加入毛竹粉末质量40%水和毛竹粉末质量5%酵母粉,搅拌混合20min后加入发酵罐中并密封罐口,在40℃下厌氧发酵5天,发酵结束后收集发酵物,按质量比1:5将发酵物加入质量分数为5%十二烷基三甲基氯化铵溶液中浸泡,浸泡5h后过滤得滤渣,将滤渣放入烘箱中,在60℃温度下干燥8h,得干燥物,按重量份数计,分别选取100份甲基乙烯基硅橡胶生胶101、20份干燥物、3份过氧化二异丙苯、2份硬脂酸和3份乳酸,加入双辊混炼机中,在20r/min转速下混炼3min,随后设置混炼机的温度为100℃,在40r/min转速下混炼20min,混炼后出料得胶料,将胶料放置平板硫化机上,在100℃温度下以5MPa压力压制成3mm厚的胶料片,将胶料片置于电子束辐照装置中,在电子束能量为20keV的条件下进行辐射硫化处理20s,处理后得改性甲基乙烯基硅橡胶,按质量比1:10将改性甲基乙烯基硅橡胶加入无水乙醇中浸泡,浸泡40min后过滤得滤饼,将滤饼放置等离子体装置内,并向等离子体装置内通入氩气,通气速率为30mL/min,通入20min后停止通入氩气,并在功率为200W,温度为100℃的条件下对滤饼进行等离子体处理,处理60s后得活化甲基乙烯基硅橡胶,按质量比1:5:3,分别称取脂肪酸蔗糖酯、无水乙醇中和丙三醇,混合20min后得亲水性溶液,按质量比1:5,将活化甲基乙烯基硅橡胶加入亲水性溶液中浸泡,浸泡20h后取出固体并自然风干,即可得表面亲水抗菌医用硅橡胶。
实例2
称取3kg毛竹,晒干后加入竹子破碎机中破碎,破碎后过75目筛,得毛竹粉末,向毛竹粉末中加入毛竹粉末质量45%水和毛竹粉末质量8%酵母粉,搅拌混合25min后加入发酵罐中并密封罐口,在42℃下厌氧发酵6天,发酵结束后收集发酵物,按质量比1:5将发酵物加入质量分数为5%十二烷基三甲基氯化铵溶液中浸泡,浸泡8h后过滤得滤渣,将滤渣放入烘箱中,在65℃温度下干燥9h,得干燥物,按重量份数计,分别选取110份甲基乙烯基硅橡胶生胶101、25份干燥物、4份过氧化二异丙苯、3份硬脂酸和4份乳酸,加入双辊混炼机中,在35r/min转速下混炼4min,随后设置混炼机的温度为110℃,在60r/min转速下混炼25min,混炼后出料得胶料,将胶料放置平板硫化机上,在110℃温度下以8MPa压力压制成4mm厚的胶料片,将胶料片置于电子束辐照装置中,在电子束能量为25keV的条件下进行辐射硫化处理25s,处理后得改性甲基乙烯基硅橡胶,按质量比1:10将改性甲基乙烯基硅橡胶加入无水乙醇中浸泡,浸泡50min后过滤得滤饼,将滤饼放置等离子体装置内,并向等离子体装置内通入氩气,通气速率为40mL/min,通入25min后停止通入氩气,并在功率为250W,温度为110℃的条件下对滤饼进行等离子体处理,处理75s后得活化甲基乙烯基硅橡胶,按质量比1:5:3,分别称取脂肪酸蔗糖酯、无水乙醇中和丙三醇,混合25min后得亲水性溶液,按质量比1:5,将活化甲基乙烯基硅橡胶加入亲水性溶液中浸泡,浸泡22h后取出固体并自然风干,即可得表面亲水抗菌医用硅橡胶。
实例3
称取4kg毛竹,晒干后加入竹子破碎机中破碎,破碎后过80目筛,得毛竹粉末,向毛竹粉末中加入毛竹粉末质量50%水和毛竹粉末质量10%酵母粉,搅拌混合30min后加入发酵罐中并密封罐口,在43℃下厌氧发酵7天,发酵结束后收集发酵物,按质量比1:5将发酵物加入质量分数为5%十二烷基三甲基氯化铵溶液中浸泡,浸泡10h后过滤得滤渣,将滤渣放入烘箱中,在70℃温度下干燥10h,得干燥物,按重量份数计,分别选取120份甲基乙烯基硅橡胶生胶101、30份干燥物、5份过氧化二异丙苯、4份硬脂酸和5份乳酸,加入双辊混炼机中,在50r/min转速下混炼5min,随后设置混炼机的温度为120℃,在80r/min转速下混炼30min,混炼后出料得胶料,将胶料放置平板硫化机上,在120℃温度下以10MPa压力压制成5mm厚的胶料片,将胶料片置于电子束辐照装置中,在电子束能量为30keV的条件下进行辐射硫化处理30s,处理后得改性甲基乙烯基硅橡胶,按质量比1:10将改性甲基乙烯基硅橡胶加入无水乙醇中浸泡,浸泡60min后过滤得滤饼,将滤饼放置等离子体装置内,并向等离子体装置内通入氩气,通气速率为50mL/min,通入30min后停止通入氩气,并在功率为300W,温度为120℃的条件下对滤饼进行等离子体处理,处理90s后得活化甲基乙烯基硅橡胶,按质量比1:5:3,分别称取脂肪酸蔗糖酯、无水乙醇中和丙三醇,混合30min后得亲水性溶液,按质量比1:5,将活化甲基乙烯基硅橡胶加入亲水性溶液中浸泡,浸泡24h后取出固体并自然风干,即可得表面亲水抗菌医用硅橡胶。
对实例1~3制得的表面亲水抗菌医用硅橡胶与市售医用硅橡胶(对比例)进行性能检测,其检测结果如下表1:
表1
综上所述,本发明制得的表面亲水抗菌医用硅橡胶抗菌性能较好,还具有较好的生物相容性,使用后对人体无刺激反应,不会对人体健康造成损害,且硅橡胶压缩变性率较小,力学性能优良,有效提高了硅橡胶使用寿命。
Claims (8)
1.一种表面亲水抗菌医用硅橡胶的制备方法,其特征在于具体制备步骤为:
(1)称取毛竹,晒干后破碎,过筛,得毛竹粉末,向毛竹粉末中加入水和酵母粉,搅拌厌氧发酵,发酵结束后收集发酵物;
(2)按质量比1:5将发酵物加入十二烷基三甲基氯化铵溶液中浸泡,浸泡后过滤得滤渣,干燥得干燥物;
(3)按重量份数计,分别选取100~120份甲基乙烯基硅橡胶生胶101、20~30份干燥物、3~5份过氧化二异丙苯、2~4份硬脂酸和3~5份乳酸,加入双辊混炼机中混炼得胶料;
(4)将胶料放置平板硫化机上,压制成胶料片,置于电子束辐照装置中,辐射硫化处理后得改性甲基乙烯基硅橡胶;
(5)按质量比1:10将改性甲基乙烯基硅橡胶加入无水乙醇中浸泡,浸泡后过滤得滤饼,将滤饼放置等离子体装置内,并通入氩气进行等离子体处理,得活化甲基乙烯基硅橡胶;
(6)按质量比1:5:3,分别称取脂肪酸蔗糖酯、无水乙醇中和丙三醇,混合20~30min后得亲水性溶液;
(7)按质量比1:5,将活化甲基乙烯基硅橡胶加入亲水性溶液中浸泡,浸泡后取出固体并风干,即可得表面亲水抗菌医用硅橡胶。
2.根据权利要求1所述的一种表面亲水抗菌医用硅橡胶的制备方法,其特征在于:步骤(1)中所述水的质量为毛竹粉末质量40~50%,酵母粉质量为毛竹粉末质量5~10%。
3.根据权利要求1所述的一种表面亲水抗菌医用硅橡胶的制备方法,其特征在于:步骤(1)中所述的厌氧发酵温度为40~43℃,厌氧发酵时间为5~7天。
4.根据权利要求1所述的一种表面亲水抗菌医用硅橡胶的制备方法,其特征在于:步骤(2)中十二烷基三甲基氯化铵溶液的质量分数为5%。
5.根据权利要求1所述的一种表面亲水抗菌医用硅橡胶的制备方法,其特征在于:步骤(3)中混炼机的温度为100~120℃。
6.根据权利要求1所述的一种表面亲水抗菌医用硅橡胶的制备方法,其特征在于:步骤(4)中平板硫化机的温度为100~120℃,压力为5~10MPa。
7.根据权利要求1所述的一种表面亲水抗菌医用硅橡胶的制备方法,其特征在于:步骤(4)中所述的电子束辐照装置中的电子束能量为20~30keV,辐射硫化时间为20~30s。
8.据权利要求1所述的一种表面亲水抗菌医用硅橡胶的制备方法,其特征在于:步骤(5)中所述的等离子体装置的功率为200~300W,温度为100~120℃。
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