CN110358228B - 一种高阻隔阻燃珍珠母/聚偏氯乙烯乳液及其制备方法 - Google Patents
一种高阻隔阻燃珍珠母/聚偏氯乙烯乳液及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种增强的高阻隔阻燃珍珠母/聚偏氯乙烯乳液的制备方法。以珍珠母为协调剂,通过原位聚合的方法制备聚偏氯乙烯高阻隔阻燃乳液,珍珠母特殊的层状结构使其具有极高的强度、硬度与良好韧性,以此为协调剂的聚偏氯乙烯乳液具有高阻隔性,高阻燃性,良好的耐腐蚀以及增强基材的力学性能的特性。方法制备简单,产品成本低,可以广泛应用在食品、衣物、化妆品等领域。
Description
技术领域
本发明属于食品、药品、烟草、茶叶等包装领域,具体涉及一种高阻隔阻燃珍珠母/聚偏氯乙烯乳液及其制备方法。
背景技术
聚偏氯乙烯(Polyvinylidene chloride)简称PVDC,偏氯乙烯的均聚物和共聚物习惯上称为莎纶树脂,其商业聚合物是偏氯乙烯(VDC)与氯乙烯、丙烯酸酯或丙烯睛的共聚物。共聚单体的选择对于共聚物的性质影响很大,共聚物的形态应根据熔融加工、溶液涂敷、分散涂敷等加工方式来确定。聚偏氯乙烯的显著特性是气、液低透性、阻隔性及耐化学特性,使其在食品、衣物、纺织品等领域有着广泛应用。珍珠母是由文石相碳酸钙与有机质几丁质与蚕丝蛋白组成,其独特的有机无机杂化复合结构赋予其在聚合物中更好的分散性与相容性。以珍珠母复配聚偏氯乙烯制备兼具阻燃、阻隔、耐腐蚀增强型乳液的研究报道几乎没有。
发明内容
本发明的目的在于提供一种高阻隔阻燃珍珠母/聚偏氯乙烯乳液及其制备方法,本发明提供的高阻隔阻燃珍珠母/聚偏氯乙烯乳液具有高阻隔性、高阻燃性、良好的耐腐蚀以及增强基材的力学性能等特性。
本发明提供了一种高阻隔阻燃珍珠母/聚偏氯乙烯乳液,由以下重量百分比的原料制成:偏氯乙烯70~90重量份、丙烯酸甲酯3~8重量份、甲基丙烯酸甲酯3~5重量份、丙烯氰3~5重量份、丙烯酸3~5重量份、引发剂1~3重量份、乳化剂1~15重量份、珍珠母3~15重量份、pH调节剂1~3重量份、缓冲剂1~3重量份。
优选的,所述引发剂为过硫酸钾、过硫酸铵和过硫酸钠中的一种或几种。
优选的,所述乳化剂为十二烷基硫酸钠或十二烷基苯磺酸钠。
优选的,所述缓冲剂为碳酸氢钠、碳酸氢铵和碳酸氢钾中的一种或几种。
优选的,所述珍珠母的粒径为20~200nm。
优选的,所述pH调节剂为盐酸溶液,浓度为0.01mol/L~0.1mol/L。
本发明还提供了一种上述高阻隔阻燃珍珠母/聚偏氯乙烯乳液的制备方法,包括以下步骤:
S1.将珍珠母球磨、烘干,然后放入去离子水中进行超声分散,制备珍珠母分散液;
S2.将所述珍珠母分散液、引发剂、PH调节剂、缓冲剂依次加入反应釜打浆至混合均匀后将所述反应釜抽真空;
S3.将偏氯乙烯、丙烯酸甲酯、甲基丙烯酸甲酯、丙烯氰和丙烯酸以真空方式吸入所述反应釜后,向所述反应釜中充入氮气至所述反应釜中压力为常压;
S4.开启所述反应釜,室温搅拌10~15分钟,升温至60~80℃,然后保温4~6小时;
S5.冷却出料,得高阻隔阻燃珍珠母/聚偏氯乙烯乳液。
优选的,所述步骤S1中球磨时间为24小时。
优选的,所述步骤S4中搅拌速度为500rpm。
与现有技术相比,珍珠母主要是由纳米级的文石与有机质几丁质与蚕丝蛋白组成,文石是一种碳酸钙晶体。它是当海水冲刷一种彼此相连的水平薄片的有机骨架时,从海水中的离子形成的,层层结构规整。根据它的有机晶体成分,珍珠母比其组成材料(文石晶体)的抗撕裂能力高3000倍。因此本发明提供的高阻隔阻燃珍珠母/聚偏氯乙烯乳液具有高阻隔性、高阻燃性、良好的耐腐蚀以及增强基材的力学性能,且制备简单,产品成本低。
具体实施方式
下面将结合本发明实施例,对本发明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的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。
本发明提供了一种高阻隔阻燃珍珠母/聚偏氯乙烯乳液,由以下重量百分比的原料制成:偏氯乙烯70~90重量份、丙烯酸甲酯3~8重量份、甲基丙烯酸甲酯3~5重量份、丙烯氰3~5重量份、丙烯酸3~5重量份、引发剂1~3重量份、乳化剂1~15重量份、珍珠母3~15重量份、pH调节剂1~3重量份、缓冲剂1~3重量份。其中,引发剂优选为过硫酸钾、过硫酸铵和过硫酸钠中的一种或几种。pH调节剂优选为盐酸,浓度为0.01~0.1mol/L。乳化剂优选为十二烷基硫酸钠或十二烷基苯磺酸钠。缓冲剂优选为碳酸氢钠、碳酸氢铵和碳酸氢钾中的一种或几种。珍珠母的粒径优选为20~200nm。
本发明还提供了一种上述高阻隔阻燃珍珠母/聚偏氯乙烯乳液的制备方法,包括以下步骤:
S1.将珍珠母球磨并烘干后放入去离子水中进行超声分散,制备珍珠母分散液;
S2.将所述珍珠母分散液、引发剂、PH调节剂、缓冲剂依次加入反应釜后打浆15分钟至混合均匀,然后将反应釜密封,抽真空;
S3.按计量称取单体偏氯乙烯(VDC)、丙烯酸甲酯(MA)、甲基丙烯酸甲酯(MMA)、丙烯氰(AN)、丙烯酸(AA)于加料器中,然后利用反应釜的真空度将单体吸入反应釜中,然后向反应釜中充入氮气至反应釜中压力为常压;
S4.开启反应釜进行搅拌,室温下搅拌10~15分钟,升温至60~80℃,然后保温4~6小时;
S5.冷却出料,得高阻隔阻燃珍珠母/聚偏氯乙烯乳液。
其中,步骤S1中球磨时间优选为24~48小时,更优选为24小时,步骤S4中搅拌速度优选为500rpm~800rpm,更优选为500rpm。
为了进一步理解本发明,下面结合实施例对本发明提供的高阻隔阻燃珍珠母/聚偏氯乙烯乳液进行详细说明,本发明保护范围不受以下实施例的限制。
实施例1
S1.将5g珍珠母球磨24h,烘干,放入10g去离子水中进行超声分散,制备珍珠母分散液;
S2.将得到的珍珠母分散液与1g过硫酸钾、3g盐酸、3g碳酸氢钠、1g十二烷基硫酸钠依次加入反应釜后打浆15分钟至混合均匀,然后将反应釜密封,抽真空;
S3.称取70g偏氯乙烯、3g丙烯酸甲酯、3g甲基丙烯酸甲酯、3g丙烯氰、3g丙烯酸置于加料器中,然后利用反应釜的真空度将放置于加料器中的单体吸入反应釜中,然后向反应釜中充入氮气至反应釜中压力为常压;
S4.开启反应釜进行搅拌,室温下搅拌10分钟,升温至60℃,然后保温4小时;
S5.冷却出料,得高阻隔阻燃珍珠母/聚偏氯乙烯乳液。
实施例2
S1.将5g珍珠母球磨24h,烘干,放入10g去离子水中进行超声分散,制备珍珠母分散液;
S2.将得到的珍珠母分散液与3g过硫酸钠、3g盐酸、3g碳酸氢钠、1g十二烷基硫酸钠依次加入反应釜后打浆15分钟至混合均匀,然后将反应釜密封,抽真空;
S3.称取70g偏氯乙烯、3g丙烯酸甲酯、3g甲基丙烯酸甲酯、3g丙烯氰、3g丙烯酸置于加料器中,然后利用反应釜的真空度将放置于加料器中的单体吸入反应釜中,然后向反应釜中充入氮气至反应釜中压力为常压;
S4.开启反应釜进行搅拌,室温下搅拌10分钟,升温至80℃,然后保温6小时;
S5.冷却出料,得高阻隔阻燃珍珠母/聚偏氯乙烯乳液。
实施例3
S1.将8g珍珠母球磨24h,烘干,放入10g去离子水中进行超声分散,制备珍珠母分散液;
S2.将得到的珍珠母分散液与1g过硫酸铵、3g盐酸、3g碳酸氢钠、1g十二烷基苯磺酸钠依次加入反应釜后打浆15分钟至混合均匀,然后将反应釜密封,抽真空;
S3.称取70g偏氯乙烯、3g丙烯酸甲酯、3g甲基丙烯酸甲酯、3g丙烯氰、3g丙烯酸置于加料器中,然后利用反应釜的真空度将放置于加料器中的单体吸入反应釜中,然后向反应釜中充入氮气至反应釜中压力为常压;
S4.开启反应釜进行搅拌,室温下搅拌10分钟,升温至60℃,然后保温4小时;
S5.冷却出料,得高阻隔阻燃珍珠母/聚偏氯乙烯乳液。
实施例4
S1.将10g珍珠母球磨24h,烘干,放入10g去离子水中进行超声分散,制备珍珠母分散液;
S2.将得到的珍珠母分散液与1g过硫酸钾、3g盐酸、3g碳酸氢钾、6g十二烷基苯磺酸钠依次加入反应釜后打浆15分钟至混合均匀,然后将反应釜密封,抽真空;
S3.称取70g偏氯乙烯、3g丙烯酸甲酯、3g甲基丙烯酸甲酯、3g丙烯氰、3g丙烯酸置于加料器中,然后利用反应釜的真空度将放置于加料器中的单体吸入反应釜中,然后向反应釜中充入氮气至反应釜中压力为常压;
S4.开启反应釜进行搅拌,室温下搅拌15分钟,升温至60℃,然后保温4小时;
S5.冷却出料,得高阻隔阻燃珍珠母/聚偏氯乙烯乳液。
实施例5
S1.将10g珍珠母球磨24h,烘干,放入10g去离子水中进行超声分散,制备珍珠母分散液;
S2.将得到的珍珠母分散液与1g过硫酸铵、3g盐酸、3g碳酸氢铵、8g十二烷基苯磺酸钠依次加入反应釜后打浆15分钟至混合均匀,然后将反应釜密封,抽真空;
S3.称取70g偏氯乙烯、3g丙烯酸甲酯、3g甲基丙烯酸甲酯、3g丙烯氰、3g丙烯酸置于加料器中,然后利用反应釜的真空度将放置于加料器中的单体吸入反应釜中,然后向反应釜中充入氮气至反应釜中压力为常压;
S4.开启反应釜进行搅拌,室温下搅拌10分钟,升温至60℃,然后保温4小时;
S5.冷却出料,得高阻隔阻燃珍珠母/聚偏氯乙烯乳液。
取实施例1~5制备的聚偏氯乙烯乳液进行下列多项测试,实验结果见表1和表2:
表1珍珠母/聚偏氯乙烯整理纯棉织物的物理机械性能
表2珍珠母/聚偏氯乙烯整理纯棉织物的阻燃性
由表1和表2可知,随着珍珠母含量的增加,PVDC乳液透气性下降,阻隔性提高,力学性能提升,阻燃性能提高。
上面对本发明的较佳实施方式作了详细说明,但是本发明并不限于上述实施方式,在本领域的普通技术人员所具备的知识范围内,还可以在不脱离本发明宗旨的前提下作出各种变化。
Claims (9)
1.一种高阻隔阻燃珍珠母/聚偏氯乙烯乳液,其特征在于,由以下重量份的原料制成:偏氯乙烯70~90重量份、丙烯酸甲酯3~8重量份、甲基丙烯酸甲酯3~5重量份、丙烯氰3~5重量份、丙烯酸3~5重量份、引发剂1~3重量份、乳化剂1~15重量份、珍珠母3~15重量份、pH调节剂1~3重量份、缓冲剂1~3重量份。
2.根据权利要求1所述的高阻隔阻燃珍珠母/聚偏氯乙烯乳液,其特征在于:所述引发剂为过硫酸钾、过硫酸铵和过硫酸钠中的一种或几种。
3.根据权利要求1所述的高阻隔阻燃珍珠母/聚偏氯乙烯乳液,其特征在于:所述乳化剂为十二烷基硫酸钠或十二烷基苯磺酸钠。
4.根据权利要求1所述的高阻隔阻燃珍珠母/聚偏氯乙烯乳液,其特征在于:所述缓冲剂为碳酸氢钠、碳酸氢铵和碳酸氢钾中的一种或几种。
5.根据权利要求1所述的高阻隔阻燃珍珠母/聚偏氯乙烯乳液,其特征在于:所述珍珠母的粒径为20~200nm。
6.根据权利要求1所述的高阻隔阻燃珍珠母/聚偏氯乙烯乳液,其特征在于:所述pH调节剂为盐酸溶液,浓度为0.01mol/L~0.1mol/L。
7.一种应用于权利要求1~6中任一项所述的高阻隔阻燃珍珠母/聚偏氯乙烯乳液的制备方法,其特征在于,包括以下步骤:
S1.将珍珠母球磨、烘干,然后放入去离子水中进行超声分散,制备珍珠母分散液;
S2.将所述珍珠母分散液、引发剂、pH调节剂、缓冲剂、乳化剂依次加入反应釜打浆至混合均匀后将所述反应釜抽真空;
S3.将偏氯乙烯、丙烯酸甲酯、甲基丙烯酸甲酯、丙烯氰和丙烯酸以真空方式吸入所述反应釜后,向所述反应釜中充入氮气至所述反应釜中压力为常压;
S4.开启所述反应釜,室温搅拌10~15分钟,升温至60~80℃,然后保温4~6小时;
S5.冷却出料,得高阻隔阻燃珍珠母/聚偏氯乙烯乳液。
8.根据权利要求7所述的高阻隔阻燃珍珠母/聚偏氯乙烯乳液的制备方法,其特征在于,所述步骤S1中球磨时间为24~48小时。
9.根据权利要求7所述的高阻隔阻燃珍珠母/聚偏氯乙烯乳液的制备方法,其特征在于,所述步骤S4中搅拌速度为500rpm~800rpm。
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