CN107088368B - 一种结构均匀、高透气性过滤用微孔膜及其制备方法 - Google Patents
一种结构均匀、高透气性过滤用微孔膜及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种结构均匀、高透气性过滤用微孔膜,它是由下述重量份的原料组成的:聚乙烯100‑110、丙烯腈27‑30、过氧化二异丙苯0.1‑0.2、增塑剂2‑4、三氧化二锑1‑2、硼酸锌0.8‑1、抗氧化剂1‑2、热稳定剂0.8‑2、辛基异噻唑啉酮1‑2、丙酸钙1‑3、异氰尿酸三缩水甘油酯0.7‑2、二丙酮醇4‑6、油酸二乙醇酰胺0.7‑1、肉豆蔻酸钠皂0.5‑1、羟基乙酸1‑2,本发明的工艺技术与其它现有工艺相比,工艺简单,产量高,适合大规模连续生产,高效的生产效率降低了生产成本;并且本发明采用的是聚烯烃,原料价格便宜,最终空气过滤膜成本将大大降低。
Description
技术领域
本发明涉及过滤膜材料领域,具体涉及一种结构均匀、高透气性过滤用微孔膜及其制备方法。
背景技术
近年来随着雾霾、沙尘暴等环境恶化,无论身在家庭还是公众场所,人们的身体健康都受到严重危害。另外,由于生活水平提高,空调的普及使用,进入千家万户,夏天长时间使用空调的封闭空间里空气浑浊,质量及其恶劣,导致人们出现越来越多的空调综合征,如睡眠质量不好、免疫力下降等诸多严重影响身体健康的情形。冬天即使不使用空调,家庭里长期封闭门窗也有同样的问题。因此,针对此现象,美国能源部所属佛罗里达研发中心率先开发了“珀丽优”天幕系统,即空气净化补充系统,在封闭的环境中实现新鲜空气的持续净化和氧气补充,解决了因环境空气质量下降带来的诸多亚健康问题。
空气净化补充系统采用空气过滤膜对室外空气中PM2.5微尘和细菌、微生物等有毒物质进行过滤后补充到室内,同时将室内的浑浊空气抽出室外,实现持续的净化和补充,保持室内空气的质量和氧气的充足。目前应用于“珀丽优”天幕系统的空气过滤膜主要有美国ENTEC、 PPG公司产品。
空气过滤用品例如口罩、空气过滤器、防毒面具等在维护人类的绿色生活和身体健康中逐步占领重要地位。空气过滤膜必须具有将空气中的固体有害物质截留或是与之发生吸附反应等作用,才能达到净化空气,保证人类健康之目的。目前,市场上的日用、医用空气过滤膜,例如口罩、空气过滤器、防毒面具等,多数采用静电纺丝方法制备。比如,CN103480285A 公开了一种增强聚砜纳米纤维空气过滤膜及其静电纺丝制备方法,CN104368245A同样公开了一种静电纺丝空气过滤膜及其制备方法。但是,静电纺丝制备得到的空气过滤膜,机械强度低,使用过程中很容易损伤,且长期使用的抗形变能力及耐热性较差,同时使用静电纺丝工艺制备空气过滤膜效率较低。
本发明通过研究发现,采用熔融挤出拉伸法制备的聚烯烃空气过滤用微孔膜,该微孔膜两侧复合PET无纺布层或玻璃纤维针刺毡,对于PM2.5过滤效果更为显著,同时使用过程中不易损伤,且长期使用的抗形变能力及耐热性较强。
发明内容
本发明的目的在于提供一种用于空气过滤系统、能够有效过滤PM2.5的聚烯烃空气过滤用微孔膜及其制备方法。该微孔膜厚度在机械强度高,微孔分布均匀,对其PM2.5过滤效率高达90%以上。
为实现上述目的,本发明采用以下技术方案:
一种结构均匀、高透气性过滤用微孔膜,它是由下述重量份的原料组成的:
聚乙烯100-110、丙烯腈27-30、过氧化二异丙苯0.1-0.2、增塑剂2-4、三氧化二锑1-2、硼酸锌0.8-1、抗氧化剂1-2、热稳定剂0.8-2、辛基异噻唑啉酮1-2、丙酸钙1-3、异氰尿酸三缩水甘油酯0.7-2、二丙酮醇4-6、油酸二乙醇酰胺0.7-1、肉豆蔻酸钠皂0.5-1、羟基乙酸1-2。
所述的抗氧化剂为酚类、胺类、含磷化合物、含硫化合物、有机金属盐中的一种或多种。
所述的热稳定剂为三盐基碳酸铅、二盐基亚磷酸铅,硬脂酸、月桂酸的镉、钡、钙、锌、镁盐、二巯基醋酸异辛酯中的一种或多种。
一种结构均匀、高透气性过滤用微孔膜的制备方法,包括以下步骤:
(1)取辛基异噻唑啉酮,加入到其重量17-20倍的去离子水中,搅拌均匀,加入丙酸钙,升高温度为40-50℃,保温搅拌4-9分钟,加入二丙酮醇,继续保温搅拌10-20分钟,得抑菌乳液;
(2)取肉豆蔻酸钠皂,加入到其重量6-9倍的无水乙醇中,搅拌均匀,加入羟基乙酸,在70-90℃下保温搅拌20-30分钟,加入异氰尿酸三缩水甘油酯,搅拌至常温,得皂化酯溶液;
(3)取三氧化二锑、硼酸锌混合,加入到混合料重量26-30倍的去离子水中,搅拌均匀,加入油酸二乙醇酰胺,在40-50℃下保温搅拌10-20分钟,得阻燃酰胺分散液;
(4)取丙烯腈,加入到上述抑菌乳液中,搅拌均匀,送入到反应釜中,调节反应釜温度为76-80℃,通入氮气,加入过氧化二异丙苯,保温搅拌1-2小时,出料,与上述皂化酯溶液混合,搅拌均匀,蒸馏除去乙醇,送入到烘箱中,在86-90℃下干燥40-50分钟,出料冷却,得高粘度聚丙烯腈;
(5)取热稳定剂,加入到上述阻燃酰胺分散液中,搅拌均匀,加入上述高粘度聚丙烯腈,在60-70℃下保温搅拌30-40分钟,得阻燃聚丙烯腈酰胺分散液;
(6)取上述阻燃聚丙烯腈酰胺分散液,与聚乙烯、增塑剂、抗氧化剂混合,搅拌均匀,脱水,送入到挤出机中,在温度为200-240℃的条件下熔融塑化均匀成熔体;
(7)将所得熔体从模头挤出的铸片,随后进入流延工序,模头温度为185-240℃,流延温度为50-110℃,制备出厚度在8-40μm的中间体膜Ⅰ;
(8)将中间体膜Ⅰ进行微张力下退火处理,退火温度为90-160℃,膜在退火设备中的速度为1-20m/min,纵向张力0.1-3.0N,纵向的拉伸比为1.0-2.0,退火时间5-60min,得到中间体膜Ⅱ;
(9)将中间体膜Ⅱ进行纵向延伸开孔,温度为100-150℃,速比为0.5-3.0,得到中间体膜Ⅲ。
(10)将中间体膜Ⅲ进行回缩定型,回缩比为1.0-1.5,定型温度为100-160℃,得到中间体膜Ⅳ;
(11)将中间体膜Ⅳ进行纵向二次延伸开孔,温度为100-140℃,速比为0.5-2.0,得到所述结构均匀、高透气性过滤用微孔膜。
本发明的优点:
本发明采用熔融挤出拉伸法制备得到的聚烯烃空气过滤膜用微孔膜,生产过程中能够通过调节熔体的粘度、拉伸倍率、热处理退火温度等来精确控制微孔膜的厚度、孔径分布及孔径通透性,其制备的空气过滤膜对于PM2.5过滤效果尤其显著,其PM2.5过滤效率高达90%以上,尤其本发明优选的技术方案过滤效率高达95%,远远高于现有技术80%左右的过滤效率;
采用本发明制备的空气过滤膜用微孔膜,机械强度,如拉伸强度,抗穿刺强度等远远大于通过熔纺、静电纺丝等方法制备的纳米纤维膜;
本发明的工艺技术与其它现有工艺相比,工艺简单,产量高,适合大规模连续生产,高效的生产效率降低了生产成本;并且本发明采用的是聚烯烃,原料价格便宜,最终空气过滤膜成本将大大降低;
采用本发明的工艺技术,过程中不适用或者产生小分子液体溶剂,尤其是对环境造成污染影响的成分,具有环境友好性;
本发明采用辛基异噻唑啉酮、丙酸钙混合作为抑菌助剂,得到抑菌乳液,然后以丙烯腈为单体,抑菌乳液为反应溶剂,在过氧化二异丙苯的引发作用下进行聚合,得到的聚合物具有很好的抑菌性能,可以有效的提高成品微孔膜的抑菌性;
本发明采用肉豆蔻酸钠皂在酯化溶液中分散,然后改性处理抑菌聚丙烯腈,可以有效的提高聚合物的黏度,提高成品微孔膜的稳定性强度。
附图说明:
图1:为本发明实施例1制备的微孔隔膜的电镜图片。
具体实施方式
实施例1
一种结构均匀、高透气性过滤用微孔膜,它是由下述重量份的原料组成的:
聚乙烯110、丙烯腈30、过氧化二异丙苯0.2、增塑剂4、三氧化二锑2、硼酸锌1、三乙醇胺2、二盐基亚磷酸铅2、辛基异噻唑啉酮2、丙酸钙3、异氰尿酸三缩水甘油酯2、二丙酮醇6、油酸二乙醇酰胺1、肉豆蔻酸钠皂1、羟基乙酸2。
一种结构均匀、高透气性过滤用微孔膜的制备方法,包括以下步骤:
(1)取辛基异噻唑啉酮,加入到其重量20倍的去离子水中,搅拌均匀,加入丙酸钙,升高温度为50℃,保温搅拌9分钟,加入二丙酮醇,继续保温搅拌20分钟,得抑菌乳液;
(2)取肉豆蔻酸钠皂,加入到其重量9倍的无水乙醇中,搅拌均匀,加入羟基乙酸,在 90℃下保温搅拌30分钟,加入异氰尿酸三缩水甘油酯,搅拌至常温,得皂化酯溶液;
(3)取三氧化二锑、硼酸锌混合,加入到混合料重量30倍的去离子水中,搅拌均匀,加入油酸二乙醇酰胺,在50℃下保温搅拌20分钟,得阻燃酰胺分散液;
(4)取丙烯腈,加入到上述抑菌乳液中,搅拌均匀,送入到反应釜中,调节反应釜温度为80℃,通入氮气,加入过氧化二异丙苯,保温搅拌2小时,出料,与上述皂化酯溶液混合,搅拌均匀,蒸馏除去乙醇,送入到烘箱中,在90℃下干燥50分钟,出料冷却,得高粘度聚丙烯腈;
(5)取热稳定剂,加入到上述阻燃酰胺分散液中,搅拌均匀,加入上述高粘度聚丙烯腈,在70℃下保温搅拌40分钟,得阻燃聚丙烯腈酰胺分散液;
(6)取上述阻燃聚丙烯腈酰胺分散液,与聚乙烯、增塑剂、抗氧化剂混合,搅拌均匀,脱水,送入到挤出机中,在温度为240℃的条件下熔融塑化均匀成熔体;
(7)将所得熔体从模头挤出的铸片,随后进入流延工序,模头温度为240℃,流延温度为110℃,制备出厚度在8-40μm的中间体膜Ⅰ;
(8)将中间体膜Ⅰ进行微张力下退火处理,退火温度为160℃,膜在退火设备中的速度为20m/min,纵向张力3.0N,纵向的拉伸比为2.0,退火时间60min,得到中间体膜Ⅱ;
(9)将中间体膜Ⅱ进行纵向延伸开孔,温度为150℃,速比为3.0,得到中间体膜Ⅲ。
(10)将中间体膜Ⅲ进行回缩定型,回缩比为1.5,定型温度为160℃,得到中间体膜Ⅳ;
(11)将中间体膜Ⅳ进行纵向二次延伸开孔,温度为140℃,速比为2.0,得到所述结构均匀、高透气性过滤用微孔膜。
实施例2
一种结构均匀、高透气性过滤用微孔膜,它是由下述重量份的原料组成的:
聚乙烯100、丙烯腈27、过氧化二异丙苯0.1、增塑剂2、三氧化二锑1、硼酸锌0.8、硫化亚锡1、二巯基醋酸异辛酯0.8、辛基异噻唑啉酮1、丙酸钙1、异氰尿酸三缩水甘油酯 0.7、二丙酮醇4、油酸二乙醇酰胺0.7、肉豆蔻酸钠皂0.5、羟基乙酸1。
一种结构均匀、高透气性过滤用微孔膜的制备方法,包括以下步骤:
(1)取辛基异噻唑啉酮,加入到其重量17倍的去离子水中,搅拌均匀,加入丙酸钙,升高温度为40℃,保温搅拌4分钟,加入二丙酮醇,继续保温搅拌10分钟,得抑菌乳液;
(2)取肉豆蔻酸钠皂,加入到其重量6倍的无水乙醇中,搅拌均匀,加入羟基乙酸,在 70℃下保温搅拌20分钟,加入异氰尿酸三缩水甘油酯,搅拌至常温,得皂化酯溶液;
(3)取三氧化二锑、硼酸锌混合,加入到混合料重量26倍的去离子水中,搅拌均匀,加入油酸二乙醇酰胺,在40℃下保温搅拌10分钟,得阻燃酰胺分散液;
(4)取丙烯腈,加入到上述抑菌乳液中,搅拌均匀,送入到反应釜中,调节反应釜温度为76℃,通入氮气,加入过氧化二异丙苯,保温搅拌1小时,出料,与上述皂化酯溶液混合,搅拌均匀,蒸馏除去乙醇,送入到烘箱中,在86℃下干燥40分钟,出料冷却,得高粘度聚丙烯腈;
(5)取热稳定剂,加入到上述阻燃酰胺分散液中,搅拌均匀,加入上述高粘度聚丙烯腈,在60℃下保温搅拌30分钟,得阻燃聚丙烯腈酰胺分散液;
(6)取上述阻燃聚丙烯腈酰胺分散液,与聚乙烯、增塑剂、抗氧化剂混合,搅拌均匀,脱水,送入到挤出机中,在温度为200℃的条件下熔融塑化均匀成熔体;
(7)将所得熔体从模头挤出的铸片,随后进入流延工序,模头温度为185℃,流延温度为50℃,制备出厚度在8-40μm的中间体膜Ⅰ;
(8)将中间体膜Ⅰ进行微张力下退火处理,退火温度为90℃,膜在退火设备中的速度为10m/min,纵向张力0.1N,纵向的拉伸比为1.0,退火时间5min,得到中间体膜Ⅱ;
(9)将中间体膜Ⅱ进行纵向延伸开孔,温度为100℃,速比为0.5,得到中间体膜Ⅲ。
(10)将中间体膜Ⅲ进行回缩定型,回缩比为1.0,定型温度为100℃,得到中间体膜Ⅳ;
(11)将中间体膜Ⅳ进行纵向二次延伸开孔,温度为100℃,速比为0.5,得到所述结构均匀、高透气性过滤用微孔膜。
实施例3
一种结构均匀、高透气性过滤用微孔膜,它是由下述重量份的原料组成的:
聚乙烯110、丙烯腈27、过氧化二异丙苯0.1、增塑剂2、三氧化二锑1-硼酸锌0.8、抗氧化剂1、热稳定剂0.9、辛基异噻唑啉酮1、丙酸钙2、异氰尿酸三缩水甘油酯0.9、二丙酮醇4、油酸二乙醇酰胺0.8、肉豆蔻酸钠皂0.7、羟基乙酸1。
所述的抗氧化剂为蓖麻油酸锌。
所述的热稳定剂为三盐基碳酸铅。
一种结构均匀、高透气性过滤用微孔膜的制备方法,包括以下步骤:
(1)取辛基异噻唑啉酮,加入到其重量17倍的去离子水中,搅拌均匀,加入丙酸钙,升高温度为48℃,保温搅拌7分钟,加入二丙酮醇,继续保温搅拌17分钟,得抑菌乳液;
(2)取肉豆蔻酸钠皂,加入到其重量7倍的无水乙醇中,搅拌均匀,加入羟基乙酸,在 70℃下保温搅拌26分钟,加入异氰尿酸三缩水甘油酯,搅拌至常温,得皂化酯溶液;
(3)取三氧化二锑、硼酸锌混合,加入到混合料重量26倍的去离子水中,搅拌均匀,加入油酸二乙醇酰胺,在48℃下保温搅拌16分钟,得阻燃酰胺分散液;
(4)取丙烯腈,加入到上述抑菌乳液中,搅拌均匀,送入到反应釜中,调节反应釜温度为76℃,通入氮气,加入过氧化二异丙苯,保温搅拌1小时,出料,与上述皂化酯溶液混合,搅拌均匀,蒸馏除去乙醇,送入到烘箱中,在86℃下干燥48分钟,出料冷却,得高粘度聚丙烯腈;
(5)取热稳定剂,加入到上述阻燃酰胺分散液中,搅拌均匀,加入上述高粘度聚丙烯腈,在70℃下保温搅拌40分钟,得阻燃聚丙烯腈酰胺分散液;
(6)取上述阻燃聚丙烯腈酰胺分散液,与聚乙烯、增塑剂、抗氧化剂混合,搅拌均匀,脱水,送入到挤出机中,在温度为240℃的条件下熔融塑化均匀成熔体;
(7)将所得熔体从模头挤出的铸片,随后进入流延工序,模头温度为240℃,流延温度为90℃,制备出厚度在8-40μm的中间体膜Ⅰ;
(8)将中间体膜Ⅰ进行微张力下退火处理,退火温度为100℃,膜在退火设备中的速度为10m/min,纵向张力0.6N,纵向的拉伸比为1.0,退火时间30min,得到中间体膜Ⅱ;
(9)将中间体膜Ⅱ进行纵向延伸开孔,温度为130℃,速比为1.5,得到中间体膜Ⅲ。
(10)将中间体膜Ⅲ进行回缩定型,回缩比为1.0,定型温度为130℃,得到中间体膜Ⅳ;
(11)将中间体膜Ⅳ进行纵向二次延伸开孔,温度为140℃,速比为0.5,得到所述结构均匀、高透气性过滤用微孔膜。
上述所有测试结果列于表1中:
表1
项目 | 实施例1 | 实施例2 | 实施例3 |
拉伸强度(MD,MPa) | 180 | 192 | 186 |
拉伸强度(TD,MPa) | 80 | 75 | 90 |
透气度(sec/100ml) | 75 | 55 | 64 |
穿刺强度(g) | 600 | 560 | 650 |
PM2.5过滤效率(%) | 96 | 97 | 96 |
由表1可知,采用本发明方法制备的高透气性过滤用微孔膜的机械强度高,微孔分布均匀,使用过程中不易损伤,具有优良抗形变能力及耐热性较强。对其PM2.5过滤效率高达90%以上。
以上所述仅为本发明的优选实施例而已,并不用于限制本发明,对于本领域的技术人员来说,本发明可以有各种更改和变化。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (3)
1.一种结构均匀、高透气性过滤用微孔膜,其特征在于,它是由下述重量份的原料组成的:聚乙烯100-110、丙烯腈27-30、过氧化二异丙苯0.1-0.2、增塑剂2-4、三氧化二锑1-2、硼酸锌0.8-1、抗氧化剂1-2、热稳定剂0.8-2、辛基异噻唑啉酮1-2、丙酸钙1-3、异氰尿酸三缩水甘油酯0.7-2、二丙酮醇4-6、油酸二乙醇酰胺0.7-1、肉豆蔻酸钠皂0.5-1、羟基乙酸1-2;
所述的结构均匀、高透气性过滤用微孔膜的制备方法为:
(1)取辛基异噻唑啉酮,加入到其重量17-20倍的去离子水中,搅拌均匀,加入丙酸钙,升高温度为40-50℃,保温搅拌4-9分钟,加入二丙酮醇,继续保温搅拌10-20分钟,得抑菌乳液;
(2)取肉豆蔻酸钠皂,加入到其重量6-9倍的无水乙醇中,搅拌均匀,加入羟基乙酸,在70-90℃下保温搅拌20-30分钟,加入异氰尿酸三缩水甘油酯,搅拌至常温,得皂化酯溶液;
(3)取三氧化二锑、硼酸锌混合,加入到混合料重量26-30倍的去离子水中,搅拌均匀,加入油酸二乙醇酰胺,在40-50℃下保温搅拌10-20分钟,得阻燃酰胺分散液;
(4)取丙烯腈,加入到上述抑菌乳液中,搅拌均匀,送入到反应釜中,调节反应釜温度为76-80℃,通入氮气,加入过氧化二异丙苯,保温搅拌1-2小时,出料,与上述皂化酯溶液混合,搅拌均匀,蒸馏除去乙醇,送入到烘箱中,在86-90℃下干燥40-50分钟,出料冷却,得高粘度聚丙烯腈;
(5)取热稳定剂,加入到上述阻燃酰胺分散液中,搅拌均匀,加入上述高粘度聚丙烯腈,在60-70℃下保温搅拌30-40分钟,得阻燃聚丙烯腈酰胺分散液;
(6)取上述阻燃聚丙烯腈酰胺分散液,与聚乙烯、增塑剂、抗氧化剂混合,搅拌均匀,脱水,送入到挤出机中,在温度为200-240℃的条件下熔融塑化均匀成熔体;
(7)将所得熔体从模头挤出的铸片,随后进入流延工序,模头温度为185-240℃,流延温度为50-110℃,制备出厚度在8-40μm的中间体膜Ⅰ;
(8)将中间体膜Ⅰ进行微张力下退火处理,退火温度为90-160℃,膜在退火设备中的速度为1-20m/min,纵向张力0.1-3.0N,纵向的拉伸比为1.0-2.0,退火时间5-60min,得到中间体膜Ⅱ;
(9)将中间体膜Ⅱ进行纵向延伸开孔,温度为100-150℃,速比为0.5-3.0,得到中间体膜Ⅲ;
(10)将中间体膜Ⅲ进行回缩定型,回缩比为1.0-1.5,定型温度为100-160℃,得到中间体膜Ⅳ;
(11)将中间体膜Ⅳ进行纵向二次延伸开孔,温度为100-140℃,速比为0.5-2.0,得到所述结构均匀、高透气性过滤用微孔膜。
2.根据权利要求1所述的一种结构均匀、高透气性过滤用微孔膜,其特征在于,所述的抗氧化剂为酚类、胺类、含磷化合物、含硫化合物、有机金属盐中的一种或多种。
3.根据权利要求1所述的一种结构均匀、高透气性过滤用微孔膜,其特征在于,所述的热稳定剂为三盐基碳酸铅、二盐基亚磷酸铅,硬脂酸、月桂酸的镉、钡、钙、锌、镁盐、二巯基醋酸异辛酯中的一种或多种。
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