CN104744823A - 一种多孔聚合物载体材料及其制备方法 - Google Patents
一种多孔聚合物载体材料及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种多孔聚合物载体材料及其制备方法,是由以下组分按重量份制备而成:聚合物树脂60~99份、改性剂0~18份、成核剂0.5~4份、其它助剂0~5份、成孔剂为聚合物树脂重量的1-20%。本发明制备的多孔聚合物载体材料的表观密度在20~450g/L之间、开孔率在80%以上,具有泡孔尺寸和密度可精确控制、开孔率高、工艺稳定等特点;可用于吸附或过滤液体的助剂使用,并可利用本发明制备的多孔聚合物材料来制备高浓度液体助剂母料、高吸油材料、生物基水处理载体材料、过滤材料等产品,且具有吸收速度快、吸附率高、价廉易得等优点。
Description
技术领域
本发明属于高分子材料领域,具体涉及的一种多孔聚合物载体材料及其制备方法。
背景技术
在材料科学研究中人们注意到许多天然材料因其多孔的结构而具备高孔隙率、低密度、大比表面积等优良的性能。因此,人们发展出了各种人造多孔材料,其可分为金属和非金属两大类,也可细分为多孔陶瓷材料、聚合物多孔材料和多孔金属材料种不同的类型。
其中聚合物多孔材料具有高孔隙率、低密度、大比表面积和很好的物质输送能力等优点,在吸附与分离、催化、传感器、分子识别、生物组织工程以及环境科学等方面有着很高的应用价值,因此引起人们极大的兴趣。
现有聚合物材料多采用化学方法加工制备,存在加工效率低、泡孔密度低、泡孔大小不可控、吸附效率差等缺点,不能满足工业化生产需求。另外,采用化学方式加工容易引起溶剂残留和环境污染,不是理想的加工方式。而采用超临界流体作为成孔剂,不仅效率高,而且加工过程环保、无污染、无残留,是理想的加工方式。
发明内容
本发明的目的在于提供一种性能优越、加工稳定、泡孔大小和密度精确可控、开孔率高的多孔聚合物载体材料及其制造方法,从而克服了成孔过程中,孔径和密度稳定性差、材料泡孔均匀差、吸附率低的缺点。
一种多孔聚合物载体材料,由以下组分按重量份制备而成:
聚合物树脂:60~99份
改性剂:0~18份
成核剂:0.5~4份
其它助剂:0~5份
成孔剂:为聚合物树脂重量的1-20%;
所述多孔聚合物载体材料的表观密度为20~450g/L、开孔率≥80%。
进一步方案,所述聚合物树脂为熔体流动速率为0.5~10g/10min(230℃,2.16kg)的低密度聚乙烯、高密度聚乙烯、线性低密度聚乙烯、均聚聚丙烯、共聚聚丙烯、规共聚聚丙烯、聚苯乙烯、乙烯-醋酸乙烯酯共聚物、乙烯和丙烯的共聚物中的至少一种。
特别优选聚合物树脂的熔体流动速率为1~4g/10min。
进一步方案,所述改性剂为乙丙橡胶、乙烯或丙烯的热塑性弹性体、氯化聚乙烯、SBS、POE弹性体中的至少一种。
进一步方案,所述成核剂为碳酸钙、滑石粉、高岭土、二氧化硅、硫酸钡、炭黑、碳酸氢钠和柠檬酸混合物中的至少一种。
进一步方案,所述成孔剂包括物理成孔剂和化学成孔剂,所述物理成孔剂包括二氧化碳、氮气、丁烷、丙烷、戊烷、庚烷、水、空气、氟氯烃、氢气、氨气或氦气;
所述化学成孔剂包括偶氮类、亚硝酸类、磺酰肼类化合物、碳酸盐类化合物中的一种或多种混合物。如N,N’-二亚硝基五次甲基四胺(DPT)、N,N’-二甲基- N,N’-二亚硝基对苯二甲酰胺(ADC)、偶氮二甲酰胺(AC)、偶氮二异丁腈、偶氮二甲酸二异丙酯、偶氮二甲酸二乙酯、二偶氮氨基苯、偶氮二甲酸钡、4,4’-二磺酰肼二苯醚(OBSH)、对苯磺酰肼、3,3’-二磺酰肼二苯砜、4,4’-二苯二磺酰肼、1,3-苯二磺酰肼、1,4-苯二磺酰肼、碳酸氢钠等。
进一步方案,所述其它助剂包括热稳定剂、抗氧剂、填充剂、偶联剂、润滑剂或表面活性剂中的一种或多种。
本发明的另一个发明目的是提供上述多孔聚合物载体材料的制备方法,包括以下步骤:
(1)按配比,将聚合物树脂、改性剂、成核剂和其它助剂加入挤出机中进行充分混合;
(2)在挤出机的压缩段注入成孔剂,混合均匀后经挤出机的模头挤出得多孔聚合物载体材料。
进一步方案,所述挤出机包括单螺杆挤出机、双螺杆挤出机、串联双阶单螺杆挤出机、双螺杆-单螺杆串联双阶挤出机;所述挤出机的模头为圆形孔模,其孔径为0.5~2mm,圆形孔模的数量有2-30个。
所述挤出机从加料口到模头之间均为密封设置,挤出机的机筒耐压强度≥35MPa。
本发明中成孔剂的添加量是根据所制备的多孔聚合物载体材料所要求的表观密度进行调整。
本发明中挤出机包括单螺杆挤出机、两台串联形式的单螺杆挤出机、同向双螺杆挤出机串联单螺杆挤出机中的一种,其模头为圆形孔模,孔径为0.5~2mm、数量有2-30个,其具体大小根据所制备的多孔聚合物载体材料所要求的颗粒大小进行调整。
本发明专利中聚丙烯树脂改性剂没有特别限定,包括:乙丙橡胶、乙烯或丙烯的热塑性弹性体、氯化聚乙烯、SBS、POE等弹性体,这些橡胶或热塑性弹性体组分可以单独或两种或更多的混合作为改性剂使用。有时候为了需要还可以加入结晶成核剂、热稳定剂、抗氧剂、填充剂、偶联剂、润滑剂、表面活性剂等常用塑料助剂。
为了调节泡孔结构、泡孔大小和其均匀性,需加入成核剂。成核剂包括碳酸钙、滑石粉、高岭土、二氧化硅、硫酸钡、炭黑、碳酸氢钠与柠檬酸的混合物中的一种或多种。但是,不限于以上所述成核剂,只要是不溶于聚合物材料而且可以形成成核点的无机小分子矿物均能作为多孔聚合物载体材料制备中的成核剂。为了得到性能更优的效果,优选滑石粉作为成核剂,优选重量配比为0.5%~4%。
本发明中使用的成孔剂包括物理成孔剂和化学成孔剂。物理成孔剂包括二氧化碳、氮气、丁烷、丙烷、戊烷、庚烷中的一种或它们的混合物,但不限于以上所述几种,还包括水、空气、氟氯烃、氢气、氨气、氦气等符合“快速释压法”的物理成孔条件的惰性气体作为物理成孔剂。化学成孔剂包括偶氮类、亚硝酸类、磺酰肼类化合物、碳酸盐类化合物的一种或多种混合物。为了提高生产效率,得到良好的成孔效率和经济因素,成孔剂优选物理成孔剂。为了更好的环境适合性、安全性和控制成孔剂,因此,特别优选二氧化碳、氮气等无机成孔剂或以它们为主要成分的成孔剂。优选重量配比为1%~20%。
本发明将聚合物树脂组合物、改性剂、成核剂和其它助剂加入挤出机中进行混合;再在挤出机的压缩段注入成孔剂,混合均匀后经挤出机的模头挤出得多孔聚合物载体材料。
本发明通过试验,确定了孔径大小、流道长短与温度和系统压力的关系,使系统在0.5~2mm圆形孔模的模板下,可以保持稳定的压力和理想的成孔温度,保证了加工过程中生产的稳定性。另外加入改性剂、成核剂和其它助剂,使材料种类的多样性及适应性得到较大的提升,同时提高产品的吸附性能,使其可满足绝大多数场合使用。
本发明制备的多孔聚合物载体材料的表观密度在20~450g/L之间、开孔率在80%以上,可用于吸附或过滤液体的助剂使用。并可利用本发明制备的多孔聚合物材料来制备高浓度液体助剂母料、高吸油材料、生物基水处理载体材料、过滤材料等产品。
本发明的成孔剂在挤出机压缩段注入,可以保证系统压力稳定,避免物理成孔剂从加料口泄露,造成系统不稳定。另外,压缩段物料已经熔融,可以保证物理成孔剂迅速与聚合物物料混溶。挤出机从加料口到模头之间均为密封设置,不能有气体泄露,且挤出机的机筒耐压强度≥35MPa,从而能制备出表观密度为20~450g/L、开孔率≥80%的多孔聚合物载体材料。
具体实施方式
下面实施例中聚合物树脂的熔体流动速率为0.5~10g/10min(230℃,2.16kg);
下面实施例中挤出机可选择单螺杆挤出机、两台串联形式的单螺杆挤出机或同向双螺杆挤出机串联单螺杆挤出机,其模头为圆形孔模,孔径为0.5~2mm、数量有2-30个,该挤出机从加料口到模头之间均为密封设置,不能有气体泄露,且挤出机的机筒耐压强度≥35MPa。
实施例1
将94份共聚聚丙烯、5%的低密度聚乙烯和1份滑石粉,经搅拌机混合均匀后,加入直径为65mm、长径比为50的单螺杆挤出机的加料口中进行充分混合,然后在挤出机压缩段注入5份超临界二氧化碳气体,熔融物料在挤出机中充分混合后经其直径为1mm的圆形孔模头挤出,然后牵引、冷却、切粒成型为多孔聚合物载体材料。
经检测制备的多孔聚合物载体材料的密度为150g/L、开孔率为85%、泡孔平均直径为120微米。
实施例2
将60份线性低密度聚乙烯、35份均聚聚丙烯、2份乙烯热塑性弹性体,2份碳酸钙和2份高岭土,经搅拌机混合均匀后,加入直径为65mm、长径比为35和直径为90mm、长径比为40的串联单螺杆挤出机的加料口中进行充分混合,然后在挤出机压缩段注入1份氮气。上述熔融物料在挤出机中充分混合后经直径为1mm的圆形孔模头挤出,然后牵引、冷却、切粒成型为多孔聚合物载体材料。
经检测制备的该多孔聚合物载体材料密度在80g/L,开孔率为89%,泡孔平均直径96微米。
实施例3
将85份聚苯乙烯,12份SBS,6份POE弹性体,1份二氧化硅和2份碳酸氢钠,经搅拌机混合均匀后,加入直径为65mm、长径比为35和直径为90mm、长径比为35的串联单螺杆挤出机的加料口中进行充分混合,然后在上阶挤出机压缩段注入17份氢气。上述熔融物料在挤出机中充分混合后经直径为1.2mm的圆形孔模头挤出,然后牵引、冷却、切粒成型为多孔聚合物载体材料。
经检测制备的该多孔聚合物载体材料密度在20g/L,开孔率为93%,泡孔平均直径81微米。
实施例4
将80份乙烯-醋酸乙烯酯共聚物,10份乙丙橡胶,1份碳酸氢钠和1份柠檬酸混合物,经搅拌机混合均匀后,加入直径为45mm、长径比为40的双螺杆和直径为90mm、长径比为35的单螺杆串联的挤出机的加料口中进行充分混合,然后再在挤出机压缩段注入8份偶氮二甲酰胺成孔剂。由乙烯-醋酸乙烯酯树脂、乙丙橡胶、成核剂、成孔剂构成的熔融物料在挤出机中充分混合后经直径为0.5mm的圆形孔模头挤出,然后牵引、冷却、切粒成型为多孔聚合物载体材料。
经检测制备的该多孔聚合物载体材料密度在90g/L,开孔率为87%,泡孔平均直径131微米。
实施例5
将60份高密度聚乙烯,4份丙烯热塑性弹性体,5份表面活性剂十二烷基苯磺酸钠和0.5份硫酸钡,经搅拌机混合均匀后,加入直径为65mm、长径比为50的单螺杆挤出机的加料口中进行充分混合,然后在挤出机压缩段注入成孔剂偶氮二异丁腈3份、偶氮二甲酸二异丙酯2份,熔融物料在挤出机中充分混合后经直径为2mm的圆形孔模头挤出,然后牵引、冷却、切粒成型为多孔聚合物载体材料。
经检测制备的该多孔聚合物载体材料密度在320g/L,开孔率为83%,泡孔平均直径125微米。
以上所述,仅是本发明的较佳实施例而已,并非对本发明的技术方案作任何形式上的限制。本行业的技术人员应该了解,本发明不受上述实施例的限制,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进均仍在本发明的技术方案的范围内且属于要求保护的本发明的范围。
Claims (9)
1.一种多孔聚合物载体材料,其特征在于:由以下组分按重量份制备而成:
聚合物树脂:60~99份
改性剂:0~18份
成核剂:0.5~4份
其它助剂:0~5份
成孔剂:为聚合物树脂重量的1-20%;
所述多孔聚合物载体材料的表观密度为20~450g/L、开孔率≥80%。
2.根据权利要求1所述的多孔聚合物载体材料,其特征在于:所述聚合物树脂为熔体流动速率在230℃/2.16kg 下为0.5~10g/10min的低密度聚乙烯、高密度聚乙烯、线性低密度聚乙烯、均聚聚丙烯、共聚聚丙烯、聚苯乙烯、乙烯-醋酸乙烯酯共聚物、乙烯和丙烯的共聚物中的至少一种。
3.根据权利要求1所述的多孔聚合物载体材料,其特征在于:所述改性剂为乙丙橡胶、乙烯或丙烯的热塑性弹性体、氯化聚乙烯、SBS、POE弹性体中的至少一种。
4.根据权利要求1所述的多孔聚合物载体材料,其特征在于:所述成核剂为碳酸钙、滑石粉、高岭土、二氧化硅、硫酸钡、炭黑、碳酸氢钠和柠檬酸混合物中的至少一种。
5.根据权利要求1所述的多孔聚合物载体材料,其特征在于:所述成孔剂包括物理成孔剂和化学成孔剂,所述物理成孔剂包括二氧化碳、氮气、丁烷、丙烷、戊烷、庚烷、水、空气、氟氯烃、氢气、氨气或氦气;
所述化学成孔剂包括偶氮类、亚硝酸类、磺酰肼类化合物、碳酸盐类化合物中的一种或多种混合物。
6.根据权利要求1所述的多孔聚合物载体材料,其特征在于:所述其它助剂包括热稳定剂、抗氧剂、填充剂、偶联剂、润滑剂或表面活性剂中的一种或多种。
7.一种如权利要求1-6所述的多孔聚合物载体材料的制备方法,其特征在于:包括以下步骤:
(1)按配比,将聚合物树脂、改性剂、成核剂和其它助剂加入挤出机中进行充分混合;
(2)在挤出机的压缩段注入成孔剂,混合均匀后经挤出机的模头挤出得多孔聚合物载体材料。
8.根据权利要求7所述的制备方法,其特征在于:所述挤出机包括单螺杆挤出机、双螺杆挤出机、串联双阶单螺杆挤出机、双螺杆-单螺杆串联双阶挤出机;所述挤出机的模头为圆形孔模,其孔径为0.5~2mm,圆形孔模的数量有2-30个。
9.根据权利要求7所述的制备方法,其特征在于:所述挤出机从加料口到模头之间均为密封设置,挤出机的机筒耐压强度≥35MPa。
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