CN117534946B - 一种纳米微胶囊隔热功能母粒及其制备方法 - Google Patents
一种纳米微胶囊隔热功能母粒及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种纳米微胶囊隔热功能母粒及其制备方法,其通过有机无机复合的纳米微胶囊与聚合物基体材料混合,添加助剂造粒而成;纳米微胶囊的添加百分比为1‑20wt%,助剂的添加百分比为0.2‑0.5wt%,余量为聚合物基材;纳米微胶囊通过乳化预聚、聚合、纳米复合的方式制备。相较于一般隔热功能母粒,该母粒具备突出的稳定性、更高的隔热性以及保温性能。
Description
技术领域
本发明涉及纳米材料技术领域,具体为一种纳米微胶囊隔热功能母粒及其制备方法。
背景技术
隔热功能母粒可用于制备隔热功能薄膜、板材等塑料材料,在建筑、汽车等多个领域发挥重要功能。一般的隔热功能母粒只具备单纯的隔热功能,在隔热性能、储能保温性方面仍有较大的提升空间。中国专利CN114752142B公开了一种铯化钨体系的透明隔热母粒,其通过将纳米钨铯氧化物改性形成含有酯键的高分子链段,并通过酯交换反应得到HALS-g-EVA/PVB-g-Cs0.33WO3复合材料,实现隔热防蓝光功能。其在一般无机隔热母粒的基础上通过改性复合,提高了耐老化性和防蓝光性,在隔热性方面未有提高。中国专利CN108530843B公开了一种用于BOPET窗膜的隔热母粒,其中的隔热材料为纳米碳化纤维素、二氧化钛、聚丙烯酰胺组成的核-内壳-外壳结构组合物,通过内核的吸热性、内壳的反射性等作用以实现隔热功能。其应用性主要在于BOPET窗膜,未在隔热性及其他功能性方面做进一步提高。为了提高一般隔热母粒如钨铯氧化物的功能性,若将隔热和储能材料以微胶囊的形式施加稳定有效的结合,既通过吸热提高了隔热能力上限,又实现了储能保温性能,在日益需求节能减排的当前,对于推动社会经济发展有着重要作用。
发明内容
针对现有技术的上述不足,根据本发明的实施例,希望提供一种具有高效长久隔热、储能保温的功能母粒,以实现其功能性的提升和应用的拓展。
根据实施例,本发明提供的一种纳米微胶囊隔热功能母粒,该母粒由塑料基材和纳米微胶囊混合,添加助剂造粒制成,纳米微胶囊的添加量为母粒的1-20wt%,助剂添加量为母粒的0.2-0.5wt%,其中:塑料基材选自聚乙烯、聚丙烯、聚氯乙烯、聚甲基丙烯酸甲酯、聚对苯二甲酸乙二酯、聚苯乙烯、聚碳酸酯;纳米微胶囊为纳米钨掺杂氧化物与醇酸复合晶体有机复合形成的纳米隔热材料;助剂为乙二醇聚氧乙烯醚、γ-氨丙基三乙氧基硅烷、四-(二丁基羟基氢化肉桂酸)季戊四醇酯的复合物。
根据一个实施例,纳米微胶囊的制备方法如下:
(1)根据质量比,将0.5-1份十二烷基硫酸钠溶于50-80份去离子水中,为溶液A;将5-8份甲基丙烯酸甲酯、1-2份丙烯酸乙酯、8-15份醇酸复合晶体和0.1-0.2份偶氮二异丁腈超声混合5-10min,为溶液B;将溶液B滴加到溶液A中,20-40℃搅拌5-30min,为乳液C;将乳液C于75-85℃下搅拌反应0.5-1.5h;
(2)将1-2份十二烷基硫酸钠和1-5份甲基丙烯酸羟乙酯溶于120-150份去离子水中,为溶液D;将7-10份甲基丙烯酸甲酯、2-3份季戊四醇四丙烯酸酯和0.1-0.3份偶氮二异丁腈超声混合分散5-15min,为溶液E;将溶液E滴加到溶液D中,20-40℃搅拌5-30min,为乳液F;将乳液F加入乳液C中,75-85℃继续反应5-10h。
(3)5-10份纳米钨掺杂氧化物与0.1-0.5份聚乙烯吡咯烷酮分散于50-100份去离子水中,加盐酸至pH为5.5-6.5,超声0.5-1h,清洗过滤并烘干;将所得材料与1-2份十二烷基硫酸钠混合于30-50份去离子水中,超声10-30min,为分散液G;将分散液G滴加入聚合液中,搅拌至形成均匀液相;
(4)向聚合液中加入2-5份硅烷乳液,40-50℃搅拌1-2h;反应液进行抽滤,反复清洗,真空干燥24-48h,制得纳米微胶囊。
根据一个实施例,制备方法步骤(1)中,醇酸复合晶体选自月桂酸/十四醇复合晶体和十四酸/十七醇复合晶体的其中一种,醇酸摩尔比为1:1,以共熔融重结晶获得。
根据一个实施例,纳米微胶囊的制备方法步骤(1)和步骤(2)中,滴加速度为1-3ml/min。
根据一个实施例,纳米微胶囊的制备方法步骤(3)中,滴加速度为3-5ml/min。
根据一个实施例,纳米微胶囊的制备方法步骤(3)中,硅烷乳液由Tween-40、KH-460、去离子水以3:50:80的质量比混合至均匀而成。
技术效果本发明隔热材料与储能材料以纳米微胶囊的形式高效稳定复合,以实现更高的隔热性和保温性,并且实现了材料的稳定性。具体来说,通过醇酸复合晶体与丙烯酸类单体的乳液聚合,实现微胶囊的制备。醇酸复合晶体在聚合过程中逐渐被以甲基丙烯酸甲酯为主体的壳层包覆。其中,引入季戊四醇丙烯酸酯为微胶囊壳体的交联剂,以实现壳体的可靠性和稳定性;引入丙烯酸乙酯,以调整壳体的柔韧性。在此之外,额外引入单体甲基丙烯酸羟乙酯,作为进一步复合的活性点。同时,将纳米钨掺杂氧化物表面活化,与具有活性位点的纳米微胶囊壳层经由偶联剂实现复合。其主要特点表现为更好的隔热性和保温性,同时具备突出的稳定性。
相比现有技术,随后的实施例和试验例将证明,本发明纳米微胶囊隔热母粒具有以下优点:隔热性能出众,稳定性好,制备薄膜时具有较好的透明性和清晰度,在节能隔热材料领域具有很好的应用价值。
具体实施方式
下面结合具体实施例,进一步阐述本发明。这些实施例应理解为仅用于说明本发明而不用于限制本发明的保护范围。在阅读了本发明记载的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等效变化和修改同样落入本发明权利要求所限定的范围。
本发明纳米钨掺杂氧化物为上海沪正实业有限公司生产的GTO产品,代号为G-P100,以下实施例中所使用的其他原料如无特别标示均为市售产品。
实施例1纳米微胶囊通过以下过程制备:
(1)将6g十二烷基硫酸钠溶于750g去离子水中,为溶液A;将50g甲基丙烯酸甲酯、10g丙烯酸乙酯、100g月桂酸/十四醇复合晶体(醇酸摩尔比为1:1)和1g偶氮二异丁腈超声混合10min,为溶液B。将溶液B以2ml/min的速率滴加到溶液A中, 40℃搅拌20min,为乳液C,将乳液C于75℃下搅拌反应1h;
(2)将10g十二烷基硫酸钠和30g甲基丙烯酸羟乙酯溶于1200g去离子水中,为溶液D;将70g甲基丙烯酸甲酯、20g季戊四醇四丙烯酸酯和1g偶氮二异丁腈超声混合分散10min,为溶液E;将溶液E以2ml/min的速率滴加到溶液D中,40℃搅拌30min,为乳液F;将乳液F加入乳液C中,75℃继续反应7h;
(3)80g纳米钨掺杂氧化物G-P100与2g聚乙烯吡咯烷酮分散于800g去离子水中,加盐酸至pH为6.0,超声0.5h,清洗过滤并烘干;将所得材料与10g十二烷基硫酸钠混合于300g去离子水中,超声10min,为分散液G;将分散液G以3ml/min的速率滴加入聚合液中,搅拌至形成均匀液相;
(4)将Tween-40、KH-460、去离子水以3:50:80的质量比混合至均匀,形成硅烷乳液,向聚合液中加入30g硅烷乳液,40℃搅拌2h;反应液进行抽滤,反复清洗3次,真空干燥48h,制得纳米微胶囊。
将100g纳米微胶囊,897g聚对苯二甲醇乙二酯塑料切片,0.8g乙二醇聚氧乙烯醚,1.2g四-(二丁基羟基氢化肉桂酸)季戊四醇酯,1g γ-氨丙基三乙氧基硅烷,在充分搅拌的情况下,加入到塑料造粒机中,制得纳米微胶囊隔热功能母粒。
实施例2纳米微胶囊通过以下过程制备:
(1)将5g十二烷基硫酸钠溶于800g去离子水中,为溶液A;将60g甲基丙烯酸甲酯、15g丙烯酸乙酯、12g十四酸/十七醇复合晶体(醇酸摩尔比为1:1)和1g偶氮二异丁腈超声混合10min,为溶液B;将溶液B以3ml/min的速率滴加到溶液A中,40℃搅拌30min,为乳液C;将乳液C于75℃下搅拌反应1h;
(2)将10g十二烷基硫酸钠和35g甲基丙烯酸羟乙酯溶于1500g去离子水中,为溶液D;将80g甲基丙烯酸甲酯、30g季戊四醇四丙烯酸酯和1.5g偶氮二异丁腈超声混合分散15min,为溶液E;将溶液E以3ml/min的速率滴加到溶液D中,40℃搅拌30min,为乳液F;将乳液F加入乳液C中,80℃继续反应9h;
(3)90g纳米钨掺杂氧化物G-P100与3g聚乙烯吡咯烷酮分散于1000g去离子水中,加盐酸至pH为5.5,超声1h,清洗过滤并烘干;将所得材料与15g十二烷基硫酸钠混合于400g去离子水中,超声30min,为分散液G;将分散液G以4ml/min的速率滴加入聚合液中,搅拌至形成均匀液相;
(4)将Tween-40、KH-460、去离子水以3:50:80的质量比混合至均匀,形成硅烷乳液,向聚合液中加入35g硅烷乳液,45℃搅拌2h;反应液进行抽滤,反复清洗3次,真空干燥48h,制得纳米微胶囊。
将100g纳米微胶囊,897g聚丙烯塑料切片,0.7g乙二醇聚氧乙烯醚, 1.5g四-(二丁基羟基氢化肉桂酸)季戊四醇酯,1g γ-氨丙基三乙氧基硅烷。在充分搅拌的情况下,加入到塑料造粒机中,制得纳米微胶囊隔热功能母粒。
实施例3纳米微胶囊通过以下过程制备:
(1)将6g十二烷基硫酸钠溶于800g去离子水中,为溶液A;将65g甲基丙烯酸甲酯、15g丙烯酸乙酯、14g十四酸/十七醇复合晶体(醇酸摩尔比为1:1)和1g偶氮二异丁腈超声混合10min,为溶液B;将溶液B以3ml/min的速率滴加到溶液A中,40℃搅拌30min,为乳液C;将乳液C于75℃下搅拌反应1h;
(2)将10g十二烷基硫酸钠和40g甲基丙烯酸羟乙酯溶于1500g去离子水中,为溶液D;将80g甲基丙烯酸甲酯、30g季戊四醇四丙烯酸酯和1.5g偶氮二异丁腈超声混合分散15min,为溶液E;将溶液E以3ml/min的速率滴加到溶液D中,40℃搅拌30min,为乳液F;将乳液F加入乳液C中,80℃继续反应8h;
(3)80g纳米钨掺杂氧化物G-P100与2g聚乙烯吡咯烷酮分散于1000g去离子水中,加盐酸至pH为6.0,超声1h,清洗过滤并烘干;将所得材料与12g十二烷基硫酸钠混合于400g去离子水中,超声30min,为分散液G;将分散液G以4ml/min的速率滴加入聚合液中,搅拌至形成均匀液相;
(4)将Tween-40、KH-460、去离子水以3:50:80的质量比混合至均匀,形成硅烷乳液,向聚合液中加入35g硅烷乳液,45℃搅拌2h;反应液进行抽滤,反复清洗3次,真空干燥48h,制得纳米微胶囊。
将100g纳米微胶囊,897g聚甲基丙烯酸甲酯塑料切片,0.7g乙二醇聚氧乙烯醚,1.5g四-(二丁基羟基氢化肉桂酸)季戊四醇酯,1g γ-氨丙基三乙氧基硅烷。在充分搅拌的情况下,加入到塑料造粒机中,制得纳米微胶囊隔热功能母粒。
对比例纳米隔热材料通过以下方法制备:
(1)将6g十二烷基硫酸钠溶于800g去离子水中,为溶液A;将65g甲基丙烯酸甲酯、15g丙烯酸乙酯、14g月桂酸/十四醇复合晶体(醇酸摩尔比为1:1)和1g偶氮二异丁腈超声混合10min,为溶液B;将溶液B以3ml/min的速率滴加到溶液A中,40℃搅拌30min,为乳液C;将乳液C于75℃下搅拌反应1h;
(2)将10g十二烷基硫酸钠和40g甲基丙烯酸羟乙酯溶于1500g去离子水中,为溶液D;将80g甲基丙烯酸甲酯、30g季戊四醇四丙烯酸酯和1.5g偶氮二异丁腈超声混合分散15min,为溶液E;将溶液E以3ml/min的速率滴加到溶液D中,40℃搅拌30min,为乳液F;将乳液F加入乳液C中,80℃继续反应8h;
(3)向其中加入80g纳米钨掺杂氧化物G-P100,混合至均相,反应液抽滤,反复清洗3次,真空干燥48h,得到纳米隔热材料。
将100g纳米隔热材料,897g聚甲基丙烯酸甲酯塑料切片,0.7g乙二醇聚氧乙烯醚,1.5g四-(二丁基羟基氢化肉桂酸)季戊四醇酯,1g γ-氨丙基三乙氧基硅烷,在充分搅拌的情况下,加入到塑料造粒机中,制得对比隔热功能母粒。
试验例以各实施例制备的纳米微胶囊隔热功能母粒,按5%的质量比与对应的基材母粒共混挤出,采用双向拉伸工艺,制取厚度50μm薄膜,测试其性能。薄膜的红外阻隔率、可见光透过率通过分光光度仪和光学透过率仪测试。红外阻隔率测试波段为950nm和1400nm。耐候性测试根据ASTM-D4329-13人工加速耐候性测试方法进行测试。清晰度(雾度)通过雾度检测仪测试。测试结果如表1所示。可以看到,制备的薄膜具备较好的可见光透过率,并表现出很好的隔热效果,阻隔率可达99.9%,隔热性能十分突出,较一般隔热薄膜效果有明显提升。同时,薄膜也表现出很好的耐老化性,通过了QUV5000h的试验,表明其突出的耐候性。在清晰度方面,雾度均小于0.5%,表现出了很好的清晰度。其中,对比例采用了类似的纳米隔热材料,纳米无掺杂氧化物没有进一步修饰改性并与纳米微胶囊形成有效复合,从而出现粒子相分离和易迁移的问题。其在相容性方面存在明显问题,尽管在可见光透过率和红外阻隔率方面没有造成明显影响,但在其耐候性方面,其均匀性和相容性明显不及各实施例,因而经QUV5000h后出现发雾现象。通过以上各项试验表明,由各实施例的纳米微胶囊隔热功能母粒制备的功能薄膜,具备很好的透明性、清晰度以及突出的稳定性和很好的隔热性,在隔热节能领域具备重要的应用价值。
表1 纳米微胶囊隔热母粒制备的薄膜性能测试
以上内容是结合具体的实施例对本发明所作的详细说明,不能认定本发明具体实施仅限于这些说明。对于本发明所属技术领域的技术人员来说,在不脱离本发明构思的前提下,还可以做出若干简单推演或替换,都应当视为属于本发明保护的范围。
Claims (4)
1.一种纳米微胶囊隔热功能母粒,其特征在于:该母粒由塑料基材和纳米微胶囊混合,添加助剂造粒制成,纳米微胶囊的添加量为母粒的1-20wt%,助剂添加量为母粒的0.2-0.5wt%;其中塑料基材选自聚乙烯、聚丙烯、聚氯乙烯、聚甲基丙烯酸甲酯、聚对苯二甲酸乙二酯、聚苯乙烯、聚碳酸酯;纳米微胶囊为纳米钨掺杂氧化物与醇酸复合晶体有机复合形成的纳米隔热材料;助剂为乙二醇聚氧乙烯醚、γ-氨丙基三乙氧基硅烷、四-(二丁基羟基氢化肉桂酸)季戊四醇酯的复合物;
纳米微胶囊的制备方法为:
(1)根据质量比,将0.5-1份十二烷基硫酸钠溶于50-80份去离子水中,为溶液A;将5-8份甲基丙烯酸甲酯、1-2份丙烯酸乙酯、8-15份醇酸复合晶体和0.1-0.2份偶氮二异丁腈超声混合5-10min,为溶液B;将溶液B滴加到溶液A中,20-40℃搅拌5-30min,为乳液C;将乳液C于75-85℃下搅拌反应0.5-1.5h;
醇酸复合晶体选自月桂酸/十四醇复合晶体和十四酸/十七醇复合晶体的其中一种,醇酸摩尔比为1:1,以共熔融重结晶获得;
(2)将1-2份十二烷基硫酸钠和1-5份甲基丙烯酸羟乙酯溶于120-150份去离子水中,为溶液D;将7-10份甲基丙烯酸甲酯、2-3份季戊四醇四丙烯酸酯和0.1-0.3份偶氮二异丁腈超声混合分散5-15min,为溶液E;将溶液E滴加到溶液D中,20-40℃搅拌5-30min,为乳液F;将乳液F加入乳液C中,75-85℃继续反应5-10h;
(3)5-10份纳米钨掺杂氧化物与0.1-0.5份聚乙烯吡咯烷酮分散于50-100份去离子水中,加盐酸至pH为5.5-6.5,超声0.5-1h,清洗过滤并烘干;将所得材料与1-2份十二烷基硫酸钠混合于30-50份去离子水中,超声10-30min,为分散液G;将分散液G滴加入聚合液中,搅拌至形成均匀液相;
(4)向聚合液中加入2-5份硅烷乳液,40-50℃搅拌1-2h,反应液进行抽滤,反复清洗,真空干燥24-48h,制得纳米微胶囊。
2.根据权利要求1所述纳米微胶囊隔热功能母粒的制备方法,其特征在于:步骤(1)和步骤(2)中,滴加速度为1-3ml/min。
3.根据权利要求1所述纳米微胶囊隔热功能母粒的制备方法,其特征在于:步骤(3)中,滴加速度为3-5ml/min。
4.根据权利要求1所述纳米微胶囊隔热功能母粒的制备方法,其特征在于:步骤(3)中,硅烷乳液由Tween-40、KH-460、去离子水以3:50:80的质量比混合至均匀而成。
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