CN112250974A - 一种透明聚偏氟乙烯耐候抗菌薄膜专用料及其制备方法 - Google Patents
一种透明聚偏氟乙烯耐候抗菌薄膜专用料及其制备方法 Download PDFInfo
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- 239000002033 PVDF binder Substances 0.000 title claims abstract description 63
- 229920002981 polyvinylidene fluoride Polymers 0.000 title claims abstract description 63
- 239000000463 material Substances 0.000 title claims abstract description 61
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000002667 nucleating agent Substances 0.000 claims abstract description 29
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- 150000001412 amines Chemical class 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
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- 239000000203 mixture Substances 0.000 claims description 5
- 239000004611 light stabiliser Substances 0.000 claims description 4
- 229910021645 metal ion Inorganic materials 0.000 claims description 4
- 229910044991 metal oxide Inorganic materials 0.000 claims description 4
- 150000004706 metal oxides Chemical class 0.000 claims description 4
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 4
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- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 3
- 239000012965 benzophenone Substances 0.000 claims description 3
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 3
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- HHKVOYUYPYZFHJ-SOFGYWHQSA-N (e)-3-(3,4-dihydroxyphenyl)-1-phenylprop-2-en-1-one Chemical compound C1=C(O)C(O)=CC=C1\C=C\C(=O)C1=CC=CC=C1 HHKVOYUYPYZFHJ-SOFGYWHQSA-N 0.000 description 1
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
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- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
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Abstract
本发明公开了一种透明聚偏氟乙烯耐候抗菌薄膜专用料及其制备方法,专用料中增强树脂同时起到增强和增韧作用,大大增加薄膜的抗撕裂性能;同时增强树脂的加入在成型过程中大大降低银烧的风险,增强树脂的加入具有降低材料比表面积的作用,减少聚偏氟乙烯与抗菌剂的接触,降低材料自由基产生的概率,从而减少聚偏氟乙烯降解情况的产生;抗菌剂的引入可以大幅度提高材料的抗菌性能,同时具有永久的抗菌效果;在熔融状态下成核剂和抗菌剂提供所需的晶核,聚偏氟乙烯从原来的均相成核转变为异相成核,可以提高聚偏氟乙烯的结晶度从而增加材料的透明度。使用本发明制备的薄膜有耐候性优异、抗菌性能卓越、透明度高、力学性能优异的特点。
Description
技术领域
本发明涉及聚偏氟乙烯薄膜技术领域,具体涉及一种透明聚偏氟乙烯耐候 抗菌薄膜专用料及其制备方法。
背景技术
聚偏氟乙烯(PVDF)是氟塑料家族中的重要一员,但由于其流动性差,熔融 加工困难,成膜更难。另一方面,聚偏氟乙烯具有突出的耐高低温、耐化学腐 蚀和耐候性,优异的电绝缘性,已经应用于工业、民用的许多领域。然而聚偏 氟乙烯薄膜受限于自身的抗菌性能以及透明度,在医疗行业、养老院、幼儿园 等领域仍然处于空白阶段。现在运用在这些行业的材料多为(聚氯乙烯)PVC材 料,聚偏氟乙烯材料相对于(聚氯乙烯)PVC材料来说,具有更加优越的耐候性 能,耐腐蚀性能,抗菌性能以及自清洁性能。
聚偏氟乙烯抗菌薄膜在制备过程中同时存在银烧的现象(聚偏氟乙烯与大 部分的抗菌材料在螺杆中加热共混一段时间后会出现反应产生难闻的气体甚至 出现焦黑现象),银烧现象产生原理:当PVDF体系内有自由基或者可以形成自 由基的物质存在时,高温下树脂分解加速,可以使得树脂分解变色同时释放HF, 然后“拉链式”地脱去HF形成具有共轭双键结构的有色物质,同时大部分抗菌 材料具有较强的活性,这样会进一步的加快聚偏氟乙烯的降解反应。因此聚偏 氟乙烯抗菌材料的技术难点在于在保证产品优异抗菌材料的同时具有良好的生 产加工稳定性和较高的透明度。
发明内容
本发明的目的是为了解决现有技术中的问题,提供一种透明聚偏氟乙烯耐 候抗菌薄膜专用料及其制备方法,此专用料可以用于制备耐候性优异、抗菌性 能卓越、透明度高、力学性能优异的聚偏氟乙烯薄膜。
为了达到上述目的,本发明的技术方案是:
一种透明聚偏氟乙烯耐候抗菌薄膜专用料,括以下质量份的组分,
优选的,所述聚偏氟乙烯的分子量为20~100万,且在230℃*2.16kg的条 件下,熔体流动速率为8~30g/10min。
优选的,所述增强树脂为丙烯酸酯类、甲基丙烯酸酯类树脂中的至少一种。
优选的,所述增强树脂中每种组分的分子量均在10~75万,且在230℃ *2.16kg的条件下,熔体流动速率均为0.5~10g/10min。
优选的,所述成核剂为山梨醇类成核剂、盐酸类成核剂、稀土金属类成核 剂、氧化物类成核剂中的至少一种。通过添加成核剂让材料进行再次结晶,提 高透明度。
优选的,所述抗氧剂为受阻酚类抗氧剂、受阻胺类抗氧剂、亚磷酸酯类抗 氧剂、硫酯类抗氧剂中的至少一种。抗氧剂可以阻止材料加工或使用过程中的 热氧老化,提高其使用寿命和性能。
优选的,所述紫外吸收剂为水杨酸酯类紫外吸收剂、苯酮类紫外吸收剂、 受阻胺类光稳定剂、苯并三唑类紫外吸收剂中的至少一种。紫外吸收剂对太阳 光中的紫外线进行吸收,对本材料的耐候性能起到主要作用。
优选的,所述抗菌剂为金属离子抗菌剂、光催化抗菌剂、金属氧化物抗菌 剂中的至少一种。抗菌剂能够提高材料的抗菌性能,同时还能和成核剂起协同 作用。成核剂和抗菌剂均优选采用粒径为纳米级的纳米级粉体。
一种透明聚偏氟乙烯耐候抗菌薄膜专用料的制备方法,将聚偏氟乙烯、增 强树脂、成核剂、抗氧剂、紫外吸收剂、抗菌剂按照组分比例称取,先用高速 混合机混合均匀,混合转速为300~1500rpm,混合时间为5~20min;然后将混 合物加入双螺杆挤出机进行塑化、分散与挤出切粒后得到透明聚偏氟乙烯耐候 抗菌薄膜专用料。
优选的,所述双螺杆挤出机的工作温度为150~220℃,转速为250~500rpm, 螺杆长度与直径比为36:1~52:1。
本发明的有益效果是:本发明的一种透明聚偏氟乙烯耐候抗菌薄膜专用料 及其制备方法,专用料中增强树脂同时起到增强和增韧作用,大大增加薄膜的 抗撕裂性能;同时增强树脂的加入在成型过程中大大降低银烧的风险,增强树 脂的加入具有降低材料比表面积的作用,减少聚偏氟乙烯与抗菌剂的接触面积, 降低材料自由基产生的概率,从而减少聚偏氟乙烯降解情况的产生;抗菌剂的 引入可以大幅度提高材料的抗菌性能对于金色葡萄球菌和大肠杆菌能达到 99.99%的抗菌效果,同时具有永久的抗菌效果;成核剂和抗菌剂的双重作用之 下有利于提高材料的透明度,成核剂和抗菌剂为纳米级的粉体,可以提高聚偏 氟乙烯的结晶度从而增加材料的透明度。使用本发明制备的薄膜有耐候性优异、抗菌性能卓越、透明度高、力学性能优异的特点。
具体实施方式
为了使本技术领域的人员更好地理解本发明方案,下面通过实施方式对本 发明创造作进一步的详细说明。
一种透明聚偏氟乙烯耐候抗菌薄膜专用料,括以下质量份的组分,
其中,所述聚偏氟乙烯的分子量为20~100万,且在230℃*2.16kg的条件 下,熔体流动速率为8~30g/10min。所述增强树脂为丙烯酸酯类、甲基丙烯酸 酯类树脂中的至少一种。所述增强树脂中每种组分的分子量均在10~75万,且 在230℃*2.16kg的条件下,熔体流动速率均为0.5~10g/10min。增强树脂的加 入具有降低材料比表面积的作用,减少聚偏氟乙烯与抗菌剂的接触,降低材料 自由基产生的概率,从而减少聚偏氟乙烯降解情况的产生。
所述成核剂为山梨醇类成核剂、盐酸类成核剂、稀土金属类成核剂、氧化 物类成核剂中的至少一种。通过添加成核剂让材料进行再次结晶,提高透明度。 所述抗氧剂为受阻酚类抗氧剂、受阻胺类抗氧剂、亚磷酸酯类抗氧剂、硫酯类 抗氧剂中的至少一种。抗氧剂可以阻止材料加工或使用过程中的热氧老化,提 高其使用寿命和性能。所述紫外吸收剂为水杨酸酯类紫外吸收剂、苯酮类紫外 吸收剂、受阻胺类光稳定剂、苯并三唑类紫外吸收剂中的至少一种。紫外吸收 剂对太阳光中的紫外线进行吸收,对本材料的耐候性能起到主要作用。所述抗 菌剂为金属离子抗菌剂、光催化抗菌剂、金属氧化物抗菌剂中的至少一种。抗菌剂能够提高材料的抗菌性能,同时还能和成核剂起协同作用,在熔融状态下, 由于抗菌剂提供更多所需的晶核,聚偏氟乙烯由原来的均相成核转变成异相成 核,从而加速了结晶速度,使晶粒结构细化,并有利于提高产品的刚性,缩短 成型周期,保持最终产品的尺寸稳定性,抑制光散射,改善透明性和表面光泽。 成核剂和抗菌剂均优选采用粒径为纳米级的纳米级粉体。
下面例举四种不同专用料配方的实施例(实施例1-4),参见表1。各实施 例中采用的原料如下:
聚偏氟乙烯(PVDF):牌号为1000HD(供应商为:法国阿科玛;熔融指数 为14g/10min,230℃*2.16kg,分子量36万)。
增强树脂:甲基丙烯酸树脂与丙烯酸树脂的组合。
其中,甲基丙烯酸树脂:商品名为BS 203(供应商为:法国阿科玛,分子 量17万)。丙烯酸树脂为丙烯酸树脂1和丙烯酸树脂2的复配物,其中,丙烯 酸树脂1,商品名为Acrylic K-355P(供应商为:美国罗门哈斯公司,分子量 15万);丙烯酸树脂2,商品名为Acrylic K-125P(供应商为:美国罗门哈斯 公司,分子量75万)。
成核剂:氧化物成核剂,牌号RQT-CH(供应商为:瑞奇特)。
抗氧剂:亚磷酸酯类抗氧剂,商品名为抗氧剂-1010(供应商为:德国BASF 公司)。
紫外吸收剂:受阻胺类光稳定剂,商品名为UV-770,(供应商为:德国BASF 公司)。
抗氧剂:金属离子抗菌剂/金属氧化物抗菌剂,商品名为:
HSL-PA-3702/HSL-PA-403(供应商为:中星纳米材料有限公司)。
表1实施例1-4专用料配方(质量份数)
实施例1 | 实施例2 | 实施例3 | 实施例4 | |
聚偏氟乙烯 | 65 | 75 | 70 | 60 |
甲基丙烯酸树脂 | 12 | 10 | 6 | 20 |
丙烯酸树脂 | 18 | 12 | 18 | 11 |
成核剂 | 0.5 | 1 | 1 | 0.5 |
抗氧剂 | 1 | 0.5 | 1.5 | 1.5 |
紫外吸收剂 | 1.5 | 0.5 | 3 | 2 |
抗菌剂 | 2 | 1 | 0.5 | 5 |
按照表1中的配方制备透明聚偏氟乙烯耐候抗菌薄膜专用料,制备方法如 下:将聚偏氟乙烯、增强树脂、成核剂、抗氧剂、紫外吸收剂、抗菌剂按照组 分比例称取,先用高速混合机混合均匀,混合转速为300~1500rpm,混合时间 为5~20min;然后将混合物加入双螺杆挤出机进行塑化、分散与挤出切粒后得 到透明聚偏氟乙烯耐候抗菌薄膜专用料。所述双螺杆挤出机的工作温度为150~ 220℃,转速为250~500rpm,螺杆长度与直径比为36:1~52:1。
实施例1-4高速混合机和双螺杆的温度和转速条件见表2。
表2
利用实施例1-4制备的透明聚偏氟乙烯耐候抗菌薄膜专用料粒子,均制备 成了透明聚偏氟乙烯耐候抗菌薄膜。同时,在制备聚偏氟乙烯薄膜过程中,实 施例1-4中的透明聚偏氟乙烯耐候抗菌薄膜专用料均在加工制膜过程中易于流 动、无焦烧现象,且制备的薄膜均匀、无明显条纹、薄膜厚度偏差≤5%,无明 显晶点。
下面按照JIS Z2801:2012标准,对实施例1-4的专用料所制成的透明聚偏 氟乙烯耐候抗菌薄膜以及对比样的抗菌性能进行测试;按照GB/T 1865标准,对 实施例1-4的专用料所制成的透明聚偏氟乙烯耐候抗菌薄膜以及对比样的人工 气候老化黄变指数进行测试;按照GB/T 2410标准,对实施例1-4的专用料所制 成的透明聚偏氟乙烯耐候抗菌薄膜以及对比样的自然光透过率进行测试。对比 样为市面上常用的PVC户外抗膜。测试结果参见表3。
表3
上述测试结果表明:与现PVC户外膜相比,用本发明材料制备的聚偏氟乙 烯薄膜抗菌性能能达到99.9%,透明度在85~88。通过人工气候老化黄变指数 的比较可以发现实施的案例均有更好的耐候性能(黄变指数越低说明耐候性能 越好);通过大肠杆菌抗菌率与金黄色葡萄球菌抗菌率的测试数据可以发现实 施案例均具有超强的抗菌性能(抗菌率越高说明抗菌性能越好);通过自然光 透过率的检测数据可以发现实施案例均具有优异的透明性(数值越高表示透明 性越好最高100)。综上所述,本发明的聚偏氟乙烯抗菌薄膜具有耐候性优异、 抗菌性能卓越、透明度高、力学性能优异的特点。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局 限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本 发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护 范围之内。
Claims (10)
2.根据权利要求1所述的透明聚偏氟乙烯耐候抗菌薄膜专用料,其特征在于:所述聚偏氟乙烯的分子量为20~100万,且在230℃*2.16kg的条件下,熔体流动速率为8~30g/10min。
3.根据权利要求1所述的透明聚偏氟乙烯耐候抗菌薄膜专用料,其特征在于:所述增强树脂为丙烯酸酯类、甲基丙烯酸酯类树脂中的至少一种。
4.根据权利要求3所述的透明聚偏氟乙烯耐候抗菌薄膜专用料,其特征在于:所述增强树脂中每种组分的分子量均在10~75万,且在230℃*2.16kg的条件下,熔体流动速率均为0.5~10g/10min。
5.根据权利要求1所述的透明聚偏氟乙烯耐候抗菌薄膜专用料,其特征在于:所述成核剂为山梨醇类成核剂、盐酸类成核剂、稀土金属类成核剂、氧化物类成核剂中的至少一种。
6.根据权利要求1所述的透明聚偏氟乙烯耐候抗菌薄膜专用料,其特征在于:所述抗氧剂为受阻酚类抗氧剂、受阻胺类抗氧剂、亚磷酸酯类抗氧剂、硫酯类抗氧剂中的至少一种。
7.根据权利要求1所述的透明聚偏氟乙烯耐候抗菌薄膜专用料,其特征在于:所述紫外吸收剂为水杨酸酯类紫外吸收剂、苯酮类紫外吸收剂、受阻胺类光稳定剂、苯并三唑类紫外吸收剂中的至少一种。
8.根据权利要求1所述的透明聚偏氟乙烯耐候抗菌薄膜专用料,其特征在于:所述抗菌剂为金属离子抗菌剂、光催化抗菌剂、金属氧化物抗菌剂中的至少一种。
9.根据权利要求1-8中任一项所述的透明聚偏氟乙烯耐候抗菌薄膜专用料的制备方法,其特征在于:将聚偏氟乙烯、增强树脂、成核剂、抗氧剂、紫外吸收剂、抗菌剂按照组分比例称取,先用高速混合机混合均匀,混合转速为300~1500rpm,混合时间为5~20min;然后将混合物加入双螺杆挤出机进行塑化、分散与挤出切粒后得到透明聚偏氟乙烯耐候抗菌薄膜专用料。
10.根据权利要求9所述的透明聚偏氟乙烯耐候抗菌薄膜的制备方法,其特征在于:所述双螺杆挤出机的工作温度为150~220℃,转速为250~500rpm,螺杆长度与直径比为36:1~52:1。
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