CN117143384A - 一种耐高温型pvc装饰膜及其制备方法 - Google Patents
一种耐高温型pvc装饰膜及其制备方法 Download PDFInfo
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- 238000010438 heat treatment Methods 0.000 claims abstract description 12
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- 239000003822 epoxy resin Substances 0.000 claims abstract description 10
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- MECNWXGGNCJFQJ-UHFFFAOYSA-N 3-piperidin-1-ylpropane-1,2-diol Chemical compound OCC(O)CN1CCCCC1 MECNWXGGNCJFQJ-UHFFFAOYSA-N 0.000 claims abstract description 9
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- YLBPOJLDZXHVRR-UHFFFAOYSA-N n'-[3-[diethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CCO[Si](C)(OCC)CCCNCCN YLBPOJLDZXHVRR-UHFFFAOYSA-N 0.000 claims abstract description 9
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims abstract description 8
- CVQVSVBUMVSJES-UHFFFAOYSA-N dimethoxy-methyl-phenylsilane Chemical compound CO[Si](C)(OC)C1=CC=CC=C1 CVQVSVBUMVSJES-UHFFFAOYSA-N 0.000 claims abstract description 8
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- YAHBZWSDRFSFOO-UHFFFAOYSA-L dimethyltin(2+);2-(2-ethylhexoxy)-2-oxoethanethiolate Chemical compound CCCCC(CC)COC(=O)CS[Sn](C)(C)SCC(=O)OCC(CC)CCCC YAHBZWSDRFSFOO-UHFFFAOYSA-L 0.000 claims description 9
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- 238000009740 moulding (composite fabrication) Methods 0.000 abstract description 4
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Abstract
本发明涉及一种耐高温型PVC装饰膜，该装饰膜通过将PVC裸膜进行耐高温涂覆成型加工而成的；耐高温涂覆层使用包括小粒径硅溶胶、甲基苯基二甲氧基硅烷、3‑氯丙基甲基二甲氧基硅烷、3‑氨基丙基三甲氧基硅烷、E‑51环氧树脂、三羟甲基丙烷三缩水甘油醚、N‑(2‑氨乙基)‑3‑氨丙基甲基二乙氧基硅烷在内的原料制成高分子涂料，然后经过加热烘干固化成型得到。最终在PVC裸膜上形成的有机硅膜层不仅耐高温出色，而且附着力也较好，耐磨性能也得到了一定的提升。
Description
技术领域
本发明涉及一种高分子组合物技术领域，具体地，涉及一种耐高温型PVC装饰膜及其制备方法。
背景技术
随着日常生活水平的提高和装饰行业的兴起，表面装饰材料进入了快速发展期，其中PVC薄膜材料因其生产工艺简单、装饰效果好而占据较大的市场，广泛应用于室内及家具装饰、如橱柜、桌面、台面等各种面材表面。它可以起到保护面材的作用，如防止表面出现轻微磨损、划痕等已达到延长家具的使用寿命等。然而，随着应用领域的扩展，一些用于高温领域，如家具餐桌的桌面、实验室的台面材料等领域由于需要放置较热的物品如沸腾的热水、烘箱中取出热的物品等，不仅温度较高，而且物体自身有重量，热压下，往往会导致家具表面的PVC装饰膜产生明显的痕迹，不平或者颜色加深等，不仅影响美观，而且严重影响其对面材的保护功能，为了适应相关领域的应用要求，行业内对耐高温型PVC装饰膜的需求较为迫切。
发明内容
针对上述问题，本发明采用PVC裸膜进行特殊耐高温涂覆、成型加工而成的。耐高温涂覆层使用包括小粒径硅溶胶、甲基苯基二甲氧基硅烷、3-氯丙基甲基二甲氧基硅烷、3-氨基丙基三甲氧基硅烷、E-51环氧树脂、三羟甲基丙烷三缩水甘油醚、N-(2-氨乙基)-3-氨丙基甲基二乙氧基硅烷在内的原料制成高分子涂料，然后经过加热烘干固化成型得到。
一种耐高温型PVC装饰膜，所述耐高温涂覆层包括以质量份计的如下原料：
组分中还包括盐酸与催化剂。
优选的，催化剂为二月桂酸二正辛基锡，用量为3-氯丙基甲基二甲氧基硅烷质量的0.05-0.08％；盐酸质量分数为28-30％。
优选的，小粒径硅溶胶的粒径为10-15nm。例如型号SS3015，粒径10-15nm，SiO2含量30％，购自山东百特新材料有限公司。
如上所述一种耐高温型PVC装饰膜，所述PVC裸膜包括PVC树脂、DOP增塑剂与热稳定剂，其质量比对应为100:25:3；热稳定剂为有机锡液体热稳定剂硫醇甲基锡。
所述一种耐高温型PVC装饰膜的制备方法，包括以下步骤：
A、将配方量的小粒径硅溶胶、甲基苯基二甲氧基硅烷、3-氯丙基甲基二甲氧基硅烷及异丙醇加入反应釜中，启动搅拌，加入质量分数为28-30％的盐酸，调节溶液的pH至4-4.5，然后加热至70℃-75℃进行聚合反应；
B、取样检测，待体系聚合物的粘度达到700-900mPa·s(25℃)时，将配方量的催化剂、3-氨基丙基三甲氧基硅烷加入反应釜中，并继续在70-75℃保温进行扩链聚合反应；
C、取样检测，待体系聚合物的粘度达到1300-1500mPa·s(25℃)时，此时加入配方量的E-51环氧树脂、三羟甲基丙烷三缩水甘油醚的混合原料，在76-79℃进行接枝聚合反应；
D、取样检测，待聚合物的粘度达到1900-2100mPa·s(25℃)时，降温至室温，加入配方量的N-(2-氨乙基)-3-氨丙基甲基二乙氧基硅烷，室温充分搅拌均匀后，出料得到PVC裸膜专用耐高温型产品；
E、取已经制备好的PVC裸膜产品，将D步骤得到的产品采用采用精密涂布机在PVC裸膜的单面涂布耐高温涂层；涂布后进入烘房进行加热烘干固化处理，然后冷却收卷即可得到耐高温型PVC装饰膜。
优选的，步骤E中，所述PVC裸膜包括PVC树脂、DOP增塑剂与热稳定剂，其质量比对应为100:25:3；热稳定剂为有机锡液体热稳定剂硫醇甲基锡。
优选的，步骤E中，涂布湿膜厚度控制在35-40μm；烘干固化温度控制在90-95℃，烘干固化时间保持在3-3.5min。
例如，一种耐高温型PVC装饰膜的制备方法，包括以下步骤：
A、将配方量的小粒径硅溶胶、甲基苯基二甲氧基硅烷、3-氯丙基甲基二甲氧基硅烷及异丙醇加入反应釜中，启动搅拌，加入质量分数为28-30％的盐酸溶液，调节溶液的pH至4-4.5，然后加热至70℃-75℃进行聚合反应；
B、取样检测，待体系聚合物的粘度达到700-900mPa·s(25℃)时，将配方量的催化剂、3-氨基丙基三甲氧基硅烷加入反应釜中，并继续在70-75℃保温进行扩链聚合反应；
C、取样检测，待体系聚合物的粘度达到1300-1500mPa·s(25℃)时，此时加入配方量的E-51环氧树脂、三羟甲基丙烷三缩水甘油醚的混合原料，在76-79℃进行接枝聚合反应；
D、取样检测，待聚合物的粘度达到1900-2100mPa·s(25℃)时，降温至室温，加入配方量的N-(2-氨乙基)-3-氨丙基甲基二乙氧基硅烷，室温充分搅拌均匀后，出料得到PVC裸膜专用耐高温型产品；
E、取制备好的PVC裸膜产品(PVC树脂与DOP增塑剂及硫醇甲基锡热稳定剂的质量比为100:25:3)，将D步骤得到的产品采用采用精密涂布机在PVC裸膜的单面涂布耐高温涂层，涂布湿膜厚度控制在35-40μm；涂布后进入烘房进行加热烘干固化处理，烘干固化温度控制在90-95℃，烘干固化时间保持在3-3.5min，然后冷却收卷即可得到耐高温型PVC装饰膜。
有益效果：
本方案采用PVC裸膜进行特殊耐高温涂覆、成型加工而成的。耐高温涂覆层使用包括小粒径硅溶胶、甲基苯基二甲氧基硅烷、3-氯丙基甲基二甲氧基硅烷、3-氨基丙基三甲氧基硅烷、E-51环氧树脂、三羟甲基丙烷三缩水甘油醚、N-(2-氨乙基)-3-氨丙基甲基二乙氧基硅烷在内的原料制成高分子涂料，然后经过加热烘干固化成型得到。本发明制备的环氧树脂改性有机硅涂覆液是在有机硅涂覆液的基础上，借助E-51环氧树脂及三羟甲基丙烷三缩水甘油醚与有机硅涂覆液中活性氨基的反应交联作用来提升涂膜的附着力及涂膜的硬度，最终在成膜时再与双氨基的有机硅单体N-(2-氨乙基)-3-氨丙基甲基二乙氧基硅烷进行烘干固化得到成型涂膜。该涂膜在PVC裸膜上形成的有机硅-环氧膜层不仅耐高温出色，而且附着力和疏水性好，耐磨性能也得到了有效的提升。
具体实施方式
下面结合实施例对本发明进一步说明。需要说明的是，在不冲突的情况下，本申请中的实施例及实施例中的技术特征可以相互结合。需要指出的是，除非另有指明，本申请使用的所有技术和科学术语具有与本申请所属技术领域的普通技术人员通常理解的相同含义。本发明公开使用的“包括”或者“包含”等类似的词语意指出现该词前面的元件或者物件涵盖出现在该词后面列举的元件或者物件及其等同，而不排除其他元件或者物件。
本发明所述原料均为市售可得。如小粒径硅溶胶型号SS3015，粒径10-15nm，SiO2含量30％，购自山东百特新材料有限公司。
实施例1
一种耐高温型PVC装饰膜，所述耐高温涂覆层包括以质量份计的如下原料：
催化剂为二月桂酸二正辛基锡，用量为3-氯丙基甲基二甲氧基硅烷质量的0.08％；盐酸质量分数为30％。
所述PVC裸膜包括PVC树脂、DOP增塑剂与热稳定剂，其质量比对应为100:25:3；热稳定剂为有机锡液体热稳定剂硫醇甲基锡。
制备方法包括以下步骤：
A、将配方量的小粒径硅溶胶、甲基苯基二甲氧基硅烷、3-氯丙基甲基二甲氧基硅烷及异丙醇加入反应釜中，启动搅拌，加入盐酸溶液，调节溶液的pH至4.5，然后加热至75℃进行聚合反应；
B、取样检测，待体系聚合物的粘度达到900mPa·s(25℃)时，将配方量的催化剂、3-氨基丙基三甲氧基硅烷加入反应釜中，并继续在75℃保温进行扩链聚合反应；
C、取样检测，待体系聚合物的粘度达到1500mPa·s(25℃)时，此时加入配方量的E-51环氧树脂、三羟甲基丙烷三缩水甘油醚的混合原料，在79℃进行接枝聚合反应；
D、取样检测，待聚合物的粘度达到2100mPa·s(25℃)时，降温至室温，加入配方量的N-(2-氨乙基)-3-氨丙基甲基二乙氧基硅烷，室温充分搅拌均匀后，出料得到PVC裸膜专用耐高温型产品；
E、取制备好的PVC裸膜产品，将D步骤得到的产品采用采用精密涂布机在PVC裸膜的单面涂布耐高温涂层，涂布湿膜厚度控制在40μm；涂布后进入烘房进行加热烘干固化处理，烘干固化温度控制在95℃，烘干固化时间保持在3.5min，然后冷却收卷即可得到耐高温型PVC装饰膜。
实施例2
一种耐高温型PVC装饰膜，所述耐高温涂覆层包括以质量份计的如下原料：
催化剂为二月桂酸二正辛基锡，用量为3-氯丙基甲基二甲氧基硅烷质量的0.08％；盐酸质量分数为28％。
所述PVC裸膜包括PVC树脂、DOP增塑剂与热稳定剂，其质量比对应为100:25:3；热稳定剂为有机锡液体热稳定剂硫醇甲基锡。
制备方法同实施例1。
实施例3
一种耐高温型PVC装饰膜，所述耐高温涂覆层包括以质量份计的如下原料：
催化剂为二月桂酸二正辛基锡，用量为3-氯丙基甲基二甲氧基硅烷质量的0.08％；盐酸质量分数为30％。
所述PVC裸膜包括PVC树脂、DOP增塑剂与热稳定剂，其质量比对应为100:25:3；热稳定剂为有机锡液体热稳定剂硫醇甲基锡。
制备方法同实施例1。
实施例4
一种耐高温型PVC装饰膜，所述耐高温涂覆层包括以质量份计的如下原料：
催化剂为二月桂酸二正辛基锡，用量为3-氯丙基甲基二甲氧基硅烷质量的0.07％；盐酸质量分数为30％。
所述PVC裸膜包括PVC树脂、DOP增塑剂与热稳定剂，其质量比对应为100:25:3；热稳定剂为有机锡液体热稳定剂硫醇甲基锡。
制备方法同实施例1。
对比例1：
采用PVC裸膜作为对比。
PVC裸膜包括PVC树脂、DOP增塑剂与热稳定剂，其质量比对应为100:25:3；热稳定剂为有机锡液体热稳定剂硫醇甲基锡。
测试方法：
附着力测试依据GB/T 9286-1998《色漆与清漆漆膜的划格试验》，耐高温性能是将PVC膜首先固定在平整的台面上，然后将加热至170℃/200℃的圆形砝码(重量200g)用镊子直接取出放在PVC膜上进行自然冷却，冷却至室温后观察PVC膜与砝码接触位置变化。耐磨性能测试GB/T23988-2009《涂料耐磨性能测定落砂法》，单位膜层磨损所需要的落砂量越大，表示耐磨性越好。
上述实施例和对比例制得PVC装饰膜测试结果如下表1中所示。
表1PVC装饰膜性能
从表1可以看出，本发明产品经过特殊工艺及配方制备的PVC装饰膜表观平整光滑、固化后的涂膜附着力也出色，附着力等级达到0级，在180℃及200℃承重式的热压下，均无明显变化，说明环氧改性的有机硅涂层固化成膜后，耐高温性能出色，且有机硅涂膜的疏水能力强，光滑度高，耐磨性能也较裸膜有明显的提高。
对比例1是采用普通的PVC裸膜，其在180℃承重热压时表面即有轻微不平，这说明有轻微熔化，而在200℃热压时更为明显，且耐磨性能也低于本发明特殊涂装后的涂膜。
以上只通过说明的方式描述了本发明的某些示范性实施例，毋庸置疑，对于本领域的普通技术人员，在不偏离本发明的精神和范围的情况下，可以用各种不同的方式对所描述的实施例进行修正。因此，上述描述在本质上是说明性的，不应理解为对本发明权利要求保护范围的限制。
Claims (9)
1.一种耐高温型PVC装饰膜，其特征在于，该装饰膜通过将PVC裸膜进行耐高温涂覆成型加工而成的；耐高温涂覆层使用包括小粒径硅溶胶、甲基苯基二甲氧基硅烷、3-氯丙基甲基二甲氧基硅烷、3-氨基丙基三甲氧基硅烷、E-51环氧树脂、三羟甲基丙烷三缩水甘油醚、N-(2-氨乙基)-3-氨丙基甲基二乙氧基硅烷在内的原料制成高分子涂料，然后经过加热烘干固化成型。
2.如权利要求1所述一种耐高温型PVC装饰膜，其特征在于，所述耐高温涂覆层包括以质量份计的如下原料：
原料中还包括盐酸与催化剂。
3.如权利要求2所述一种耐高温型PVC装饰膜，其特征在于，催化剂为二月桂酸二正辛基锡，用量为3-氯丙基甲基二甲氧基硅烷质量的0.05-0.08％；盐酸质量分数为28-30％。
4.如权利要求2所述一种耐高温型PVC装饰膜，其特征在于，小粒径硅溶胶的粒径为10-15nm。
5.如权利要求1所述一种耐高温型PVC装饰膜，其特征在于，所述PVC裸膜包括PVC树脂、DOP增塑剂与热稳定剂，其质量比对应为100:25:3；热稳定剂为有机锡液体热稳定剂硫醇甲基锡。
6.如权利要求1-5任一项所述一种耐高温型PVC装饰膜的制备方法，其特征在于，包括以下步骤：
A、将配方量的小粒径硅溶胶、甲基苯基二甲氧基硅烷、3-氯丙基甲基二甲氧基硅烷及异丙醇加入反应釜中，启动搅拌，加入质量分数为28-30％的盐酸，调节溶液的pH至4-4.5，然后加热至70℃-75℃进行聚合反应；
B、取样检测，待体系聚合物的粘度达到700-900mPa·s(25℃)时，将配方量的催化剂、3-氨基丙基三甲氧基硅烷加入反应釜中，并继续在70-75℃保温进行扩链聚合反应；
C、取样检测，待体系聚合物的粘度达到1300-1500mPa·s(25℃)时，此时加入配方量的E-51环氧树脂、三羟甲基丙烷三缩水甘油醚的混合原料，在76-79℃进行接枝聚合反应；
D、取样检测，待聚合物的粘度达到1900-2100mPa·s(25℃)时，降温至室温，加入配方量的N-(2-氨乙基)-3-氨丙基甲基二乙氧基硅烷，室温充分搅拌均匀后，出料得到PVC裸膜专用耐高温型产品；
E、取已经制备好的PVC裸膜产品，将D步骤得到的产品采用采用精密涂布机在PVC裸膜的单面涂布耐高温涂层；涂布后进入烘房进行加热烘干固化处理，然后冷却收卷即可得到耐高温型PVC装饰膜。
7.如权利要求6所述一种耐高温、耐磨型PVC装饰膜的制备方法，其特征在于，步骤E中，所述PVC裸膜包括PVC树脂、DOP增塑剂与热稳定剂，其质量比对应为100:25:3；热稳定剂为有机锡液体热稳定剂硫醇甲基锡。
8.如权利要求6所述一种耐高温、耐磨型PVC装饰膜的制备方法，其特征在于，步骤E中，涂布湿膜厚度控制在35-40μm。
9.如权利要求6所述一种耐高温、耐磨型PVC装饰膜的制备方法，其特征在于，步骤E中，烘干固化温度控制在90-95℃，烘干固化时间保持在3-3.5min。
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