CN106273836A - 一种高耐候性隔热膜的制备方法 - Google Patents
一种高耐候性隔热膜的制备方法 Download PDFInfo
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- 238000002955 isolation Methods 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000003756 stirring Methods 0.000 claims abstract description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000376 reactant Substances 0.000 claims abstract description 26
- 239000011521 glass Substances 0.000 claims abstract description 22
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 20
- 239000013078 crystal Substances 0.000 claims abstract description 20
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000725 suspension Substances 0.000 claims abstract description 16
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 14
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 11
- 229960004756 ethanol Drugs 0.000 claims abstract description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000010408 film Substances 0.000 claims description 44
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- 239000011248 coating agent Substances 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- JHJUUEHSAZXEEO-UHFFFAOYSA-M sodium;4-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=C(S([O-])(=O)=O)C=C1 JHJUUEHSAZXEEO-UHFFFAOYSA-M 0.000 claims description 6
- 239000010409 thin film Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- 125000005395 methacrylic acid group Chemical class 0.000 claims description 3
- 239000003643 water by type Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 6
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 abstract description 5
- 238000002834 transmittance Methods 0.000 abstract description 5
- 230000032683 aging Effects 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 238000009413 insulation Methods 0.000 description 12
- 238000012216 screening Methods 0.000 description 4
- 229910003978 SiClx Inorganic materials 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 3
- 241000790917 Dioxys <bee> Species 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 238000000034 method Methods 0.000 description 2
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- 125000004494 ethyl ester group Chemical group 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- -1 methacryloxypropyl Chemical group 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种高耐候性隔热膜的制备方法，属于隔热膜制备技术领域。本发明将制备的氮化硅晶须浆液与乙醇搅拌混合制得悬浮液，再利用正硅酸乙酯、无水乙醇和催化剂反应，制得的二氧化硅醇溶胶，并接枝甲基丙烯酸制得改性二氧化硅溶胶，将改性二氧化硅溶胶与上述悬浮液混合并加热反应，得到的反应液涂覆在清洗干燥后的玻璃板表面，反复涂覆、干燥工序，即可得高耐候性隔热膜，本发明制备工艺简单，制得的隔热膜具有优异的耐磨、耐候性及稳定性，隔热膜透光率高，隔热性能充分，对于紫外、紫外线的反射率高，不易老化，具有广泛的应用前景。
Description
技术领域
本发明公开了一种高耐候性隔热膜的制备方法，属于隔热膜制备技术领域。
背景技术
隔热膜又被称为防晒隔热膜，“防晒”是指能有效阻隔紫外线达90%以上。第三代产品运用了很多新技术，如“磁控镀膜”、“微米技术”、“纳米技术”、“航天科技”等，紫外线阻隔率提高到90～100%左右，红外线阻隔率提高到30～95%左右，胶的粘性更强，从而达到既降低膜的厚度又提高了防爆性能的效果。
汽车后市场渐渐成为“黄金产业”，而汽车防晒隔热膜市场在汽车后市场中所占的比重已经相当重了，毕竟在夏日里需要防晒隔热，需要防止紫外线的辐射对人体造成伤害，还可以有效防爆以最低限度的减少事故危害。随着私车家的增加，防晒隔热膜市场一片繁荣景象，行业渐渐发展起来。
隔热膜能有效阻挡太阳辐射的热量，防止热气进去室内，无须花钱把热气泵出。与窗帘和百叶窗不同，太阳隔热膜挡掉可能会通过窗户进入屋内高达79%的热气，换言之这相当于每100平方英尺承受阳光照射的玻璃每小时可节约12000个英国热量单位。
目前市面上的隔热膜大致可分为三种： (1)染色膜：就是一般所称的普通膜，这种隔热膜用起来就象是糊灯笼的玻璃纸，可说是一点隔热效果也没有，而且视线非常的差，因此时间一久就会慢慢褪色，而且受热后会散发异味。(2)半反光纸：这种太阳膜通常是4S店赠送用户的那种，隔热率大约20%～30%。(3)防爆隔热膜：具有双重效果，防爆隔热膜具有耐磨、半反光和防爆的功能，万一遇到碰撞，玻璃破碎时，还要以有效防止碎片飞散，不会危害到驾驶者的安全，安全性相当高，隔热率可以达到50%以上。
现有技术制备的隔热膜耐磨性及稳定性较差，容易老化脱落，且耐候性较差，对于红外线、紫外线的反射率较低，隔热膜透光率较低，隔热性不充分。
发明内容
本发明主要解决的技术问题：针对目前技术制备的隔热膜耐磨性及稳定性较差，容易老化脱落，且耐候性较差，对于红外线、紫外线的反射率较低，隔热膜透光率较低，隔热性不充分的问题，提供一种高耐候性隔热膜的制备方法，该方法将制备的氮化硅晶须浆液与乙醇搅拌混合制得悬浮液，再利用正硅酸乙酯、无水乙醇和催化剂反应，制得的二氧化硅醇溶胶，并接枝甲基丙烯酸制得改性二氧化硅溶胶，将改性二氧化硅溶胶与上述悬浮液混合并加热反应，得到的反应液涂覆在清洗干燥后的玻璃板表面，反复涂覆、干燥工序，即可得高耐候性隔热膜，本发明制备工艺简单，制得的隔热膜具有优异的耐磨、耐候性及稳定性，隔热膜透光率高，隔热性能充分，对于紫外、紫外线的反射率高，不易老化，具有广泛的应用前景。
为了解决上述技术问题，本发明所采用的技术方案是：
（1）称取20～30g氮化硅晶须，按固液比1：4与质量分数3%十二烷基苯磺酸钠溶液混合，搅拌混合30～50min后得到氮化硅晶须浆液，将氮化硅晶须浆液按体积比1：2与质量分数80%乙醇混合后在300～500r/min转速下机械搅拌1～2h，搅拌后得悬浮液，备用；
（2）依次取20.8～22.5mL正硅酸乙酯、275～285mL无水乙醇和70～80mL去离子水加入到三口烧瓶中，用质量分数10%氢氧化钠溶液调节pH为8.0后放入水浴锅中，在50～60℃温度下搅拌反应8～10h，反应后冷却至室温并出料，得到二氧化硅醇溶胶；
（3）量取100～150mL上述二氧化硅醇溶胶加入500mL三口烧瓶中，向三口烧瓶中加入0.5～0.7g甲基丙烯酰氧基丙基三甲氧基硅烷和50～60mL甲基丙烯酸，放入水浴锅中，在70～80℃温度下搅拌反应3～5h，反应结束后，得到改性二氧化硅溶胶；
（4）将上述制备得到的改性二氧化硅溶胶按体积比20：1与步骤（1）备用的悬浮液混合得混合液，将混合液加热至36～38℃，并保温搅拌反应15～20h，搅拌结束后冷却至室温，得反应液；
（5）将玻璃板分别用去离子水、无水乙醇、丙酮超声清洗5～10min后用吹风机吹干表面，将干燥的玻璃板表面均匀涂覆上述反应液，涂覆后放入烘箱中在80～100℃干燥60～80min后取出，再涂覆一层上述反应液，放入鼓风干燥箱中，在150～180℃温度下干燥1～2h后取出，并均匀涂覆一层上述反应液，放入真空干燥箱中在200～220℃温度下干燥2～4h，干燥后取出，冷却至室温后将薄膜从玻璃板下取下，最终形成厚度为0.8～1.2mm的隔热膜。
经检测，本发明制得的高耐候性隔热膜其可见光透过率在85%以上，同时具有70～80%的近红外屏蔽率，98～99%的紫外光屏蔽率，且耐温范围在-300～500℃，导热系数在0.03W/m·K以下，具有优异的隔热性能，使用寿命较普通的隔热膜长3倍以上。
本发明的有益效果是：
（1）本发明制得的高耐候性隔热膜牢固性强，隔热效果及耐磨性好，隔热膜整体性能稳定，提高了隔热膜使用寿命；
（2）本发明制得的高耐候性隔热膜耐候性及稳定性好，对于紫外、紫外线的反射率高，透光率佳高。
具体实施方式
首先称取20～30g氮化硅晶须，按固液比1：4与质量分数3%十二烷基苯磺酸钠溶液混合，搅拌混合30～50min后得到氮化硅晶须浆液，将氮化硅晶须浆液按体积比1：2与质量分数80%乙醇混合后在300～500r/min转速下机械搅拌1～2h，搅拌后得悬浮液，备用；随后依次取20.8～22.5mL正硅酸乙酯、275～285mL无水乙醇和70～80mL去离子水加入到三口烧瓶中，用质量分数10%氢氧化钠溶液调节pH为8.0后放入水浴锅中，在50～60℃温度下搅拌反应8～10h，反应后冷却至室温并出料，得到二氧化硅醇溶胶；再量取100～150mL上述二氧化硅醇溶胶加入500mL三口烧瓶中，向三口烧瓶中加入0.5～0.7g甲基丙烯酰氧基丙基三甲氧基硅烷和50～60mL甲基丙烯酸，放入水浴锅中，在70～80℃温度下搅拌反应3～5h，反应结束后，得到改性二氧化硅溶胶；再将上述制备得到的改性二氧化硅溶胶按体积比20：1与上述步骤备用的悬浮液混合得混合液，将混合液加热至36～38℃，并保温搅拌反应15～20h，搅拌结束后冷却至室温，得反应液；最后将玻璃板分别用去离子水、无水乙醇、丙酮超声清洗5～10min后用吹风机吹干表面，将干燥的玻璃板表面均匀涂覆上述反应液，涂覆后放入烘箱中在80～100℃干燥60～80min后取出，再涂覆一层上述反应液，放入鼓风干燥箱中，在150～180℃温度下干燥1～2h后取出，并均匀涂覆一层上述反应液，放入真空干燥箱中在200～220℃温度下干燥2～4h，干燥后取出，冷却至室温后将薄膜从玻璃板下取下，最终形成厚度为0.8～1.2mm的隔热膜。
实例1
首先称取20g氮化硅晶须，按固液比1：4与质量分数3%十二烷基苯磺酸钠溶液混合，搅拌混合30min后得到氮化硅晶须浆液，将氮化硅晶须浆液按体积比1：2与质量分数80%乙醇混合后在300r/min转速下机械搅拌1h，搅拌后得悬浮液，备用；随后依次取20.8mL正硅酸乙酯、275mL无水乙醇和70mL去离子水加入到三口烧瓶中，用质量分数10%氢氧化钠溶液调节pH为8.0后放入水浴锅中，在50℃温度下搅拌反应8h，反应后冷却至室温并出料，得到二氧化硅醇溶胶；再量取100mL上述二氧化硅醇溶胶加入500mL三口烧瓶中，向三口烧瓶中加入0.5g甲基丙烯酰氧基丙基三甲氧基硅烷和50mL甲基丙烯酸，放入水浴锅中，在70℃温度下搅拌反应3h，反应结束后，得到改性二氧化硅溶胶；再将上述制备得到的改性二氧化硅溶胶按体积比20：1与上述步骤备用的悬浮液混合得混合液，将混合液加热至36℃，并保温搅拌反应15h，搅拌结束后冷却至室温，得反应液；最后将玻璃板分别用去离子水、无水乙醇、丙酮超声清洗5min后用吹风机吹干表面，将干燥的玻璃板表面均匀涂覆上述反应液，涂覆后放入烘箱中在80℃干燥60min后取出，再涂覆一层上述反应液，放入鼓风干燥箱中，在150℃温度下干燥1h后取出，并均匀涂覆一层上述反应液，放入真空干燥箱中在200℃温度下干燥2h，干燥后取出，冷却至室温后将薄膜从玻璃板下取下，最终形成厚度为0.8mm的隔热膜。
经实例检测，本发明制得的高耐候性隔热膜其可见光透过率为88%，同时具有70%的近红外屏蔽率，98%的紫外光屏蔽率，且耐低温度为-300℃，导热系数为0.02W/m·K，具有优异的隔热性能，使用寿命较普通的隔热膜长3.5倍。
实例2
首先称取25g氮化硅晶须，按固液比1：4与质量分数3%十二烷基苯磺酸钠溶液混合，搅拌混合40min后得到氮化硅晶须浆液，将氮化硅晶须浆液按体积比1：2与质量分数80%乙醇混合后在400r/min转速下机械搅拌1.5h，搅拌后得悬浮液，备用；随后依次取21.7mL正硅酸乙酯、280mL无水乙醇和75mL去离子水加入到三口烧瓶中，用质量分数10%氢氧化钠溶液调节pH为8.0后放入水浴锅中，在55℃温度下搅拌反应9h，反应后冷却至室温并出料，得到二氧化硅醇溶胶；再量取125mL上述二氧化硅醇溶胶加入500mL三口烧瓶中，向三口烧瓶中加入0.6g甲基丙烯酰氧基丙基三甲氧基硅烷和55mL甲基丙烯酸，放入水浴锅中，在75℃温度下搅拌反应4h，反应结束后，得到改性二氧化硅溶胶；再将上述制备得到的改性二氧化硅溶胶按体积比20：1与上述步骤备用的悬浮液混合得混合液，将混合液加热至37℃，并保温搅拌反应18h，搅拌结束后冷却至室温，得反应液；最后将玻璃板分别用去离子水、无水乙醇、丙酮超声清洗8min后用吹风机吹干表面，将干燥的玻璃板表面均匀涂覆上述反应液，涂覆后放入烘箱中在90℃干燥70min后取出，再涂覆一层上述反应液，放入鼓风干燥箱中，在165℃温度下干燥1.5h后取出，并均匀涂覆一层上述反应液，放入真空干燥箱中在210℃温度下干燥3h，干燥后取出，冷却至室温后将薄膜从玻璃板下取下，最终形成厚度为1.0mm的隔热膜。
经实例检测，本发明制得的高耐候性隔热膜其可见光透过率为92%，同时具有75%的近红外屏蔽率，98.5%的紫外光屏蔽率，且耐热温度为100℃，导热系数为0.015W/m·K，具有优异的隔热性能，使用寿命较普通的隔热膜长4倍。
实例3
首先称取30g氮化硅晶须，按固液比1：4与质量分数3%十二烷基苯磺酸钠溶液混合，搅拌混合50min后得到氮化硅晶须浆液，将氮化硅晶须浆液按体积比1：2与质量分数80%乙醇混合后在500r/min转速下机械搅拌2h，搅拌后得悬浮液，备用；随后依次取22.5mL正硅酸乙酯、285mL无水乙醇和80mL去离子水加入到三口烧瓶中，用质量分数10%氢氧化钠溶液调节pH为8.0后放入水浴锅中，在60℃温度下搅拌反应10h，反应后冷却至室温并出料，得到二氧化硅醇溶胶；再量取150mL上述二氧化硅醇溶胶加入500mL三口烧瓶中，向三口烧瓶中加入0.7g甲基丙烯酰氧基丙基三甲氧基硅烷和60mL甲基丙烯酸，放入水浴锅中，在80℃温度下搅拌反应5h，反应结束后，得到改性二氧化硅溶胶；再将上述制备得到的改性二氧化硅溶胶按体积比20：1与上述步骤备用的悬浮液混合得混合液，将混合液加热至38℃，并保温搅拌反应20h，搅拌结束后冷却至室温，得反应液；最后将玻璃板分别用去离子水、无水乙醇、丙酮超声清洗10min后用吹风机吹干表面，将干燥的玻璃板表面均匀涂覆上述反应液，涂覆后放入烘箱中在100℃干燥80min后取出，再涂覆一层上述反应液，放入鼓风干燥箱中，在180℃温度下干燥2h后取出，并均匀涂覆一层上述反应液，放入真空干燥箱中在220℃温度下干燥4h，干燥后取出，冷却至室温后将薄膜从玻璃板下取下，最终形成厚度为1.2mm的隔热膜。
经实例检测，本发明制得的高耐候性隔热膜其可见光透过率为95%，同时具有80%的近红外屏蔽率，99%的紫外光屏蔽率，且耐高温度为500℃，导热系数为0.01W/m·K，具有优异的隔热性能，使用寿命较普通的隔热膜长4.5倍。
Claims (1)
1.一种高耐候性隔热膜的制备方法，其特征在于具体制备方法：
（1）称取20～30g氮化硅晶须，按固液比1：4与质量分数3%十二烷基苯磺酸钠溶液混合，搅拌混合30～50min后得到氮化硅晶须浆液，将氮化硅晶须浆液按体积比1：2与质量分数80%乙醇混合后在300～500r/min转速下机械搅拌1～2h，搅拌后得悬浮液，备用；
（2）依次取20.8～22.5mL正硅酸乙酯、275～285mL无水乙醇和70～80mL去离子水加入到三口烧瓶中，用质量分数10%氢氧化钠溶液调节pH为8.0后放入水浴锅中，在50～60℃温度下搅拌反应8～10h，反应后冷却至室温并出料，得到二氧化硅醇溶胶；
（3）量取100～150mL上述二氧化硅醇溶胶加入500mL三口烧瓶中，向三口烧瓶中加入0.5～0.7g甲基丙烯酰氧基丙基三甲氧基硅烷和50～60mL甲基丙烯酸，放入水浴锅中，在70～80℃温度下搅拌反应3～5h，反应结束后，得到改性二氧化硅溶胶；
（4）将上述制备得到的改性二氧化硅溶胶按体积比20：1与步骤（1）备用的悬浮液混合得混合液，将混合液加热至36～38℃，并保温搅拌反应15～20h，搅拌结束后冷却至室温，得反应液；
（5）将玻璃板分别用去离子水、无水乙醇、丙酮超声清洗5～10min后用吹风机吹干表面，将干燥的玻璃板表面均匀涂覆上述反应液，涂覆后放入烘箱中在80～100℃干燥60～80min后取出，再涂覆一层上述反应液，放入鼓风干燥箱中，在150～180℃温度下干燥1～2h后取出，并均匀涂覆一层上述反应液，放入真空干燥箱中在200～220℃温度下干燥2～4h，干燥后取出，冷却至室温后将薄膜从玻璃板下取下，最终形成厚度为0.8～1.2mm的隔热膜。
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| CN109627870A (zh) * | 2018-12-06 | 2019-04-16 | 天津中亚慧通科技有限公司 | 一种高耐候性防雾隔热膜的制备工艺 |
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