WO2018103063A1 - 一种纳米ato透明隔热节能玻璃涂层的制作工艺 - Google Patents

一种纳米ato透明隔热节能玻璃涂层的制作工艺 Download PDF

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WO2018103063A1
WO2018103063A1 PCT/CN2016/109160 CN2016109160W WO2018103063A1 WO 2018103063 A1 WO2018103063 A1 WO 2018103063A1 CN 2016109160 W CN2016109160 W CN 2016109160W WO 2018103063 A1 WO2018103063 A1 WO 2018103063A1
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stirring
ato
water
treatment
glass
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PCT/CN2016/109160
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French (fr)
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王涛
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苏州蓝锐纳米科技有限公司
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Priority to PCT/CN2016/109160 priority Critical patent/WO2018103063A1/zh
Publication of WO2018103063A1 publication Critical patent/WO2018103063A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B37/00—Compounds having molecular sieve properties but not having base-exchange properties
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00—Compounds of tin
    • C01G19/02—Oxides
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04—Polyurethanes

Definitions

  • the invention relates to the technical field of glass coating, in particular to a manufacturing process of nano-ATO transparent heat-insulating energy-saving glass coating.
  • thermal insulation glass is energy saving and emission reduction.
  • the number of air conditioners and cooling starts can be greatly reduced.
  • heat is reduced to the outside, and ultraviolet rays can also block the aging damage of human body and indoor objects.
  • the mature insulating glass on the market has the following types: 1. Insulating glass, although the insulating glass is better than the single-layer glass in winter, but it can not resist the infrared rays emitted by the summer sun, so the insulating glass can not function in the summer. 2.
  • Louis Glass Louis Glass is a coated glass, its performance is very good, whether it is good in summer or winter insulation, but because of the huge investment in production of Louis Glass, the technical difficulty, so the price is expensive, making it difficult for ordinary people. accept. 3. Stained glass, this type of glass is currently used more than glass curtain wall, mainly for aesthetics. Privacy does not play a role in thermal insulation, but also blocks certain visible light to darken the room, while looking out to the outside is always feeling Yin Heaven brings unhappiness to people's moods. 4. Glass film, the real effect of the glass film is expensive, the bad film is counter-inverted, so that the more hot and hot, this car family should have feelings.
  • ATO yttrium-doped tin oxide
  • Light Resistant to organic solvents. Not oxidized. Flame retardant. High temperature and corrosion resistance. Good mechanical stability.
  • ATO nanoparticles have very low absorbance in the visible light (380 nm - 780 nm) band, so they have high transparency.
  • the method used on the market is to directly disperse the ordinary ATO powder in an alcohol-soluble or water-soluble resin.
  • the disadvantage is that the particle size distribution is wide.
  • the morphology is amorphous.
  • the dispersed particle size is mixed in the resin. Therefore, it can only play the role of infrared absorption, that is to say, even if the ATO insulation material acts to block the infrared rays, the glass increases by 10-20 degrees than the room temperature, thus forming a natural radiator to radiate heat to the room twice. The effect of indoor cooling is not great.
  • a nano-ATO transparent heat-insulating energy-saving glass coating process was proposed.
  • the object of the present invention is to provide a process for fabricating a nano-ATO transparent heat-insulating and energy-saving glass coating to solve the problems raised in the above background art.
  • a nano ATO transparent heat-insulating energy-saving glass coating manufacturing process comprising the following steps:
  • raw material preparation water-soluble ATO powder, water-based resin, mesoporous silica particles;
  • melt water treatment dissolve the water-soluble ATO powder in water, stir at the same time, stirring speed 240-260r/min, stirring time 60-75min, stirring temperature 50-60 ° C, after stirring, get ATO solution, where water soluble
  • the ATO powder accounts for 45-55% of the powder, and the balance is water;
  • S4 particle treatment adding mesoporous silica particles to the mixed solution obtained after S3 treatment, stirring at the same time, stirring speed 200-250r/min, stirring temperature 55-65 ° C, stirring time 100-120min, after stirring is completed Producing a slurry of particles, wherein the proportion of mesoporous silica particles is 65-75%;
  • drying treatment the slurry of the particles treated in S4 is evenly sprayed on the glass table by spraying equipment The surface is sprayed to a thickness of 0.5-1 mm, and is naturally dried at a normal temperature, and after drying, a film can be formed on the surface of the glass.
  • the aqueous resin is an aqueous polyurethane.
  • the mesoporous silica particles have a mesoporosity of 65-75% and a particle diameter of 12-15 nm.
  • the performance data of the glass after using the coating is as follows: visible light transmittance: 70% (spectrophotometer), infrared reflectivity: 60% - 70% (spectrophotometer), heat insulation rate: 50% -60% (infrared heat tester), hardness: 3H (pencil hardness tester), service life: 10 years (artificial aging), summer indoor and outdoor temperature difference: 7-15 degrees energy saving 20% -30%.
  • the invention has the beneficial effects that the ATO powder is directly added to the aqueous resin after being dissolved in water.
  • the cumbersome grinding and dispersion process is eliminated, and no additives such as dispersing agents and grinding aids and anti-settling agents are added.
  • ATO is dispersed in atomic form in aqueous resin, arranged in order.
  • the nanoparticles are spherical monodisperse and agglomerated, with high similarity and narrow particle size distribution. Nanoparticles are made by using nano-scale silica as template in production.
  • the mesoporous morphology is used as a shield for outdoor cold radiation in winter. After the coating is dried, the nanoparticles are arranged in the form of photonic crystals, so they have a high reflectance to infrared rays. After use, the indoor temperature will be lower than the external temperature in summer, and warmer in winter.
  • a nano ATO transparent heat-insulating energy-saving glass coating manufacturing process comprises the following steps:
  • S1 raw material preparation water-soluble ATO powder, water-based resin, mesoporous silica particles, the aqueous resin is water-based polyurethane, the mesoporous silica particles having a mesoporosity of 65%, a particle diameter of 12 nm;
  • melt water treatment dissolve the water-soluble ATO powder in water while stirring, stirring speed 240r / min, stirring time 60min, stirring temperature 50 ° C, after the completion of the stirring to obtain ATO solution, wherein the water-soluble ATO powder accounted for 45%, the balance is water;
  • Drying treatment The slurry of the particles treated in S4 is uniformly sprayed on the surface of the glass by a spraying device, and the thickness of the spraying is 0.5 mm, and the film is naturally dried at normal temperature, and after drying, a film can be formed on the surface of the glass.
  • a nano ATO transparent heat-insulating energy-saving glass coating manufacturing process comprises the following steps:
  • S1 raw material preparation water-soluble ATO powder, water-based resin, mesoporous silica particles, the aqueous resin is water-based polyurethane, the mesoporous silica particles have a mesoporosity of 75%, a particle diameter of 15 nm;
  • melt water treatment the water-soluble ATO powder is dissolved in water, stirring at the same time, stirring speed 260r / min, stirring time 75min, stirring temperature 60 ° C, after stirring is completed to obtain ATO solution, wherein the proportion of water-soluble ATO powder 55%, the balance is water;
  • drying treatment the slurry of the particles treated in S4 is evenly sprayed on the glass through the spraying equipment.
  • the surface of the glass is sprayed to a thickness of 1 mm, and is naturally dried at room temperature. After drying, a film can be formed on the surface of the glass.
  • a nano ATO transparent heat-insulating energy-saving glass coating manufacturing process comprises the following steps:
  • S1 raw material preparation: water-soluble ATO powder, water-based resin, mesoporous silica particles, the aqueous resin is aqueous polyurethane, the mesoporous silica particles having a mesoporosity of 67%, a particle diameter of 14 nm;
  • melt water treatment dissolve the water-soluble ATO powder in water, stir at the same time, stirring speed 245r/min, stirring time 65min, stirring temperature 55 °C, after stirring, ATO solution is obtained, wherein the proportion of water-soluble ATO powder 46%, the balance is water;
  • Drying treatment The slurry of the particles treated in S4 is uniformly sprayed on the surface of the glass by a spraying device, and the thickness of the spraying is 0.6 mm, and the film is naturally dried at normal temperature, and after drying, a film can be formed on the surface of the glass.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Paints Or Removers (AREA)

Abstract

一种纳米ATO透明隔热节能玻璃涂层的制作工艺，包括如下步骤：原料准备：融水处理、混合处理、粒子处理和干燥处理；将ATO粉体溶于水中后直接加入水性树脂中。省去了繁琐的研磨与分散工艺，无需添加分散剂与研磨助剂以及防沉剂等助剂。ATO在水性树脂中以原子形态分散，排列有序，纳米粒子为球形单分散无团聚，相似度高，粒径分布窄，纳米粒子在生产时用了纳米级二氧化硅做模板将其制成了介孔形态以作为冬天对室外冷辐射屏蔽的性能。涂层干燥后纳米粒子会以光子晶体形式排列，因此对红外线有很高的反射率，使用后室内温度夏天会比外部温度降低，而冬天则更保暖。

Description

一种纳米ATO透明隔热节能玻璃涂层的制作工艺 技术领域
本发明涉及玻璃涂层技术领域，具体为一种纳米ATO透明隔热节能玻璃涂层的制作工艺。
背景技术
全球变暖温度升高这是个不争的事实，同时也给节能环保行业带来了生机。现在就国内建筑来讲不管是高楼大厦还是多层建筑玻璃的使用面积越来越大而室内夏天热辐射主要是来自于玻璃(可占到60％以上)，冬天室内散热也主要是通过玻璃散发的。现在虽然室外墙体国家已经实行强制保温了但是玻璃行业国家目前还没出台政策，原因是国内对于这种产品的研究还刚刚起步，能够掌握核心技术的企业很少，大部分企业使用的核心原料依赖进口，其价格昂贵，导致成品价格过高难以推广。如果现在有一种效果好的产品而且价格又适中那么相信国家很快就会出台强制玻璃保温的政策。保温隔热玻璃最大的好处是节能减排，夏天可大幅度减少空调制冷启动次数，冬天减少热量向室外散发，同时还可阻挡紫外线对人体及室内物品的老化损坏。目前市场上成熟的保温玻璃有以下几种.1.中空玻璃，中空玻璃虽然在冬天比单层玻璃保温效果要好但是它不能抵挡夏天太阳发射的红外线，所以中空玻璃在夏天起不了作用。2.路易玻璃，路易玻璃是一种镀膜玻璃，其性能很好，不管是夏天还是冬天保温效果都很好，但是由于生产路易玻璃投资巨大，技术难度强，因此导致其价格昂贵使普通老百姓难以接受。3.染色玻璃，这类玻璃目前玻璃幕墙使用较多，主要起美观.隐私作用并不起保温隔热作用，同时还会阻挡一定的可见光使室内变暗，同时向室外望去老是感觉阴天，给人们的心情带来不快。4.玻璃贴膜，真正有效果的玻璃贴膜价格昂贵，不好的贴膜反倒起反作用，以致越贴越热，这个有车一族应该都有感受。
ATO(锑掺杂氧化锡)颜色为灰蓝色粉体，具有耐化学性.耐酸.耐碱.耐 光.耐有机溶剂.不氧化.阻燃.耐高温耐腐蚀.机械稳定性好等特点。ATO纳米粒子对可见光(380纳米-780纳米)波段的吸收性极弱，所以有着高透明性。
目前市面上所用的方法是将普通ATO粉体经研磨后直接分散在醇溶性或者水溶性树脂中，其弊端在于粒径尺寸分布宽.形貌为无定型.在树脂中分散杂乱粒径排列混杂.因此只能起到红外吸收的作用，也就是说即便ATO隔热材料起到了阻挡红外线作用的同时玻璃要比室温增加10-20度因而形成了一个天然暖气片二次向室内辐射热量所以对室内降温的作用不是很大。为此，提出一种纳米ATO透明隔热节能玻璃涂层的制作工艺。
发明内容
本发明的目的在于提供一种纳米ATO透明隔热节能玻璃涂层的制作工艺，以解决上述背景技术中提出的问题。
为实现上述目的，本发明提供如下技术方案：一种纳米ATO透明隔热节能玻璃涂层的制作工艺，包括如下步骤：
S1、原料准备：水溶性ATO粉体，水性树脂，介孔二氧化硅粒子；
S2、融水处理：将水溶性ATO粉体溶于水中，同时进行搅拌，搅拌速度240-260r/min，搅拌时间60-75min，搅拌温度50-60℃，搅拌完成后得到ATO溶液，其中水溶性ATO粉体占比45-55％，余量为水；
S3、混合处理：向S2中制得的ATO溶液加入水性树脂，同时再次进行搅拌，搅拌速度300-350r/min，搅拌温度55-65℃，搅拌时间45-55min，搅拌完成后制得混合溶液，其中ATO溶液占比30-45％，余量为水性树脂；
S4、粒子处理：向S3处理后得到的混合溶液内添加介孔二氧化硅粒子，同时进行搅拌，搅拌速度200-250r/min，搅拌温度55-65℃，搅拌时间100-120min，搅拌完成后制得粒子浆体，其中介孔二氧化硅粒子占比为65-75％；
S5、干燥处理：将S4中处理后的粒子浆体通过喷涂设备均匀喷在玻璃表 面，喷涂厚度为0.5-1mm，在常温下进行自然干燥，干燥成后即可在玻璃表面形成膜。
优选的，所述水性树脂为水性聚氨酯。
优选的，所述介孔二氧化硅粒子介孔率为65-75％，粒径12-15nm。
通过实验得出，玻璃使用该涂层后的性能数据如下：可见光透过率：70％(分光光度计)，红外反射率：60％-70％(分光光度计)，隔热率：50％-60％(红外线热量测试仪)，硬度：3H(铅笔硬度计)，使用寿命：10年(人工老化)，夏天室内与室外温差：7-15度节能20％-30％。
与现有技术相比，本发明的有益效果是：本发明将ATO粉体溶于水中后直接加入水性树脂中。省去了繁琐的研磨与分散工艺，无需添加分散剂与研磨助剂以及防沉剂等助剂。ATO在水性树脂中以原子形态分散，排列有序，纳米粒子为球形单分散无团聚，相似度高，粒径分布窄，纳米粒子在生产时用了纳米级二氧化硅做模板将其制成了介孔形态以作为冬天对室外冷辐射屏蔽的性能。涂层干燥后纳米粒子会以光子晶体形式排列，因此对红外线有很高的反射率，使用后室内温度夏天会比外部温度降低，而冬天则更保暖。
具体实施方式
下面将结合本发明实施例中的具体说明，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
一种纳米ATO透明隔热节能玻璃涂层的制作工艺，包括如下步骤：
S1、原料准备：水溶性ATO粉体，水性树脂，介孔二氧化硅粒子，所述水性树脂为水性聚氨酯，所述介孔二氧化硅粒子介孔率为65％，粒径12nm；
S2、融水处理：将水溶性ATO粉体溶于水中，同时进行搅拌，搅拌速度 240r/min，搅拌时间60min，搅拌温度50℃，搅拌完成后得到ATO溶液，其中水溶性ATO粉体占比45％，余量为水；
S3、混合处理：向S2中制得的ATO溶液加入水性树脂，同时再次进行搅拌，搅拌速度300r/min，搅拌温度55℃，搅拌时间45min，搅拌完成后制得混合溶液，其中ATO溶液占比30％，余量为水性树脂；
S4、粒子处理：向S3处理后得到的混合溶液内添加介孔二氧化硅粒子，同时进行搅拌，搅拌速度200r/min，搅拌温度55℃，搅拌时间100min，搅拌完成后制得粒子浆体，其中介孔二氧化硅粒子占比为65％；
S5、干燥处理：将S4中处理后的粒子浆体通过喷涂设备均匀喷在玻璃表面，喷涂厚度为0.5mm，在常温下进行自然干燥，干燥成后即可在玻璃表面形成膜。
实施例2
一种纳米ATO透明隔热节能玻璃涂层的制作工艺，包括如下步骤：
S1、原料准备：水溶性ATO粉体，水性树脂，介孔二氧化硅粒子，所述水性树脂为水性聚氨酯，所述介孔二氧化硅粒子介孔率为75％，粒径15nm；
S2、融水处理：将水溶性ATO粉体溶于水中，同时进行搅拌，搅拌速度260r/min，搅拌时间75min，搅拌温度60℃，搅拌完成后得到ATO溶液，其中水溶性ATO粉体占比55％，余量为水；
S3、混合处理：向S2中制得的ATO溶液加入水性树脂，同时再次进行搅拌，搅拌速度350r/min，搅拌温度65℃，搅拌时间55min，搅拌完成后制得混合溶液，其中ATO溶液占比45％，余量为水性树脂；
S4、粒子处理：向S3处理后得到的混合溶液内添加介孔二氧化硅粒子，同时进行搅拌，搅拌速度250r/min，搅拌温度65℃，搅拌时间120min，搅拌完成后制得粒子浆体，其中介孔二氧化硅粒子占比为75％；
S5、干燥处理：将S4中处理后的粒子浆体通过喷涂设备均匀喷在玻 璃表面，喷涂厚度为1mm，在常温下进行自然干燥，干燥成后即可在玻璃表面形成膜。
实施例3
一种纳米ATO透明隔热节能玻璃涂层的制作工艺，包括如下步骤：
S1、原料准备：水溶性ATO粉体，水性树脂，介孔二氧化硅粒子，所述水性树脂为水性聚氨酯，所述介孔二氧化硅粒子介孔率为67％，粒径14nm；
S2、融水处理：将水溶性ATO粉体溶于水中，同时进行搅拌，搅拌速度245r/min，搅拌时间65min，搅拌温度55℃，搅拌完成后得到ATO溶液，其中水溶性ATO粉体占比46％，余量为水；
S3、混合处理：向S2中制得的ATO溶液加入水性树脂，同时再次进行搅拌，搅拌速度312r/min，搅拌温度56℃，搅拌时间47min，搅拌完成后制得混合溶液，其中ATO溶液占比35％，余量为水性树脂；
S4、粒子处理：向S3处理后得到的混合溶液内添加介孔二氧化硅粒子，同时进行搅拌，搅拌速度222r/min，搅拌温度56℃，搅拌时间110min，搅拌完成后制得粒子浆体，其中介孔二氧化硅粒子占比为67％；
S5、干燥处理：将S4中处理后的粒子浆体通过喷涂设备均匀喷在玻璃表面，喷涂厚度为0.6mm，在常温下进行自然干燥，干燥成后即可在玻璃表面形成膜。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。

Claims (3)

  1. 一种纳米ATO透明隔热节能玻璃涂层的制作工艺，其特征在于：包括如下步骤：
    S1、原料准备：水溶性ATO粉体，水性树脂，介孔二氧化硅粒子；
    S2、融水处理：将水溶性ATO粉体溶于水中，同时进行搅拌，搅拌速度240-260r/min，搅拌时间60-75min，搅拌温度50-60℃，搅拌完成后得到ATO溶液，其中水溶性ATO粉体占比45-55％，余量为水；
    S3、混合处理：向S2中制得的ATO溶液加入水性树脂，同时再次进行搅拌，搅拌速度300-350r/min，搅拌温度55-65℃，搅拌时间45-55min，搅拌完成后制得混合溶液，其中ATO溶液占比30-45％，余量为水性树脂；
    S4、粒子处理：向S3处理后得到的混合溶液内添加介孔二氧化硅粒子，同时进行搅拌，搅拌速度200-250r/min，搅拌温度55-65℃，搅拌时间100-120min，搅拌完成后制得粒子浆体，其中介孔二氧化硅粒子占比为65-75％；
    S5、干燥处理：将S4中处理后的粒子浆体通过喷涂设备均匀喷在玻璃表面，喷涂厚度为0.5-1mm，在常温下进行自然干燥，干燥成后即可在玻璃表面形成膜。
  2. 根据权利要求1所述的一种纳米ATO透明隔热节能玻璃涂层的制作工艺，其特征在于：所述水性树脂为水性聚氨酯。
  3. 根据权利要求1所述的一种纳米ATO透明隔热节能玻璃涂层的制作工艺，其特征在于：所述介孔二氧化硅粒子介孔率为65-75％，粒径12-15nm。
PCT/CN2016/109160 2016-12-09 2016-12-09 一种纳米ato透明隔热节能玻璃涂层的制作工艺 WO2018103063A1 (zh)

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