CN106977982A - A kind of nano-pore heat insulating materials coating for surface protection and preparation method thereof - Google Patents
A kind of nano-pore heat insulating materials coating for surface protection and preparation method thereof Download PDFInfo
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- CN106977982A CN106977982A CN201710205701.2A CN201710205701A CN106977982A CN 106977982 A CN106977982 A CN 106977982A CN 201710205701 A CN201710205701 A CN 201710205701A CN 106977982 A CN106977982 A CN 106977982A
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- 239000011810 insulating material Substances 0.000 title claims abstract description 21
- 239000011148 porous material Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 4
- 238000000576 coating method Methods 0.000 title claims description 43
- 239000011248 coating agent Substances 0.000 title claims description 40
- 239000007788 liquid Substances 0.000 claims abstract description 42
- 239000002245 particle Substances 0.000 claims abstract description 29
- 239000011253 protective coating Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000010455 vermiculite Substances 0.000 claims abstract description 19
- 229910052902 vermiculite Inorganic materials 0.000 claims abstract description 19
- 235000019354 vermiculite Nutrition 0.000 claims abstract description 19
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000010445 mica Substances 0.000 claims abstract description 18
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 18
- 229910000272 alkali metal oxide Inorganic materials 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 14
- XYRAEZLPSATLHH-UHFFFAOYSA-N trisodium methoxy(trioxido)silane Chemical compound [Na+].[Na+].[Na+].CO[Si]([O-])([O-])[O-] XYRAEZLPSATLHH-UHFFFAOYSA-N 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000011343 solid material Substances 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 18
- 229910021536 Zeolite Inorganic materials 0.000 claims description 13
- 239000010457 zeolite Substances 0.000 claims description 13
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 12
- 239000002270 dispersing agent Substances 0.000 claims description 10
- 239000000395 magnesium oxide Substances 0.000 claims description 10
- 239000011787 zinc oxide Substances 0.000 claims description 9
- BSYNRYMUTXBXSQ-UHFFFAOYSA-N Aspirin Chemical group CC(=O)OC1=CC=CC=C1C(O)=O BSYNRYMUTXBXSQ-UHFFFAOYSA-N 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000004078 waterproofing Methods 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 5
- 239000011159 matrix material Substances 0.000 claims description 3
- 239000004115 Sodium Silicate Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 6
- -1 phosphoric acid aluminum Chemical compound 0.000 claims 6
- 238000000498 ball milling Methods 0.000 claims 4
- 238000009472 formulation Methods 0.000 claims 2
- 230000003647 oxidation Effects 0.000 claims 2
- 238000007254 oxidation reaction Methods 0.000 claims 2
- CAQWNKXTMBFBGI-UHFFFAOYSA-N C.[Na] Chemical compound C.[Na] CAQWNKXTMBFBGI-UHFFFAOYSA-N 0.000 claims 1
- 208000005156 Dehydration Diseases 0.000 claims 1
- 208000021017 Weight Gain Diseases 0.000 claims 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims 1
- 239000004411 aluminium Substances 0.000 claims 1
- 230000037396 body weight Effects 0.000 claims 1
- 230000018044 dehydration Effects 0.000 claims 1
- 238000006297 dehydration reaction Methods 0.000 claims 1
- 238000010422 painting Methods 0.000 claims 1
- 235000019795 sodium metasilicate Nutrition 0.000 claims 1
- 238000009955 starching Methods 0.000 claims 1
- 235000019786 weight gain Nutrition 0.000 claims 1
- 229910052725 zinc Inorganic materials 0.000 claims 1
- 239000011701 zinc Substances 0.000 claims 1
- 239000012774 insulation material Substances 0.000 abstract description 31
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 abstract description 23
- 238000000034 method Methods 0.000 abstract description 22
- 239000000758 substrate Substances 0.000 abstract description 17
- 239000007921 spray Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 18
- 238000009413 insulation Methods 0.000 description 10
- 238000010998 test method Methods 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- 239000010410 layer Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 230000002209 hydrophobic effect Effects 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 5
- 239000004744 fabric Substances 0.000 description 5
- 238000002791 soaking Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 230000001680 brushing effect Effects 0.000 description 4
- 238000005336 cracking Methods 0.000 description 4
- 239000003365 glass fiber Substances 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- 238000004513 sizing Methods 0.000 description 4
- 238000002679 ablation Methods 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000008199 coating composition Substances 0.000 description 3
- 230000003628 erosive effect Effects 0.000 description 3
- 238000009434 installation Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 239000002585 base Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000011162 core material Substances 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 229910021485 fumed silica Inorganic materials 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000002557 mineral fiber Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000005660 hydrophilic surface Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000004848 polyfunctional curative Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
Classifications
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- 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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Paints Or Removers (AREA)
Abstract
本发明公开了一种纳米孔绝热材料表面保护涂层及其制备方法,固体材料的处理:将膨胀蛭石颗粒经高温预处理后与液态磷酸二氢铝混匀、将沸石颗粒按浸没量加入液态磷酸二氢铝,球磨至平均粒径小于4μm;碱金属氧化物加入乙醇、球磨至平均粒径小于4μm,将云母颗粒用水浸没后球磨至平均粒径小于4μm,后经300℃烘烤脱水;上述处理好的固体材料与液态磷酸二氢铝、甲基硅酸钠按比例混合制成浆料,进入高剪切混合机中以1500‑3000 rpm混合30‑100分钟,以喷涂或涂刷方式施加到纳米孔绝热材料基体上以浸渍入孔,干燥后形成防水的保护涂层。本发明无尘、不脱落,可以抵抗相对较高的碰撞冲击,防水、防火且环保。The invention discloses a surface protective coating of a nanoporous heat insulating material and a preparation method thereof. The treatment of the solid material includes: mixing the expanded vermiculite particles with liquid aluminum dihydrogen phosphate after high-temperature pretreatment, and adding the zeolite particles according to the submerged amount Liquid aluminum dihydrogen phosphate, ball milled to an average particle size of less than 4 μm; adding ethanol to alkali metal oxides, ball milled to an average particle size of less than 4 μm, immersing mica particles in water, ball milled to an average particle size of less than 4 μm, and then baked and dehydrated at 300°C ; The above-mentioned processed solid material is mixed with liquid aluminum dihydrogen phosphate and sodium methyl silicate in proportion to make a slurry, enter the high-shear mixer and mix for 30-100 minutes at 1500-3000 rpm to spray or brush The method is applied to the nanoporous insulation material substrate to impregnate into the pores, and forms a waterproof protective coating after drying. The invention is dust-free, does not fall off, can resist relatively high collision impact, is waterproof, fireproof and environmentally friendly.
Description
技术领域technical field
本发明涉及材料技术领域,特别涉及一种纳米孔绝热材料表面保护涂层,同时还涉及该纳米孔绝热材料表面保护涂层的制备方法。The invention relates to the field of material technology, in particular to a protective coating on the surface of a nanoporous heat insulating material, and also relates to a preparation method for the protective coating on the surface of a nanoporous heat insulating material.
背景技术Background technique
纳米孔绝热材料是一种新近发展,主要面向高、低温绝热工程,采用纳米技术制作的新型隔热材料,其纳米孔隙 (小于100nm)的网络结构及其对工业波长的红外辐射和散射特性能够有效抑制固、气态热传导,气体对流和辐射传热。和传统隔热材料相比,纳米孔绝热材料通常可降低隔热层厚度3/4,在相同隔热层厚度下,节能率普遍达到25-30%,不仅可显著降低生产和使用中的能耗,还相应使设备的尺寸和重量得以大幅降低。Nanoporous thermal insulation material is a new development, mainly for high and low temperature thermal insulation projects. It is a new type of thermal insulation material made by nanotechnology. Its network structure of nanopores (less than 100nm) and its infrared radiation and scattering characteristics of industrial wavelengths can Effectively inhibit solid and gaseous heat conduction, gas convection and radiation heat transfer. Compared with traditional heat insulation materials, nanoporous heat insulation materials can usually reduce the thickness of the heat insulation layer by 3/4, and under the same heat insulation layer thickness, the energy saving rate generally reaches 25-30%, which not only can significantly reduce the energy consumption in production and use consumption, and correspondingly, the size and weight of the equipment can be greatly reduced.
近年来,纳米孔绝热材料因其优异的隔热、阻燃性能,在玻璃工业、工业窑炉、电解铝,电热蓄能器、电梯、船舶、军工等需要高效节能和阻燃、防火等领域获得了广泛应用。但该材料为保证其优异的传热学性能,在常规生产中未使用有机或无机粘接剂而主要采用粉压成型工艺,因此其表面不耐磨、不防水、整体强度低,不能碰撞。常规工艺中,一般采用经特殊处理的玻璃纤维布做封套材料进行保护,以便于运输和安装。该工艺采用玻纤布封套和芯体材料一次成型法,适用于对精度要求不高的常规板材的制作。在一些对精度要求较高,且需要曲面、开孔、沟槽、台阶等异型结构件的领域,采用玻璃布封装需要大量的人工裁减和贴合工序,就此增加了生产成本,并使工艺流程较为复杂,难以达到工业化生产的目标。特别是玻璃纤维布的封装方式,仍然存在粉尘泄漏问题,无法满足食品工业设备、医疗健康设备以及军用光学设备的使用条件,因而限制了纳米孔绝热材料的应用领域。In recent years, due to its excellent heat insulation and flame retardant properties, nanoporous thermal insulation materials have been used in glass industry, industrial furnaces, electrolytic aluminum, electric heating accumulators, elevators, ships, military industries, etc. has been widely used. However, in order to ensure its excellent heat transfer performance, the material does not use organic or inorganic adhesives in conventional production, but mainly adopts powder pressing molding process, so its surface is not wear-resistant, not waterproof, and its overall strength is low, so it cannot be collided. In the conventional process, specially treated glass fiber cloth is generally used as the envelope material for protection, so as to facilitate transportation and installation. This process adopts the one-time molding method of glass fiber cloth envelope and core material, which is suitable for the production of conventional plates that do not require high precision. In some areas that require high precision and require special-shaped structural parts such as curved surfaces, openings, grooves, and steps, the use of glass cloth packaging requires a large number of manual cutting and laminating processes, which increases production costs and makes the process flow More complicated, it is difficult to achieve the goal of industrialized production. In particular, the packaging method of glass fiber cloth still has the problem of dust leakage, which cannot meet the conditions of use in food industry equipment, medical and health equipment, and military optical equipment, thus limiting the application fields of nanoporous thermal insulation materials.
为了生产结构稳定且表面无尘的纳米孔绝热材料构件,在其表面制作保护性涂层是最易实现的方法。该涂层应满足结构稳定、成膜均匀、和芯材之间的结合力强,表面无龟裂和粉尘脱落,具备耐高温和抗热震的特性且不影响基材性能。In order to produce structurally stable and dust-free nanoporous insulation components, it is easiest to implement protective coatings on their surfaces. The coating should meet the requirements of stable structure, uniform film formation, strong bonding with the core material, no cracks and dust shedding on the surface, high temperature resistance and thermal shock resistance, and does not affect the performance of the substrate.
经发明人大量实验表明,耐火隔热材料领域常规使用的高温有机和无机涂料均存在涂层龟裂、脱落等现象,难以使用。保护性涂层相关的大量文献报道几乎大多集中于结构强度较高的多孔陶瓷领域,有关针对纳米孔绝热材料的涂层解决方案,美国专利5,474,806公开了一种施加水基保护性涂层到纳米孔绝热材料表面的方法,该方法认为由于常规纳米孔绝热材料的亲水性,施加水基保护性涂层,很容易造成材料表面润湿和吸水,水在干燥过程中会破坏微孔结构,从而导致绝热性能的降低。该专利因此提出用疏水型气相二氧化硅来制造纳米孔绝热材料,采用燃气喷嘴烁烧或在炉体中高温加热来破坏有机疏水层,生成表面亲水,基体疏水的隔热材料,随后用水基硅酸钠粘接剂进行表面处理,这样很容易润湿表层并吸附在那里或形成连续的保护涂层,可实现耐磨并抵抗碰撞而不会造成基体材料的收缩和微孔结构的破坏。该方法的原理虽较为简单,但在生产过程中需要使用昂贵的疏水型气相二氧化硅,且需要增加破坏表面疏水层的高温烧蚀工艺,致使产品的生产成本大幅提高,而且高温烧蚀工艺的温度及处理时间是很难控制的,这决定了烧蚀层的厚度,进而决定了涂层厚度,在工业生产的情况下,材料一般采用堆垛放置,各层之间存在温度梯度,最终涂层的厚度必定厚薄不一,且硅酸盐粘接剂在纳米孔绝热材料通常的高温应用中,因其较高的碱性和脆性并不是合适的粘接剂。此外,疏水型气相氧化物粒子由于有机包覆层的存在,降低了粒子之间的粘接强度,材料的整体强度更低、更不耐磨,这样的保护层很可能是得不偿失的。A large number of experiments by the inventors have shown that the high-temperature organic and inorganic coatings routinely used in the field of fire-resistant and heat-insulating materials all have coating cracks and peeling off, which are difficult to use. A large number of literature reports related to protective coatings are almost mostly concentrated in the field of porous ceramics with high structural strength. Regarding the coating solution for nanoporous insulation materials, US Patent 5,474,806 discloses a water-based protective coating applied to nano The method on the surface of porous thermal insulation materials. This method believes that due to the hydrophilicity of conventional nanoporous thermal insulation materials, applying a water-based protective coating can easily cause the surface of the material to wet and absorb water. Water will destroy the microporous structure during the drying process. This results in a reduction in thermal insulation performance. Therefore, the patent proposes to use hydrophobic fumed silica to manufacture nanoporous thermal insulation materials, use gas nozzles to burn or heat at high temperatures in the furnace to destroy the organic hydrophobic layer, and generate a thermal insulation material with a hydrophilic surface and a hydrophobic matrix, and then water Sodium silicate adhesive for surface treatment, so that it is easy to wet the surface and adsorb there or form a continuous protective coating, which can achieve wear resistance and impact resistance without causing shrinkage of the base material and damage to the microporous structure . Although the principle of this method is relatively simple, expensive hydrophobic fumed silica needs to be used in the production process, and a high-temperature ablation process that destroys the surface hydrophobic layer needs to be added, resulting in a significant increase in the production cost of the product, and the high-temperature ablation process The temperature and processing time are difficult to control, which determines the thickness of the ablation layer, and then determines the thickness of the coating. In the case of industrial production, the materials are generally placed in stacks, and there is a temperature gradient between the layers. Finally, The thickness of the coating must vary, and the silicate adhesive is not a suitable adhesive for the high-temperature application of nanoporous insulation materials due to its high alkalinity and brittleness. In addition, due to the presence of the organic coating layer on the hydrophobic fumed oxide particles, the bonding strength between the particles is reduced, the overall strength of the material is lower, and it is less wear-resistant. Such a protective layer is probably not worth the candle.
发明内容Contents of the invention
本发明的目的在于克服上述缺点而提供的一种无尘、不脱落,可以抵抗相对较高的碰撞冲击,防水、防火且环保的纳米孔绝热材料表面保护涂层。The object of the present invention is to overcome the above disadvantages and provide a dust-free, non-shedding, relatively high impact resistance, waterproof, fireproof and environmentally friendly nanoporous heat insulating material surface protective coating.
本发明的另一目的在于提供该纳米孔绝热材料表面保护涂层的制备方法。Another object of the present invention is to provide a method for preparing the protective coating on the surface of the nanoporous heat insulating material.
本发明的一种纳米孔绝热材料表面保护涂层,其配方重量份如下:A surface protection coating of a nanoporous heat insulating material of the present invention has the following formula in parts by weight:
液态磷酸二氢铝 45-75Liquid Aluminum Dihydrogen Phosphate 45-75
膨胀蛭石 10 -30Expanded vermiculite 10 -30
沸石 3 -6Zeolite 3 -6
云母 8 -12Mica 8 -12
有机硅防水剂(甲基硅酸钠) 1.9 -7Silicone water repellent (sodium methyl silicate) 1.9 -7
碱金属氧化物(氧化锌、氧化镁) 1.5-3Alkali metal oxides (zinc oxide, magnesium oxide) 1.5-3
分散剂(Duramax D-3005) 0.1-0.5Dispersant (Duramax D-3005) 0.1-0.5
优选各成分的重量份如下:Preferably the parts by weight of each component are as follows:
液态磷酸二氢铝 60Liquid Aluminum Dihydrogen Phosphate 60
膨胀蛭石 15Expanded vermiculite 15
沸石 6Zeolite 6
云母 12Mica 12
碱金属氧化物 3Alkali metal oxides 3
有机硅防水剂(甲基硅酸钠) 3.7Silicone waterproofing agent (sodium methyl silicate) 3.7
分散剂(Duramax D-3005) 0.3Dispersant (Duramax D-3005) 0.3
本发明的一种纳米孔绝热材料的表面保护涂层的制备方法,包括以下步骤:A method for preparing a surface protective coating of a nanoporous heat insulating material of the present invention, comprising the following steps:
(1) 固体材料的处理:(1) Handling of solid materials:
a.将膨胀蛭石颗粒经高温预处理后,取2-5份与1份液态磷酸二氢铝混匀,再采用氧化铝球的球磨机中球磨24-48小时至平均粒径小于4μm(以便于渗透进入纳米孔绝热材料的表面孔隙,避免仅附着于表面而容易脱落);a. After the expanded vermiculite particles are pretreated at high temperature, take 2-5 parts and mix them with 1 part of liquid aluminum dihydrogen phosphate, and then use alumina balls in a ball mill for 24-48 hours until the average particle size is less than 4 μm (so that In order to penetrate into the surface pores of nanoporous insulation materials, to avoid only adhering to the surface and easy to fall off);
b.将沸石颗粒按浸没量(固体颗粒完全吸附液体后保持液体浸没)加入液态磷酸二氢铝,采用氧化铝球的球磨机中球磨24-48小时至平均粒径小于4μm;b. Add the zeolite particles into the liquid aluminum dihydrogen phosphate according to the immersion amount (the solid particles completely absorb the liquid and keep the liquid submerged), and use alumina balls in a ball mill for 24-48 hours until the average particle size is less than 4 μm;
c.碱金属氧化物加入乙醇,采用氧化铝球的球磨机中球磨24-48小时至平均粒径小于4μm;c. Alkali metal oxides are added with ethanol, and ball milled in a ball mill with alumina balls for 24-48 hours until the average particle size is less than 4 μm;
d.将云母颗粒用水浸没后,采用氧化铝球的球磨机中球磨24-48小时至平均粒径小于4μm,后经300℃烘烤脱水;d. After immersing the mica particles in water, mill them in a ball mill with alumina balls for 24-48 hours until the average particle size is less than 4 μm, and then bake and dehydrate at 300°C;
(2)上述处理好的固体材料与液态磷酸二氢铝、甲基硅酸钠按下述比例混合制成浆料,(2) The above-mentioned treated solid material is mixed with liquid aluminum dihydrogen phosphate and sodium methyl silicate according to the following ratio to make a slurry,
液态磷酸二氢铝 45-75Liquid Aluminum Dihydrogen Phosphate 45-75
膨胀蛭石 10 -30Expanded vermiculite 10 -30
沸石 3 -6Zeolite 3 -6
云母 8 -12Mica 8 -12
有机硅防水剂(甲基硅酸钠) 1.9-7Silicone waterproofing agent (sodium methyl silicate) 1.9-7
碱金属氧化物(氧化锌、氧化镁) 1.5-3Alkali metal oxides (zinc oxide, magnesium oxide) 1.5-3
分散剂(Duramax D-3005) 0.1-0.5Dispersant (Duramax D-3005) 0.1-0.5
进入高剪切混合机中以1500-3000 rpm混合30-100分钟,以喷涂或涂刷方式施加到纳米孔绝热材料基体上以浸渍入孔;Enter the high-shear mixer and mix at 1500-3000 rpm for 30-100 minutes, and apply it to the nanoporous insulation material substrate by spraying or brushing to impregnate the pores;
(3)在常温下干燥30分钟,再进入炉内在80-120℃下进行3-8分钟快速干燥(因基材高含气量,长时间加温会引起表层涂料鼓包、脱层或开裂,温度过低磷酸盐不能脱水固化)上浆数量为干燥后,绝热体增重1.8-3.0克/cm2,形成0.3-0.5mm的耐磨、耐高温(同基材同温)防水的保护涂层。(3) Dry at room temperature for 30 minutes, and then enter the furnace for 3-8 minutes of rapid drying at 80-120°C (due to the high gas content of the substrate, heating for a long time will cause the surface coating to bulge, delaminate or crack, and the temperature Too low phosphate cannot be dehydrated and solidified) The amount of sizing is 1.8-3.0 g/cm 2 after drying, forming a 0.3-0.5mm wear-resistant, high-temperature-resistant (same temperature as the base material) waterproof protective coating.
涂层性能测试:Coating performance test:
由于纳米孔绝热材料基材的结构强度极低,按上述方法制成的保护性涂层无法类比在金属、陶瓷、混凝土等刚性基材上形成的涂层,涂层和基材的结合强度的测定不能采用常规的,如:弯曲、基片拉伸、锉磨、磨损等实验方法。实际上在纳米孔绝热材料基材上生成保护性涂层的主要目的是方便运输、安装等人工操作同时在保持基材绝热性能的同时实现防潮和抗热震性,因此该保护性涂层无需达到那些刚性基材涂层的要求,其耐磨、抗碰撞冲击的性能采用定性法以经验判断和相对比较来表述较为适用。Due to the extremely low structural strength of the nanoporous thermal insulation material substrate, the protective coating made by the above method cannot be compared to the coating formed on rigid substrates such as metals, ceramics, concrete, etc., and the bonding strength between the coating and the substrate is limited. Determination can not adopt conventional methods, such as: bending, substrate stretching, filing, abrasion and other experimental methods. In fact, the main purpose of forming a protective coating on the nanoporous thermal insulation material substrate is to facilitate manual operations such as transportation and installation while maintaining the thermal insulation performance of the substrate while achieving moisture resistance and thermal shock resistance, so the protective coating does not need To meet the requirements of those coatings on rigid substrates, it is more suitable to use qualitative methods to express their wear resistance and impact resistance performance by empirical judgment and relative comparison.
1)耐磨、抗碰撞冲击性:常规纳米孔绝热材料如果未采用保护性玻璃纤维布封套,轻拿轻放或堆垛放置都会造成表面粉体脱落,特别是异型构件的棱、边、倒角,孔等极易在运输和安装过程中被破坏,更不耐碰撞冲击。实验中采用110*110*20的试块,无涂层材料5cm高的跌落即可造成断裂,而采用按本发明制成的保护性涂层的同样试块,跌落断裂高度提高至45cm,且安装操作方便、堆垛不掉粉,外观成膜均匀,无龟裂。1) Wear resistance, impact resistance: If the conventional nanoporous thermal insulation material is not covered with protective glass fiber cloth, it will cause the surface powder to fall off if it is handled with care or stacked, especially the edges, edges, and inversions of special-shaped components. Corners, holes, etc. are easily damaged during transportation and installation, and are not resistant to collisions and impacts. Adopt the test piece of 110*110*20 in the experiment, uncoated material 5cm high drop can cause fracture, and adopt the same test piece of protective coating made by the present invention, drop fracture height to improve to 45cm, and It is easy to install and operate, no powder will fall off when stacked, and the appearance of the film is uniform without cracks.
2)耐温性:按astmC356 Test Method for Linear Shrinkage ofPreformedHigh-Temperature Thermal Insulation Subjected to SoakingHeat(预成型高温绝热材料置于均热下的线收缩测试方法)-相关国标:GBT 5486-2008 无机硬质绝热制品试验方法:采用按本发明制成的保护性涂层的同样试块整体展现了满意的耐温性和抗热震性(在24小时,均热900度的实验中观察到没有起泡、碎裂或剥蚀。长宽方向收缩1.7%,厚度方向收缩5.5%,满足astmC1676的要求。2) Temperature resistance: according to astmC356 Test Method for Linear Shrinkage of Preformed High-Temperature Thermal Insulation Subjected to SoakingHeat (preformed high-temperature thermal insulation material under soaking linear shrinkage test method) - related national standard: GBT 5486-2008 Inorganic rigid thermal insulation Product test method: adopt the same test block integral body that adopts the protective coating made by the present invention to show satisfactory temperature resistance and thermal shock resistance (in 24 hours, observe in the experiment of soaking 900 degrees without foaming, Fragmentation or denudation. The shrinkage in the length and width direction is 1.7%, and the thickness direction shrinks by 5.5%, which meets the requirements of astmC1676.
3)吸水性:按astmC1104/C 1104M Test Method for Determining theWaterVapor Sorption of Unfaced Mineral Fiber Insulation(确定未贴面矿物纤维水蒸气吸附的测试方法)-相关国标:GBT 10299-1988 保温材料憎水性试验方法,采用按本发明制成的保护性涂层的同样试块,蒸气吸附重量百分比为6.1%,而常规材料蒸气吸附重量百分比为9.4%3) Water absorption: according to astmC1104/C 1104M Test Method for Determining the WaterVapor Sorption of Unfaced Mineral Fiber Insulation (test method for determining the water vapor adsorption of unfaced mineral fiber) - related national standard: GBT 10299-1988 Test method for hydrophobicity of thermal insulation materials, The same test piece with the protective coating made in accordance with the present invention had a vapor sorption of 6.1% by weight compared to 9.4% by weight of the conventional material.
4)导热系数:按astmC1676的测试方法,采用本发明涂层的纳米孔绝热材料,平均温度100℃时,导热系数为0.021w/m.k,平均温度500℃时,导热系数为0.0275w/m.k,常规纳米孔绝热材料相应的导热系数,平均温度100℃时,导热系数为0.020w/m.k,平均温度500℃时,导热系数为0.0270w/m.k,几乎没有变化,证明本发明的涂层并未破坏基材结构。4) Thermal conductivity: According to the test method of astmC1676, the nanoporous thermal insulation material coated with the present invention has a thermal conductivity of 0.021w/m.k when the average temperature is 100°C, and a thermal conductivity of 0.0275w/m.k when the average temperature is 500°C. The corresponding thermal conductivity of conventional nanoporous insulation materials, when the average temperature is 100°C, the thermal conductivity is 0.020w/m.k, and when the average temperature is 500°C, the thermal conductivity is 0.0270w/m.k, almost no change, which proves that the coating of the present invention does not destroy the substrate structure.
本发明同现有技术相比具有明显的优点和有益效果。由以上技术方案可知,本发明经前期大量实验和研究证明,纳米孔绝热材料表面难以生成稳定保护涂层的主要原因是除了其表面强度较低之外,内部纳米孔隙结构中富含大量的空气(含气量体积占比甚至达到90%),在环境温度发生变化时,由于气体体积的变化,同外界之间会产生不同程度的气体交换,加之涂层结构和基体的热胀冷缩会造成材料表面的微变形,而传统涂料大多是不透气材料,涂敷在纳米孔绝热材料表面会因此出现龟裂和脱落现象。为避免此现象,构成涂层的骨架材料应具有热膨胀性和透气性,即涂层骨架材料应具有作为温度的函数而发生膨胀或收缩的特性,此外当涂层结构出现微细三维变化时,也应具有保证涂层稳定的层理结构。这样的保护性涂料,即使是水基的,只要涂层较薄,所吸附水份在干燥过程中也不会破坏微孔结构。因此本发明的涂层配方,以45wt%-75wt%(45-75重量份)液态磷酸二氢铝作粘接剂,10 wt %-35wt %(10-35重量份)膨胀蛭石和3wt %-10wt %(3-10重量份)的沸石作为涂层骨料,8 wt %-18 wt %(8-18重量份)云母颗粒作为涂层稳定材料,1.5 wt %-7wt %(1.5-7重量份)碱金属氧化物作为硬化剂并加入2wt %-7wt %(2-7重量份)有机硅作为防水剂构成完整的涂料配方。其中以磷酸二氢铝作为粘接剂可实现低温高强度粘接,且和各种无机高温材料的相容性较强,特别是它可和纳米孔绝热材料表层的二氧化硅产生针型晶体,提高了粘接性,其可耐1700℃高温,覆盖了纳米孔绝热材料的温度使用范围;涂层骨架材料采用膨胀蛭石和沸石,可充分利用蛭石的膨胀性和透气性抵御环境温度的变化,且沸石具有稳定的空心结构和微米级超细孔隙,和膨胀蛭石配合,在涂层固化过程中可保证孔隙内外形成一体化结构,加强了固化强度;涂料辅料采用云母可利用其片状层理结构,加入涂料中可作为涂层的稳定剂,当涂层结构出现微细三维变化时,云母可助其变化防止龟裂等微结构破坏;加入碱金属氧化物如氧化锌和氧化镁等可加速涂层硬化;有机硅(甲基硅酸钠)易溶于水,能和本发明的其它涂料配方较好的溶合,可在纳米孔绝热材料基材表层形成一层网状防水透气膜,具有较好的防水效果和防渗、防潮优点,避免了水分吸入基底。本发明涂层无尘、不脱落,可以抵抗相对较高的碰撞冲击,且防水、防火,不会在使用过程中释放有毒气体和烟雾。Compared with the prior art, the present invention has obvious advantages and beneficial effects. From the above technical solutions, it can be seen that a large number of experiments and researches in the early stage of the present invention have proved that the main reason why it is difficult to form a stable protective coating on the surface of the nanoporous thermal insulation material is that in addition to its low surface strength, the internal nanoporous structure is rich in a large amount of air. (The volume ratio of the gas content even reaches 90%). When the ambient temperature changes, due to the change of the gas volume, there will be different degrees of gas exchange with the outside world, and the thermal expansion and contraction of the coating structure and the substrate will cause Micro-deformation on the surface of the material, while traditional coatings are mostly air-tight materials, coating on the surface of nanoporous thermal insulation materials will cause cracks and peeling off. In order to avoid this phenomenon, the skeleton material constituting the coating should have thermal expansion and gas permeability, that is, the coating skeleton material should have the characteristics of expanding or shrinking as a function of temperature. It should have a bedding structure to ensure the stability of the coating. Such a protective coating, even if it is water-based, as long as the coating is thin, the absorbed moisture will not damage the microporous structure during the drying process. Therefore, the coating formulation of the present invention uses 45wt%-75wt% (45-75 parts by weight) of liquid aluminum dihydrogen phosphate as a binder, 10wt%-35wt% (10-35 parts by weight) of expanded vermiculite and 3wt%- 10wt% (3-10 parts by weight) of zeolite as coating aggregate, 8 wt%-18 wt% (8-18 parts by weight) of mica particles as coating stabilization material, 1.5 wt%-7wt% (1.5-7 wt. parts) alkali metal oxides as a hardener and 2wt%-7wt% (2-7 parts by weight) of silicone as a waterproofing agent to form a complete coating formulation. Among them, aluminum dihydrogen phosphate is used as the adhesive to achieve low-temperature and high-strength bonding, and it has strong compatibility with various inorganic high-temperature materials, especially it can produce needle-shaped crystals with silicon dioxide on the surface of nanoporous heat-insulating materials. , improve the adhesion, it can withstand high temperature of 1700 ℃, covering the temperature range of nanoporous insulation materials; the coating skeleton material uses expanded vermiculite and zeolite, which can make full use of the expansion and gas permeability of vermiculite to resist the impact of ambient temperature The zeolite has a stable hollow structure and micron-scale ultra-fine pores, and when combined with expanded vermiculite, it can ensure the formation of an integrated structure inside and outside the pores during the coating curing process, and strengthen the curing strength; the coating auxiliary material uses mica to utilize its flakes When added into the coating, it can be used as a stabilizer for the coating. When the coating structure undergoes fine three-dimensional changes, mica can help it change and prevent microstructural damage such as cracking; adding alkali metal oxides such as zinc oxide and magnesium oxide etc. can accelerate the hardening of the coating; organic silicon (sodium methyl silicate) is easily soluble in water, and can be well blended with other coating formulations of the present invention, and can form a layer of mesh waterproof on the surface of the nanoporous heat insulating material substrate The breathable membrane has good waterproof effect, anti-seepage and moisture-proof advantages, and avoids moisture absorption into the substrate. The coating of the invention is dust-free, does not fall off, can resist relatively high collision impact, is waterproof and fireproof, and will not release toxic gas and smoke during use.
具体实施方式detailed description
实施例1Example 1
一种纳米孔绝热材料的表面保护涂层的制备方法,包括以下步骤:A method for preparing a surface protective coating of a nanoporous heat insulating material, comprising the following steps:
(1)固体材料的处理:(1) Handling of solid materials:
a.将800℃高温预处理1小时后的膨胀蛭石颗粒以4:1的比例和液态磷酸二氢铝混匀,然后在球磨机中球磨48小时后备用;a. Mix the expanded vermiculite particles after high temperature pretreatment at 800°C for 1 hour with liquid aluminum dihydrogen phosphate at a ratio of 4:1, and then ball mill in a ball mill for 48 hours before use;
b.将沸石颗粒按浸没量(固体颗粒完全吸附液体后保持液体浸没)加入液态磷酸二氢铝,随后在球磨机中球磨48小时后备用;b. Add the zeolite particles into the liquid aluminum dihydrogen phosphate according to the immersion amount (the solid particles completely absorb the liquid and keep the liquid submerged), and then ball mill in the ball mill for 48 hours before use;
c.碱金属氧化物(氧化锌、氧化镁按3:1比例)加入乙醇(固体颗粒完全吸附液体后保持液体浸没),在球磨机中球磨48小时备用;c. Alkali metal oxides (zinc oxide, magnesium oxide at a ratio of 3:1) are added to ethanol (the solid particles are completely absorbed by the liquid and kept submerged in the liquid), and ball milled in a ball mill for 48 hours for later use;
d.将云母颗粒用水浸没后,在球磨机中球磨48小时,后经300℃烘烤1小时脱水后备用;d. After immersing the mica particles in water, mill them in a ball mill for 48 hours, then bake them at 300°C for 1 hour and dehydrate them for later use;
(2)上述处理好的固体材料与液态磷酸二氢铝、甲基硅酸钠按下述比例(2) The above-mentioned treated solid material and liquid aluminum dihydrogen phosphate and sodium methyl silicate are in the following ratio
液态磷酸二氢铝 60Liquid Aluminum Dihydrogen Phosphate 60
膨胀蛭石 15Expanded vermiculite 15
沸石 6Zeolite 6
云母 12Mica 12
氧化锌 3Zinc oxide 3
甲基硅酸钠 3.7Sodium methyl silicate 3.7
分散剂(Duramax D-3005购自Rohm and Haas, France) 0.3Dispersant (Duramax D-3005 purchased from Rohm and Haas, France) 0.3
混合制成浆料,进入高剪切混合机中以3000 rpm混合75分钟,以喷涂或涂刷方式施加到纳米孔绝热材料基体;Mix to make a slurry, enter a high-shear mixer and mix for 75 minutes at 3000 rpm, and apply it to the nanoporous thermal insulation material matrix by spraying or brushing;
(3)在常温下干燥30分钟,再进入炉内在80-120℃下进行5分钟快速干燥,上浆数量为干燥后,绝热体增重2.3克/cm2,形成约0.4mm的保护涂层。(3) Dry at room temperature for 30 minutes, and then enter the oven for 5 minutes at 80-120°C for 5 minutes of rapid drying. The amount of sizing is 2.3 g/cm 2 after drying, and a protective coating of about 0.4 mm is formed.
涂层性能测试:Coating performance test:
1)耐磨、抗碰撞冲击性:涂层外观成膜均匀、无龟裂和脱落,采用110*110*20的试块,跌落断裂高度为45cm。1) Abrasion resistance, impact resistance: The appearance of the coating is uniform, without cracks and shedding. The test block of 110*110*20 is used, and the drop fracture height is 45cm.
2)耐温性:按astmC356 标准进行测试,在24小时,均热900度的实验中观察到没有起泡、碎裂或剥蚀。长宽方向收缩1.7%,厚度方向收缩5.5%,满足astmC1676的要求。2) Temperature resistance: Tested according to the astmC356 standard, no blistering, cracking or erosion was observed in the 24-hour, 900-degree soaking experiment. The shrinkage in the length and width direction is 1.7%, and the shrinkage in the thickness direction is 5.5%, which meets the requirements of astmC1676.
3)吸水性:按astmC1104/C 1104M标准进行测试,蒸气吸附重量百分比为6.1%。3) Water absorption: Tested according to astmC1104/C 1104M standard, the weight percentage of vapor adsorption is 6.1%.
4)导热系数:按astmC1676的测试方法,采用本发明涂层的纳米孔绝热材料,平均温度100℃时,导热系数为0.021w/m.k,平均温度500℃时,导热系数为0.0275w/m.k。4) Thermal conductivity: According to the test method of astmC1676, the nanoporous thermal insulation material coated with the present invention has a thermal conductivity of 0.021w/m.k when the average temperature is 100°C, and a thermal conductivity of 0.0275w/m.k when the average temperature is 500°C.
实施例2Example 2
一种纳米孔绝热材料的表面保护涂层的制备方法,包括以下步骤:A method for preparing a surface protective coating of a nanoporous heat insulating material, comprising the following steps:
(1)固体材料的处理:(1) Handling of solid materials:
a.将800℃高温预处理1小时后的膨胀蛭石颗粒以4:1的比例和液态磷酸二氢铝混匀,然后在球磨机中球磨48小时后备用;a. Mix the expanded vermiculite particles after high temperature pretreatment at 800°C for 1 hour with liquid aluminum dihydrogen phosphate at a ratio of 4:1, and then ball mill in a ball mill for 48 hours before use;
b.将沸石颗粒按浸没量(固体颗粒完全吸附液体后保持液体浸没)加入液态磷酸二氢铝,随后在球磨机中球磨48小时后备用;b. Add the zeolite particles into the liquid aluminum dihydrogen phosphate according to the immersion amount (the solid particles completely absorb the liquid and keep the liquid submerged), and then ball mill in the ball mill for 48 hours before use;
c.碱金属氧化物(氧化锌、氧化镁按3:1比例)加入乙醇(固体颗粒完全吸附液体后保持液体浸没),在球磨机中球磨48小时备用;c. Alkali metal oxides (zinc oxide, magnesium oxide at a ratio of 3:1) are added to ethanol (the solid particles are completely absorbed by the liquid and kept submerged in the liquid), and ball milled in a ball mill for 48 hours for later use;
d.将云母颗粒用水浸没后,在球磨机中球磨48小时,后经300℃烘烤1小时脱水后备用;d. After immersing the mica particles in water, mill them in a ball mill for 48 hours, then bake them at 300°C for 1 hour and dehydrate them for later use;
(2)上述处理好的固体材料与液态磷酸二氢铝、甲基硅酸钠按下述比例(2) The above-mentioned treated solid material and liquid aluminum dihydrogen phosphate and sodium methyl silicate are in the following ratio
液态磷酸二氢铝 75Liquid Aluminum Dihydrogen Phosphate 75
膨胀蛭石 10Expanded vermiculite 10
沸石 3Zeolite 3
云母 8Mica 8
氧化镁 2Magnesium oxide 2
甲基硅酸钠 1.9Sodium methyl silicate 1.9
分散剂(Duramax D-3005) 0.1Dispersant (Duramax D-3005) 0.1
混合制成浆料,进入高剪切混合机中以3000 rpm混合75分钟,以喷涂或涂刷方式施加到纳米孔绝热材料基体上以浸渍入孔;Mix to form a slurry, enter a high-shear mixer and mix for 75 minutes at 3000 rpm, and apply it to the nanoporous insulation material substrate by spraying or brushing to impregnate the pores;
(3)在常温下干燥30分钟,再进入炉内在80-120℃下进行8分钟快速干燥,上浆数量为干燥后,绝热体增重1.8克/cm2,形成约0.3mm的保护涂层。(3) Dry at room temperature for 30 minutes, then enter the furnace for 8 minutes at 80-120°C for 8 minutes of rapid drying, the amount of sizing is after drying, the weight of the insulator is 1.8 g/cm 2 , and a protective coating of about 0.3 mm is formed.
涂层性能测试:Coating performance test:
1)耐磨、抗碰撞冲击性:涂层外观成膜均匀,无龟裂,无脱落,采用110*110*20的试块,跌落断裂高度为37cm。1) Abrasion resistance, impact resistance: The appearance of the coating is uniform, without cracks, and without falling off. The test block of 110*110*20 is used, and the drop fracture height is 37cm.
2)耐温性:按astmC356 标准进行测试,在24小时,均热900度的实验中观察到没有起泡、碎裂或剥蚀。长宽方向收缩1.5%,厚度方向收缩5.7%,满足astmC1676的要求。2) Temperature resistance: Tested according to the astmC356 standard, no blistering, cracking or erosion was observed in the 24-hour, 900-degree soaking experiment. The shrinkage in the length and width direction is 1.5%, and the shrinkage in the thickness direction is 5.7%, which meets the requirements of astmC1676.
3)吸水性:按astmC1104/C 1104M标准进行测试,蒸气吸附重量百分比为7.3%。3) Water absorption: Tested according to astmC1104/C 1104M standard, the vapor adsorption weight percentage is 7.3%.
4)导热系数:按astmC1676的测试方法,采用本发明涂层的纳米孔绝热材料,平均温度100℃时,导热系数为0.020w/m.k,平均温度500℃时,导热系数为0.0251w/m.k。4) Thermal conductivity: According to the test method of astmC1676, the nanoporous thermal insulation material coated with the present invention has a thermal conductivity of 0.020w/m.k when the average temperature is 100°C, and a thermal conductivity of 0.0251w/m.k when the average temperature is 500°C.
实施例3Example 3
一种纳米孔绝热材料的表面保护涂层的制备方法,包括以下步骤:A method for preparing a surface protective coating of a nanoporous heat insulating material, comprising the following steps:
(1)固体材料的处理:(1) Handling of solid materials:
a.将800℃高温预处理1小时后的膨胀蛭石颗粒以4:1的比例和液态磷酸二氢铝混匀,然后在球磨机中球磨48小时后备用;a. Mix the expanded vermiculite particles after high temperature pretreatment at 800°C for 1 hour with liquid aluminum dihydrogen phosphate at a ratio of 4:1, and then ball mill in a ball mill for 48 hours before use;
b.将沸石颗粒按浸没量(固体颗粒完全吸附液体后保持液体浸没)加入液态磷酸二氢铝,随后在球磨机中球磨48小时后备用;b. Add the zeolite particles into the liquid aluminum dihydrogen phosphate according to the immersion amount (the solid particles completely absorb the liquid and keep the liquid submerged), and then ball mill in the ball mill for 48 hours before use;
c.碱金属氧化物(氧化锌、氧化镁按3:1比例)加入乙醇(固体颗粒完全吸附液体后保持液体浸没),在球磨机中球磨48小时备用;c. Alkali metal oxides (zinc oxide, magnesium oxide at a ratio of 3:1) are added to ethanol (the solid particles are completely absorbed by the liquid and kept submerged in the liquid), and ball milled in a ball mill for 48 hours for later use;
d.将云母颗粒用水浸没后,在球磨机中球磨48小时,后经300℃烘烤1小时脱水后备用;d. After immersing the mica particles in water, mill them in a ball mill for 48 hours, then bake them at 300°C for 1 hour and dehydrate them for later use;
(2)上述处理好的固体材料与液态磷酸二氢铝、甲基硅酸钠按下述比例(2) The above-mentioned treated solid material and liquid aluminum dihydrogen phosphate and sodium methyl silicate are in the following ratio
液态磷酸二氢铝 45Liquid Aluminum Dihydrogen Phosphate 45
膨胀蛭石 30Expanded vermiculite 30
沸石 5Zeolite 5
云母 11Mica 11
氧化锌或氧化镁 1.5Zinc oxide or magnesium oxide 1.5
甲基硅酸钠 7Sodium methyl silicate 7
分散剂(Duramax D-3005) 0.5Dispersant (Duramax D-3005) 0.5
混合制成浆料,进入高剪切混合机中以3000 rpm混合75分钟,以喷涂或涂刷方式施加到纳米孔绝热材料基体上以浸渍入孔;Mix to form a slurry, enter a high-shear mixer and mix for 75 minutes at 3000 rpm, and apply it to the nanoporous insulation material substrate by spraying or brushing to impregnate the pores;
(3)在常温下干燥30分钟,再进入炉内在80-120℃下进行3分钟快速干燥,上浆数量为干燥后,绝热体增重2.7克/cm2,形成约0.4mm的保护涂层。(3) Dry at room temperature for 30 minutes, then enter the oven for 3 minutes at 80-120°C for 3 minutes of rapid drying, the amount of sizing is 2.7 g/cm 2 after drying, and a protective coating of about 0.4 mm is formed.
涂层性能测试:Coating performance test:
1)耐磨、抗碰撞冲击性:涂层外观成膜基本均匀,有稍许裂纹,但无脱落,采用110*110*20的试块,跌落断裂高度为49cm。1) Wear resistance, impact resistance: The appearance of the coating is basically uniform, with a few cracks, but no shedding. A 110*110*20 test block is used, and the drop fracture height is 49cm.
2)耐温性:按astmC356 标准进行测试,在24小时,均热900度的实验中观察到没有起泡、碎裂或剥蚀。长宽方向收缩1.9%,厚度方向收缩7.5%,满足astmC1676的要求。2) Temperature resistance: Tested according to the astmC356 standard, no blistering, cracking or erosion was observed in the 24-hour, 900-degree soaking experiment. The shrinkage in the length and width direction is 1.9%, and the shrinkage in the thickness direction is 7.5%, which meets the requirements of astmC1676.
3)吸水性:按astmC1104/C 1104M标准进行测试,蒸气吸附重量百分比为4.7%。3) Water absorption: Tested according to astmC1104/C 1104M standard, the vapor adsorption weight percentage is 4.7%.
4)导热系数:按astmC1676的测试方法,采用本发明涂层的纳米孔绝热材料,平均温度100℃时,导热系数为0.0218w/m.k,平均温度500℃时,导热系数为0.0278w/m.k。4) Thermal conductivity: According to the test method of astmC1676, the nanoporous thermal insulation material coated with the present invention has a thermal conductivity of 0.0218w/m.k when the average temperature is 100°C, and a thermal conductivity of 0.0278w/m.k when the average temperature is 500°C.
以上所述,仅是本发明的较佳实施例而已,并非对本发明作任何形式上的限制,任何未脱离本发明技术方案内容,依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均仍属于本发明技术方案的范围内。The above is only a preferred embodiment of the present invention, and does not limit the present invention in any form. Any simple modification, Equivalent changes and modifications still fall within the scope of the technical solution of the present invention.
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| CN106316439A (en) * | 2015-06-15 | 2017-01-11 | 上海赐业新能源材料科技有限公司 | Method for preparing high strength waterproof nano micropore insulation board |
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| US5474806A (en) * | 1992-02-07 | 1995-12-12 | Zortech International Limited | Coating surface of hydrophobic microporous thermal insulation material |
| WO2000044036A1 (en) * | 1999-01-26 | 2000-07-27 | Alliedsignal Inc. | Use of multifunctional si-based oligomer/polymer for the surface modification of nanoporous silica films |
| CN103589258A (en) * | 2013-10-16 | 2014-02-19 | 纳诺科技有限公司 | Aerogel coating and production method and application thereof |
| CN104761974A (en) * | 2015-03-18 | 2015-07-08 | 蚌埠市高华电子有限公司 | Radiation heat-insulating coating having anti-cracking and peeling-resistant functions and preparation method thereof |
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