CN104944887A - Preparation method of rigid silicon dioxide aerogel insulating board - Google Patents

Preparation method of rigid silicon dioxide aerogel insulating board Download PDF

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Publication number
CN104944887A
CN104944887A CN201510376341.3A CN201510376341A CN104944887A CN 104944887 A CN104944887 A CN 104944887A CN 201510376341 A CN201510376341 A CN 201510376341A CN 104944887 A CN104944887 A CN 104944887A
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China
Prior art keywords
gel
silicon dioxide
dioxide aerogel
rigid silicon
sulfuric acid
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CN201510376341.3A
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Chinese (zh)
Inventor
陈庚
杨卓舒
刘国强
冯强
刘建波
邝清林
车君超
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卓达新材料科技集团有限公司
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Priority to CN201510376341.3A priority Critical patent/CN104944887A/en
Publication of CN104944887A publication Critical patent/CN104944887A/en

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Abstract

The invention provides a preparation method of a high-strength low-carbon environment-friendly rigid silicon dioxide aerogel insulating board, which comprises the following steps: (1) taking 68-120g of sodium water glass with the modulus of 3.1-3.6, adding 100-200g of pure water, and stirring uniformly to obtain diluted water glass; (2) weighing 25-100g of 40 wt% sulfuric acid, adding 10-40g of ethanol, and stirring uniformly to obtain a sulfuric acid solution; (3) mixing the diluted water glass and sulfuric acid solution, and regulating the pH value to 3.5-4.5 to obtain a sol; (4) pouring the sol into a reinforcing-fiber-filled mold, gelatinating the sol after 10-15 minutes, and standing for 2-10 hours while keeping at the temperature of 50-80 DEG C, thereby obtaining a gel board; (5) carrying out integrated aging and acid alcohol treatment on the alcoholic aquagel board; (6) putting the gel board subjected to acid alcohol treatment into 1000-250ml of trimethylethoxy silane, treating at room temperature, and completing hydrophobic modification and gel drainage in one step within 6-10 hours; and (7) after the drainage is finished, drying the wet gel board with hot nitrogen or carbon dioxide.

Description

The preparation method of rigid silicon dioxide aerogel heat-insulating plate
Technical field
The present invention relates to a kind of preparation method of aerogel heat-insulating plate, especially a kind of preparation method of rigid silicon dioxide aerogel heat-insulating plate.
Background technology
Building thermal insulation material huge number, can be divided into organic and inorganic two large classes.Organic materials mainly contains molded polystyrene foams plastics (EPS), extruded polystyrene foam (XPS), Ju ammonia ester Ying Zhi foam and phenolic-aldehyde heat-insulation board.Organic materials is cheap, and heat insulation effect is better, but material fire-protection rating is low, and as EPS plate belongs to inflammable material, most material can produce thick smoke when fire.Inorganic heat insulation material mainly contains rock wool, foamed concrete, pearlstone and empty glass bead.Inorganic heat insulation material unit weight is large, and heat insulation effect is poor; But fire protection flame retarding, anti-aging, stable performance.Aerosil super insulating material is the revolutionary substitute products of conventional insulation material, compared with traditional material, and energy-conservation about 30%, and there is following remarkable advantage:
(1) ultra-low thermal conductivity, superthermal insulation performance, promotes energy-saving effect;
(2) extremely strong resistance of aging, work-ing life is 8 ~ 10 times of conventional material;
(3) the use thickness of aerosil is common material 1/2 ~ 1/5, saves space;
(4) more easy construction process, and save subsidiary material in a large number;
(5) less maintenance cost, more reliable insulation effect;
(6) fire protection flame retarding, wide temperature use range, the resistance to temperature difference is impacted;
(7) waterproof, impervious, cracking resistance, antidetonation;
(8) environmental protection, protection of the environment and HUMAN HEALTH.
But aerogel insulating material main products is aerogel heat-insulating felt in the market, and felt body is softer, be not suitable for receiving use in building.
Aerogel be a kind of by nanoparticle pile up there is nano-pore structure, high-specific surface area (>700m2/g), low-density high dispersive solid-state material, wherein aerosil least density can reach 1mg/cm3, once selected Guiness World Records.Within 1931, Stanford University Kistler successfully passes the mode obtained aerosil first of hydrolysis water glass, but is limited to loaded down with trivial details technique and the long period of its method, and aerosil does not cause to be paid close attention to widely.At quiet 40 years, there was important breakthrough in the seminar that French Claud Bernard university Teichner teaches on material and preparation technology, successfully obtains high-quality aerosil.Thus from the 1970's, increasing researcher joins among the research of aerogel.With aerogel fast development also have collosol and gel science, the two promotes mutually, even to this day, no matter aerogel kind or purposes all must be extended by very big.Aerosil thermal insulation material room temperature thermal conductivity can be low to moderate 0.013w/ (mk), use temperature can up to 1300 DEG C, solid material the lightest up to now and heat-insulating property best material, the revolutionary substitute products of conventional insulation material, energy energy-conservation about 30% compared with traditional material.Building energy saving field is the maximum application market of silica aerogel material.Current restriction its be that price is higher in the major obstacle of Application in Building, but update perfect along with technique, cost progressively declines, and reaches market acceptance at present, and construction market is very huge.At present, China relates to the production and selling enterprise whole nation relevant with building energy conservation exterior wall heat-preserving system product and reaches 8000, expect the year two thousand twenty, building energy-saving renovation and new building heat preservation energy-saving market space total about reach 5 trillion yuan, and the market of super aerogel insulating material is huge.
The production technique mainly supercritical drying of current aerosil, can be divided into again the drying of alcohols high-temperature supercritical (as ethanol supercritical drying, supercritical state Tc=241.15 DEG C, Pc=6.38MPa.) and low temperature supercritical drying (as CO 2 supercritical is dry, supercritical state Tc=31.2 DEG C, Pc=7.38MPa).The problems such as any supercritical drying process all exists equipment complexity, and energy consumption is high, and the production time is long, and manufacturing cost is expensive.The aerogel material that market is sold, many employing tetraethoxys are silicon source, and trimethylchlorosilane does hydrophobic, containing the chlorion to stainless steel heavy corrosion, can not in nuclear power and the application of natural gas liquids field.Meanwhile, the aerogel heat-insulating felt intensity that market is sold is low, and not anti-folding, tears easy fracture, layering by external force, limits the widespread adoption of such material at building field.
Constant pressure and dry technology is the important means of large-scale industrial production aerogel material, and constant pressure and dry technology in the past needs loaded down with trivial details washing, exchange of solvent, surface modification, because which limit such technical development.Such as patent 101671029 carries out hydrolysis reaction 48 ~ 60h after first tetraethoxy, dehydrated alcohol, oxalic acid and water being mixed, wherein the mol ratio of tetraethoxy and water is 1:1, the mol ratio of tetraethoxy and dehydrated alcohol is 1: 7, and the mol ratio of tetraethoxy and oxalic acid is 1: 9 × 10-4; The second, then add water, DMF and ammoniacal liquor, leave standstill 24 ~ 48h and obtain gel; Three, after gel step 2 prepared places 2 ~ 6h in 20 ~ 60 DEG C of loft drier, then the aqueous solution that volumetric concentration is 80% ethanol is placed in, burin-in process 12 ~ 24h under 40 ~ 60 DEG C of conditions, be placed in tetraethoxy and alcohol mixeding liquid that volume ratio is 1: 5 again, burin-in process 12 ~ 24h under 40 ~ 60 DEG C of conditions; Four, the gel after burin-in process is put into Virahol and carry out solvent exchange 4 ~ 8h, then put into volume ratio be 1 ~ 4: 5 Virahol and normal hexane mixed solution carry out solvent exchange 1 ~ 5 time, each 4 ~ 8h, put into normal hexane again and carry out solvent exchange 4 ~ 8h, then be that 1: 1 ~ 50 trimethylchlorosilanes and normal hexane mixed solution carry out finishing to completely transparent by volume ratio, again with volume ratio be 1: 1 ~ 50 Virahols and normal hexane mixed solution cleaning 4 ~ 8h, then with normal hexane cleaning 4 ~ 8h; Five, by the dry 6 ~ 10h under 40 ~ 80 DEG C of conditions of the gel after step 4 process, obtain aerogel, process is extremely loaded down with trivial details, uses again chloride, poisonous trimethylchlorosilane as properties-correcting agent, is not suitable for suitability for industrialized production.
Patent CN101691227 first prepares wet gel with tetraethyl orthosilicate and methyltrimethoxy silane or Union carbide A-162; Then wet gel is immersed in ethanol atmosphere standing aging; After aging by soak in trimethylchlorosilane, dehydrated alcohol and normal hexane mixing solutions; Then in trimethylchlorosilane, dehydrated alcohol and normal hexane mixing solutions, take out gel, embathe with normal hexane, remove the mixing solutions remaining in sample surfaces, and make it to be immersed in normal hexane; Dry again, finally obtain silica aerogel material, process is equally very loaded down with trivial details.After patent CN101863480A is also through loaded down with trivial details exchange of solvent, adds poisonous trimethylchlorosilane and alkane by the Si-OH alkylation of gel skeleton surface, then carry out constant pressure and dry and obtain aerosil.
Rigid silicon dioxide aerogel plate technology of preparing disclosed by the invention, perfectly solve the shortcoming that felt body is softer, simultaneously advanced constant pressure and dry technology is conducive to the large-scale industrial production of aerogel heat-insulating plate, production technique low temperature, low pressure, nontoxic, production process low-carbon (LC), environmental protection, such sheet material is the splendid green building material of performance.
Summary of the invention
The invention provides that a kind of intensity is good, the preparation method of the rigid silicon dioxide aerogel heat-insulating plate of low-carbon environment-friendly.
Realize the preparation method of the rigid silicon dioxide aerogel heat-insulating plate of the object of the invention, comprise the steps:
(1) the sodium silicate 68 ~ 120g of delivery number 3.1 ~ 3.6, adds pure water 100 ~ 200g and stirs, obtain dilution water glass;
(2) take 40wt% sulfuric acid 25 ~ 100g, add 10 ~ 40g ethanol, stir, obtain sulphuric acid soln;
(3) by dilution water glass and sulphuric acid soln mixing, regulate PH to be 3.5 ~ 4.5, obtain colloidal sol;
(4) colloidal sol poured into be placed with in the mould of fortifying fibre, colloidal sol will after 10 ~ 15min gel, be then incubated 50 ~ 80 DEG C and leave standstill 2 ~ 10h, obtained gel slab;
(5) integration is aging contains alcohol water-setting offset plate with acid alcoholization: preparation 95wt% ethanol and 20 ~ 40wt% sulfuric acid mass ratio are the molten 1500 ~ 3000ml of mixing of 20:1 ~ 60:1, are inserted by gel slab, are incubated 50 ~ 80 DEG C of process 5 ~ 10 hours;
(6) gel slab completing acid alcohol is inserted in the trimethylethoxysilane of 1000 ~ 2500ml, process under room temperature, in 6 ~ 10h, a step is completed hydrophobically modified and gel discharge opeing;
(7), after discharge opeing completes, wet gel plate is carried out hot nitrogen or CO 2 supercritical drying, temperature is 60 ~ 100 DEG C, time 30 ~ 80min.
The beneficial effect of the preparation method of rigid silicon dioxide aerogel heat-insulating plate of the present invention is as follows:
The preparation method of rigid silicon dioxide aerogel heat-insulating plate of the present invention, solve the shortcoming that felt body is softer, simultaneously advanced constant pressure and dry technology is conducive to the large-scale industrial production of aerogel heat-insulating plate, production technique low temperature, low pressure, nontoxic, production process low-carbon (LC), environmental protection, the sheet material of preparation is the splendid green building material of performance.Avoid chlorion and fluorion use in process, significantly improve the intensity of aerogel insulating material, cost is reduced to desirable scope simultaneously.
Aerogel particle prepared by the present invention has high-specific surface area, large pore volume, nano aperture, transparency are high, and indices reaches and is even better than organosilicon source aerogel particle.
In the present invention, rigidity aerogel heat-insulating felt thermal conductivity is minimum reaches 0.017 w/ (m k), is better than the aerogel heat-insulating felt that market is sold.Silicon sol, from after different filamentary material compound, through the aging scheme process optimized, can obtain the aerogel composite of various form and purposes.
Dry atmosphere of the present invention is nitrogen or carbonic acid gas, and by these two kinds of protection of inert gas, greatly improve the security of drying process, be beneficial to suitability for industrialized production, equipment operation and maintenance is easy.
Preparation method of the present invention, adds ethanol in the sulphuric acid soln of joining glue, and the obtained hydrogel containing ethanol, is conducive to the lifting of exchange of solvent efficiency, reaches raising reaction efficiency, reduce costs.
Preparation method of the present invention, improves the holding temperature (50 ~ 80 DEG C) of wet gel plate, extends time of repose (2 ~ 10h), is conducive to the intensity improving wet gel plate, can obtains rigidity aerogel plate by high strength wet gel plate.
Embodiment
Embodiment 1
The preparation method of rigid silicon dioxide aerogel heat-insulating plate of the present invention:
Take the sodium silicate 68g of modulus 3.1, add pure water 100g and stir, obtain dilution water glass.Take 40wt% sulfuric acid 100g, add 20g ethanol, stir.By two solution mixing, regulate PH, until reach 4, poured into by colloidal sol and be placed with in the mould of fortifying fibre, colloidal sol incites somebody to action gel, then 50 DEG C of standing 1h after 20 min.Then integrated aging and acid alcoholization is containing alcohol water-setting offset plate, preparation 95wt% ethanol and 20wt% sulfuric acid mass ratio be 20:1 the molten 1500ml of mixing, gel slab is inserted, 50 DEG C of process 5 hours.The gel slab completing acidifying is inserted in the dimethyldiethoxysilane of 1000ml, processes under room temperature, in 6h, a step is completed hydrophobically modified and gel discharge opeing.After discharge opeing completes, wet gel plate is carried out hot nitrogen supercritical drying, temperature is 100 DEG C, and 30min inner drying completes.
It is light blue for obtaining rigid silicon dioxide aerogel heat-insulating plate of the present invention, and translucent particle, volume density is low to moderate 70kg/m 3, specific surface area is up to 820m 2/ g, most probable pore size is 20nm.Aerogel heat-insulating plate thermal conductivity is low to moderate 0.018 w/ (m k), and volume water absorption rate is lower than 3%; Tensile strength is greater than 1MPa, and ultimate compression strength is greater than 0.1MPa, and mechanical strength is better than EPS plate.
Embodiment 2
The preparation method of rigid silicon dioxide aerogel heat-insulating plate of the present invention:
Take the sodium silicate 70g of modulus 3.6, add pure water 150g and stir, obtain dilution water glass.Take 40wt% sulfuric acid 25g, add 40g ethanol, stir.By the mixing of two solution, regulate PH, until reach 3.5, colloidal sol poured into and is placed with in the mould of fortifying fibre, colloidal sol will after 15min gel, then 50 DEG C of standing 2h.Then integrated aging and acid alcoholization is containing alcohol water-setting offset plate, preparation 95wt% ethanol and 40wt% sulfuric acid mass ratio be 20:1 the molten 1500ml of mixing, gel slab is inserted, 50 DEG C of process 5 hours.The gel slab completing acidifying is inserted in the trimethylethoxysilane of 1000ml, processes under room temperature, in 6h, a step is completed hydrophobically modified and gel discharge opeing.After discharge opeing completes, wet gel plate is carried out hot nitrogen supercritical drying, temperature is 100 DEG C, and 30min inner drying completes.
It is light blue for obtaining rigid silicon dioxide aerogel heat-insulating plate of the present invention, and translucent particle, volume density reaches 90kg/m 3, specific surface area is 620m 2/ g, most probable pore size is 25nm.Aerogel heat-insulating plate thermal conductivity is low to moderate 0.020 w/ (m k), and volume water absorption rate is lower than 3%; Tensile strength is greater than 1.5MPa, and ultimate compression strength is greater than 0.15MPa.
Embodiment recited above is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; do not departing under the present invention designs spiritual prerequisite; the various distortion that the common engineering technical personnel in this area make technical solution of the present invention and improvement, all should fall in protection domain that claims of the present invention determine.

Claims (4)

1. a preparation method for rigid silicon dioxide aerogel heat-insulating plate, comprises the steps:
(1) get sodium silicate 68 ~ 120g, add pure water 100 ~ 200g and stir, obtain dilution water glass;
(2) take 40wt% sulfuric acid 25 ~ 100g, add 10 ~ 40g ethanol, stir, obtain sulphuric acid soln;
(3) by dilution water glass and sulphuric acid soln mixing, regulate PH to be 3.5 ~ 4.5, obtain colloidal sol;
(4) colloidal sol poured into be placed with in the mould of fortifying fibre, colloidal sol will after 10 ~ 15min gel, be then incubated 50 ~ 80 DEG C and leave standstill 2 ~ 10h, obtained gel slab;
(5) integration is aging contains alcohol water-setting offset plate with acid alcoholization: preparation 95wt% ethanol and 20 ~ 40wt% sulfuric acid mass ratio are the molten 1500 ~ 3000ml of mixing of 20:1 ~ 60:1, are inserted by gel slab, are incubated 50 ~ 80 DEG C of process 5 ~ 10 hours;
(6) insert in the trimethylethoxysilane of 1000 ~ 2500ml by the gel slab completing acid alcohol, process under room temperature, a step completes hydrophobically modified and gel discharge opeing;
(7), after discharge opeing completes, wet gel plate is carried out hot nitrogen or CO 2 supercritical drying.
2. the preparation method of rigid silicon dioxide aerogel heat-insulating plate according to claim 1, is characterized in that: the sodium silicate modulus in described step (1) is 3.1 ~ 3.6.
3. the preparation method of rigid silicon dioxide aerogel heat-insulating plate according to claim 1, is characterized in that: the treatment time of described step (6) is 6 ~ 10h.
4. according to the preparation method of the arbitrary described rigid silicon dioxide aerogel heat-insulating plate of claim 1 ~ 3, it is characterized in that: in described step (7), drying temperature is 60 ~ 100 DEG C, and the time is 30 ~ 80min.
CN201510376341.3A 2015-07-01 2015-07-01 Preparation method of rigid silicon dioxide aerogel insulating board CN104944887A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105500780A (en) * 2015-12-04 2016-04-20 卓达新材料科技集团有限公司 Aerogel vacuum insulated panel and preparation method thereof
CN105645803A (en) * 2016-01-13 2016-06-08 太原理工大学 Preparation method of aerogel expanded perlite
CN108316487A (en) * 2018-01-20 2018-07-24 金粤幕墙装饰工程有限公司 A kind of inertia aeroge and preparation method
CN109265131A (en) * 2018-11-12 2019-01-25 中研信源(北京)节能科技有限公司 A kind of preparation method of aerogel vacuum thermal insulation plate and its core material
CN109265734A (en) * 2018-09-05 2019-01-25 哈尔滨工程大学 A method of foam of polymers anti-flammability is improved by aerosil thermal insulation fire-proof layer
TWI663062B (en) * 2016-02-05 2019-06-21 Skc股份有限公司 Aerogel complex and preparation method thereof

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EP0859740A1 (en) * 1995-11-09 1998-08-26 Hoechst Research & Technology Deutschland GmbH & Co. KG Process for preparing organically modified aerogels in which the salts formed are precipitated out
CN101837982A (en) * 2010-03-19 2010-09-22 福建师范大学 Method for preparing silicon dioxide aerogel powder
CN102020285A (en) * 2009-09-16 2011-04-20 深圳大学 Preparation method for hydrophobic silica aerogel
CN104030301A (en) * 2014-06-18 2014-09-10 金承黎 Silicon dioxide aerogel material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0859740A1 (en) * 1995-11-09 1998-08-26 Hoechst Research & Technology Deutschland GmbH & Co. KG Process for preparing organically modified aerogels in which the salts formed are precipitated out
CN102020285A (en) * 2009-09-16 2011-04-20 深圳大学 Preparation method for hydrophobic silica aerogel
CN101837982A (en) * 2010-03-19 2010-09-22 福建师范大学 Method for preparing silicon dioxide aerogel powder
CN104030301A (en) * 2014-06-18 2014-09-10 金承黎 Silicon dioxide aerogel material and preparation method thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105500780A (en) * 2015-12-04 2016-04-20 卓达新材料科技集团有限公司 Aerogel vacuum insulated panel and preparation method thereof
CN105645803A (en) * 2016-01-13 2016-06-08 太原理工大学 Preparation method of aerogel expanded perlite
CN105645803B (en) * 2016-01-13 2018-01-12 太原理工大学 The preparation method of aeroge expanded perlite
TWI663062B (en) * 2016-02-05 2019-06-21 Skc股份有限公司 Aerogel complex and preparation method thereof
US10940670B2 (en) 2016-02-05 2021-03-09 Skc Co., Ltd. Aerogel composite and method for preparing same
CN108316487A (en) * 2018-01-20 2018-07-24 金粤幕墙装饰工程有限公司 A kind of inertia aeroge and preparation method
CN109265734A (en) * 2018-09-05 2019-01-25 哈尔滨工程大学 A method of foam of polymers anti-flammability is improved by aerosil thermal insulation fire-proof layer
CN109265131A (en) * 2018-11-12 2019-01-25 中研信源(北京)节能科技有限公司 A kind of preparation method of aerogel vacuum thermal insulation plate and its core material

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