CN102701700A - SiO2 aerogel/inorganic cotton compound thermal insulation felt and preparation method thereof - Google Patents

SiO2 aerogel/inorganic cotton compound thermal insulation felt and preparation method thereof Download PDF

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CN102701700A
CN102701700A CN2012101181043A CN201210118104A CN102701700A CN 102701700 A CN102701700 A CN 102701700A CN 2012101181043 A CN2012101181043 A CN 2012101181043A CN 201210118104 A CN201210118104 A CN 201210118104A CN 102701700 A CN102701700 A CN 102701700A
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sio
inorganic cotton
thermal insulation
gel
insulation felt
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CN102701700B (en
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史非
王晓杰
刘敬肖
白麓楠
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Dalian Polytechnic University
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Dalian Polytechnic University
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Abstract

The invention relates to a SiO2 aerogel/inorganic cotton compound thermal insulation felt and a preparation method of the SiO2 aerogel/inorganic cotton compound thermal insulation felt. The method comprises the following steps of: compounding silica sol and inorganic cotton; ageing the silica sol and the inorganic cotton; carrying out modification and solvent replacement processing; and drying at normal pressure to obtain the SiO2 aerogel/inorganic cotton compound thermal insulation felt. The preparation method of the SiO2 aerogel/inorganic cotton compound thermal insulation felt, which is disclosed by the invention, is characterized in that cheap and easily-obtained industrial raw materials, such as industrial sodium silicate, industrial silica sol, glass wool, rock wool and mineral wool are adopted, the production cost can be lowered, and the ordinary pressure drying technology is convenient and easy to realize, is simple to operate and is suitable for large-scale industrial production. Meanwhile, the product is nontoxic and harmless and does not pollute the environment.

Description

A kind of SiO 2Gas gel/inorganic cotton composite thermal insulation felt and preparation method
Technical field
The present invention relates to the SiO of a kind of low density, low thermal conductivity 2Gas gel/inorganic cotton composite thermal insulation felt and constant pressure and dry preparation method thereof.
Background technology
Building energy-saving heat-insulating material comprises that mainly PS is the lagging material of main raw material; Like extrusion molding polystyrol plastic foam plate (XPS), molded polystyrene plastic foamboard (EPS), spraying PS (SPS), and polyurethane foam lagging materials such as (PUR).Yet there are problems such as poor fire, chance give off heavy smoke when fiery in heat preserving and insulating materials such as existing polyphenyl, urethane.
Silicon-dioxide (SiO 2) gas gel is a kind of novel light nano-porous materials, has characteristics such as high-specific surface area, high porosity and lower thermal conductivity, has excellent thermal and insulating performance.For obtaining the SiO of vesicular structure 2Gas gel, adopting more method in the past is the supercritical drying drying process, however the supercritical drying arts demand is used autoclave, complex process, cost height, and certain danger is arranged.Adopt constant pressure and dry technology more to help accomplishing scale production and practical application.
At present, in order to realize SiO 2Gas gel is at the practical application of heat preservation and insulation field, SiO 2Gas gel and fiber composite and SiO 2The research of airsetting collodion felt is existing to be reported.Document (fabrics for industrial use, 2009,11:9-12) middle report is base material and SiO with the fibre felt 2Gas gel is compound, and surface modification and constant pressure and dry are processed fibre felt composite S iO 2The gas gel heat preserving and insulating material, specifically preparation process is: adopting multi-polysiloxane is the silicon source, obtains SiO through hydrolysis-condensation 2Gel; With the wet gel dipping, gel is penetrated in the fibre felt base material, obtain fibre felt/SiO 2The gel complex body; Aging in the ethanol then, soak a couple of days with hexamethyldisiloxane (oxygen alkane), trimethylchlorosilane is modified, at last at 200 ℃ or the hydrophobic fibre felt composite S iO of ir lamp constant pressure and dry acquisition 2Gas gel.The National University of Defense technology is preparation of raw material colloidal sol with the tetraethoxy, carries out supercritical drying behind the dipping flexible fiber felt and has prepared flexible heat-insulation composite material (Rare Metals Materials and engineering, 2008,37 (suppl.2): 170-173).J.Chandradass etc. utilize service water glass to be raw material, have prepared SiO through constant pressure and dry 2Gas gel/glass fiber blanket, the document is raw materials used identical with this patent with glass wool, but concrete process procedure is different, adopts tetraethoxy (TEOS)/SiO in the document 2/ alcohol solution dipping glass wool, technology is more loaded down with trivial details, and modified solution is different with this patent, drying temperature higher (230 ℃), do not have the thermal conductivity test result data (Journal ofNon-Crystalline Solid, 2008,354:4115-4119).
Utilize SiO 2Gas gel high porosity, lower thermal conductivity characteristics, the New Si O for preparing a kind of lower thermal conductivity, has excellent heat insulating effect and fire resistance 2Gas gel/inorganic cotton composite thermal insulation material will be played a great role in heat preservation and insulation field, have the market outlook that wide application field is become reconciled.
Summary of the invention
The object of the present invention is to provide a kind of by SiO 2Gas gel and inorganic cotton compound have the high-efficiency insulated lagging material of clean environment firendly, lower thermal conductivity, and provide the industrial raw material that utilizes cheapness through this SiO of constant pressure and dry prepared 2The low-cost preparation method of gas gel/inorganic cotton composite thermal insulation felt.
SiO of the present invention 2Gas gel/inorganic cotton composite thermal insulation felt is a raw material with the service water glass or the silicon sol of cheapness, the SiO of the constant pressure and dry prepared lower thermal conductivity through novel quick solvent exchange/surface-treated 2Gas gel/inorganic cotton composite thermal insulation felt, preparation cycle is shorter, is suitable for large-scale production and commercialization practical application.
SiO of the present invention 2The preparation method of gas gel/inorganic cotton composite thermal insulation felt comprises the steps:
1. prepare silicon acid solution;
2. silicic acid sol and inorganic cotton carry out compoundly, obtain SiO 2Gel/inorganic cotton composite block;
3. to SiO 2Gel/inorganic cotton composite block carries out ageing, and modification and solvent replacing are handled; Described properties-correcting agent comprises organosilane and alkanes reagent; Accomplish the plural gel block of back after with alkanes reagent cleaning modification;
4. the SiO after modification being handled 2Gel/inorganic cotton composite block carries out constant pressure and dry to be handled, and obtains SiO 2Gas gel/inorganic cotton composite thermal insulation felt.
Wherein, Among the above-mentioned preparation method, before inorganic cotton and silicic acid sol are compound, also comprise the preparatory coating modification processed steps of inorganic cotton; The concrete operations step is: former inorganic cotton is calcined 2～3h down at 450～500 ℃; Be cooled to room temperature, soak with alumina sol, titanium oxide sol or silica sol again, carry out surface coating modification processing in advance.Among the present invention,, shorten the production cycle in order to accelerate the modification speed of plural gel block; In silicic acid sol, add preparatory properties-correcting agent; Described preparatory properties-correcting agent is SWS-F 221, trimethylethoxysilane, Union carbide A-162 or methyltrimethoxy silane.
And among the present invention, inorganic cotton is preferably glass wool, rock wool, mineral wool or refractory fibre.Also comprise alcohols in the modified solution that step is adopted in 3., alcohols is preferably ethanol or Virahol; Organosilane is preferably one or more mixtures in trimethylchlorosilane, Union carbide A-162, trimethylethoxysilane or the methyltrimethoxy silane; And the volume ratio of properties-correcting agent and alkanes reagent is about 1: 0.5～1: 1, and the alkanes reagent that is used to clean gel is preferably normal hexane, hexanaphthene or heptane.The dry concrete operations step of step in 4. is: successively at 50 ℃, 70 ℃, 90 ℃, 110 ℃, 130 ℃, 150 ℃ each heat preservation and dryness 1.5～2h or at 50 ℃, 80 ℃, 100～120 ℃, 150 ℃ each heat preservation and dryness 2h down down.
Among the preparation method of the present invention, the detailed process of the compound method of silicate solution is: at first the service water glass of modulus=3.38 is pressed V with deionized water Service water glass: V Deionized water=1: 4～1: 5 dilution proportion, carry out IX with strongly acidic styrene's Zeo-karb then, get the silicate solution of pH=2～3.
Among the preparation method of the present invention, the 2. middle SiO of said step 2The preparation method of gel/inorganic cotton composite block is: with step 1. in prepared silicate solution carry out compoundly with inorganic cotton by a certain percentage, require to add the silicate solutions of different amounts according to different heat-insulating property.
Method to the invention described above is further described, and more specifically, this method should comprise following operation steps:
1. prepare aluminum oxide, titanium oxide or silica sol:
The preparation of alumina sol: a certain amount of aluminum isopropylate of weighing; Join in a certain amount of deionized water, stir down, dissolve fully until aluminum isopropylate at 80 ℃; Add an amount of concentrated nitric acid then; Can obtain alumina sol after continuing to stir 2～4h, the concentration of aluminum isopropylate is 1.25～5mol/L in the alumina sol of being prepared, and the concentration of concentrated nitric acid is 0.125～0.75mol/L.
The preparation of titanium oxide sol: with the butyl(tetra)titanate is the titanium source, prepares TiO with reference to sol-gel method 2The film pertinent literature is prepared (silicate journal, 2001,29 (4): 350-354).
The preparation of silica sol: (TEOS) is the silicon source with tetraethoxy, prepares SiO with reference to sol-gel method 2The colloidal sol pertinent literature is prepared (silicate journal, 2001,29 (4): 350-354); Or be raw material with service water glass, obtain the silicic acid of pH=2～3 as stated above after, transfer pH=3～5 to obtain silica sol with sodium hydroxide or ammoniacal liquor; Or be raw material with the industry silicasol, do not dilute or with deionized water by V Industry silicasol: V Deionized water=1: 0.5～1: 1 dilutes, and obtains silica sol.
2. prepare silicon acid solution:
The service water glass of modulus=3.38 is pressed V with deionized water Service water glass: V Deionized water=1: 4～1: 5 dilution proportion, carry out IX with strongly acidic styrene's Zeo-karb then, get the silicate solution of pH=2～3.
3. the preparatory silicate solution of modification:
Add preparatory properties-correcting agent in the silicic acid sol, described preparatory properties-correcting agent is SWS-F 221, trimethylethoxysilane, Union carbide A-162, methyltrimethoxy silane.
4. the preparatory coating modification of inorganic cotton is handled:
Inorganic cotton is calcined 2～3h down at 450～500 ℃; Be cooled to room temperature; Soak with alumina sol, titanium oxide sol or silica sol again, carry out surface coating modification processing in advance, make it abundant absorption; Then gently extruding will unnecessary alumina sol or titanium oxide sol or silica sol liquid put into baking oven after extruding, at 100 ℃ of drying 2～4h down.
5. silicate solution and inorganic cotton is compound, obtains SiO 2Gel/inorganic cotton composite block:
The silicate solution of preparatory modification is poured on the pretreated inorganic cotton, makes it abundant absorption, the saturated inorganic cotton complex body of absorption silicic acid is placed under 60 ℃ of environment makes its gelling, obtain SiO 2Gel/inorganic cotton composite block.Can be in the actual production according to requirements such as different heat-insulating properties, pour the silicate solutions of different amounts into, the volume (ml) of the quality of inorganic cotton (g) and silicate solution is than being 1: 4～1: 20.
6. SiO 2The ageing of gel/inorganic cotton composite block and modification:
To SiO 2The aged condition of gel/inorganic cotton composite block is for carrying out 1～24h under 20～50 ℃; SiO 2Gel/inorganic cotton composite block carries out solvent exchange-surface modification treatment; Modification liquid is made up of organosilicon alkanes, alcohols and alkanes reagent, and wherein the organosilicon alkanes is trimethylchlorosilane or Union carbide A-162, and alcohols is ethanol or Virahol; Also can not add alcohols; Alkane is selected from normal hexane, hexanaphthene or heptane, and the used organosilicon alkanes properties-correcting agent total amount and the volume ratio of silicate solution be about 1: 0.8～1: 1, and the consumption of alkane solvents is for just can submergence SiO 2Gel/inorganic cotton composite block, it is 24～72h that total time is handled in modification, divides 1～3 completion; Modification accomplish the back after with alkanes reagent cleaning modification SiO 2Gel/inorganic cotton composite block.
7. the SiO after modification being handled 2Gel/inorganic cotton composite block carries out constant pressure and dry to be handled, and promptly successively at 50 ℃, 70 ℃, 90 ℃, 110 ℃, 130 ℃, 150 ℃ following each heat preservation and dryness 1.5h～2h, or at 50 ℃, 80 ℃, 100～120 ℃, 150 ℃ following each heat preservation and dryness 2h, obtains SiO 2Gas gel/inorganic cotton composite thermal insulation felt.
Another object of the present invention is to the SiO that provides above-mentioned arbitrary described method to prepare 2Gas gel/inorganic cotton composite thermal insulation felt, the density that it is characterized in that this material is 0.10～0.30g/cm 3, thermal conductivity is 0.010～0.029Wm -1℃ -1
SiO of the present invention 2Gas gel/inorganic cotton composite thermal insulation felt has excellent heat insulation performance, demonstrates extremely strong hydrophobicity, and water-intake rate is zero, can satisfy the heat insulating needs of inner wall of building heat insulating and other special dimension; And has good flame retardant property because of it; Can bear the direct calcination of flame for a long time; General fiber-like lagging material fusing perforation or the broken situation of porous mineral plate class lagging material fracture can not occur, therefore be with a wide range of applications aspect the inner wall of building heat insulating.
SiO involved in the present invention 2The preparation method of gas gel/inorganic cotton composite thermal insulation felt adopts industrial raw material cheap and easy to get such as service water glass, industry silicasol and glass wool, rock wool, mineral wool etc.; Can reduce production costs; And constant pressure and dry technology is convenient and easy, and is simple to operate, is fit to large-scale industrial production; Product is nontoxic simultaneously, can not pollute environment.
Description of drawings
Accompanying drawing 2 width of cloth of the present invention,
Fig. 1 is the SiO of embodiment 1 2Gas gel/glass wool composite thermal insulation felt and surface hydrophobicity photo thereof, visible by figure, prepared SiO 2Gas gel/glass wool composite thermal insulation felt demonstrates obvious hydrophobic, and water droplet is not sprawled on the heat insulation felt surface fully, explains that it has humidity resistance;
Fig. 2 is pure glass wool and SiO 2The comparison diagram of gas gel/glass wool composite thermal insulation felt after by calcination; Wherein, a is a glass wool, and b is SiO 2Gas gel/glass wool heat insulation felt.Visible by Fig. 2, compare SiO with pure glass wool 2Gas gel/glass wool composite thermal insulation felt shows excellent fire-resistant and fire resistance, and pure glass wool can be lighted, and burns; And meanwhile, SiO 2Gas gel/glass wool composite thermal insulation felt is difficult to lighted, can burn.
Embodiment
Following non-limiting example can make those of ordinary skill in the art more fully understand the present invention, but does not limit the present invention in any way.Among the following embodiment,, adopt following means to prepared SiO like no specified otherwise 2The performance of gas gel/inorganic cotton composite thermal insulation felt is measured.
(1) mensuration of density: measure the diameter (d) and the thickness (t) (respectively measure 4 groups, average) of sample respectively with vernier callipers, then according to formula V=π (d/2) 2* t calculates the volume of sample; Weigh the quality m of sample with analytical balance, calculate the density of sample according to formula ρ=m/V.
(2) thermal conductivity or Determination of Thermal Conductivity: utilize YBF3 type thermal conductivity measuring apparatus to measure SiO 2The thermal conductivity of gas gel/inorganic cotton composite thermal insulation felt.Concrete test process is following: 1. earlier sample is put in up and down between two copper coins of thermal conductivity measuring apparatus, fixes, the temperature that the initial temperature of thermal conductivity measuring apparatus is promptly gone up copper coin is adjusted to 100 ℃ of (V T1); 2. pick up counting, every separated 15min note is once played the temperature of copper coin, reaches a fixed value (V up to the temperature of playing copper coin T2), write down this fixed value; 3. sample is removed, copper coin under the heating, the temperature that is heated to than record stops heating for high about about 10 ℃, and every then separated 2min record once plays the temperature of copper coin, calculates the rate of heat release (δ T/ δ t) of copper coin down.At last according to formula
λ = 54 × d ( D 2 ) 2 ( V T 1 - V T 2 ) · δT δt
Calculate the thermal conductivity of sample.
Embodiment 1
Preparation density is 0.23g/cm 3SiO 2Gas gel/glass wool composite thermal insulation felt
1. prepare alumina sol:
The aluminum isopropylate of weighing 20.4g adds the 200ml deionized water and stirs down at 80 ℃, dissolves fully until aluminum isopropylate, adds the concentrated nitric acid of 0.3ml then, is alumina sol after continuing to stir 3h.
2. prepare silicon acid solution:
Measure 60ml service water glass (modulus=3.38, mSiO 2%=26, ρ=1.37g/ml) mix with the 240ml deionized water, IX is carried out through strongly acidic styrene's Zeo-karb in the back that stirs, and obtains the silicate solution of pH=2～3.
3. the preparatory coating of glass wool is handled:
The glass wool of 15.531g is placed in the high temperature sintering furnace to descend to calcine 2h at 500 ℃, and the taking-up weigh is 14.426g; Get on the glass wool after the alumina sol 50ml for preparing is poured on pre-burning, make it abundant absorption, extruding is put into baking oven after unnecessary alumina sol is extruded gently then, dry 2h under 80 ℃.
4. silicate solution and glass wool is compound:
Get the silicate solution 260ml for preparing and be poured on the pretreated glass wool, make it abundant absorption, the glass wool complex body is placed under 60 ℃ of environment it is solidified, after gel and ageing, obtain SiO 2Gel/glass wool composite block.
5. SiO 2The ageing and the modification of gel/glass wool composite block:
To SiO 2Gel/glass wool composite block carries out modification to be handled, and modification liquid is made up of properties-correcting agent trimethylchlorosilane and solvent normal hexane, and the normal hexane consumption is not for just can having SiO in the modifying process 2Gel/glass wool composite block, the volume ratio of used properties-correcting agent trimethylchlorosilane total amount and silicate solution is about 1: 1, and it is 72h that total time is handled in modification; Modification divides to be carried out for three times, and every at a distance from 24h adding properties-correcting agent once the properties-correcting agent add-on is about 1/3 of a total amount for the first time, and the properties-correcting agent add-on is about 1/2 of a total amount for the second time, and the properties-correcting agent add-on is about 1/6 of a total amount for the third time; The glass wool complex body of back after with normal hexane cleaning modification accomplished in modification.
6. the SiO after modification being handled 2Gel/glass wool composite block carries out constant pressure and dry to be handled, and promptly each heat preservation and dryness 2h under 50 ℃, 70 ℃, 90 ℃, 110 ℃, 130 ℃, 150 ℃ obtains SiO 2Gas gel/glass wool complex body.
Through measuring this SiO 2Quality after gas gel-glass wool composite thermal insulation drying of materials is 25.973g, and volume is 112.26cm 3, density is 0.23g/cm 3, thermal conductivity is 0.020Wm -1℃ -1
Embodiment 2
Preparation density is 0.23g/cm 3SiO 2Gas gel-inorganic cotton composite thermal insulation felt
1. prepare alumina sol: 1. with embodiment 1 step;
2. prepare silicon acid solution:
Measure 30ml service water glass (modulus=3.38, mSiO 2%=26, ρ=1.37g/ml) mix with the 120ml deionized water, IX is carried out through strongly acidic styrene's Zeo-karb in the back that stirs, and obtains the silicic acid of pH=2～3.
3. the preparatory coating of glass wool is handled:
The glass wool of 18.890g is placed in the high temperature sintering furnace to descend to burn 2h at 500 ℃, and the taking-up weigh is 16.854g; Get on the glass wool after the alumina sol 80ml for preparing is poured on pre-burning, make it abundant absorption, unnecessary alumina sol is extruded in extruding gently then, then the pretreated glass wool of alumina sol is put into baking oven, dry 2h under 80 ℃.
4. silicate solution and glass wool is compound:
Get the silicate solution 140ml that has prepared,, after stirring it is poured on the pretreated glass wool, make it abundant absorption, the glass wool complex body is placed under 60 ℃ of environment makes its gelling, obtain SiO toward wherein adding the preparatory properties-correcting agent SWS-F 221 of 40ml 2Gel/inorganic cotton composite block.
5. SiO 2The ageing and the modification of gel/glass wool composite block:
To SiO 2Gel/glass wool composite block carries out modification to be handled; Modification liquid is made up of properties-correcting agent trimethylchlorosilane and normal hexane; The volume ratio of trimethylchlorosilane total amount and silicate solution is about 1: 0.8, and the normal hexane consumption is a minimum standard for can not having the plural gel block; It is 48h that total time is handled in modification, and modification is carried out at twice, every 24h modification once, the add-on of properties-correcting agent is about about 1/3 of total amount for the first time, the add-on of properties-correcting agent is about about 2/3 of total amount for the second time; The SiO of back after with normal hexane cleaning modification accomplished in modification 2Gel/glass wool composite block.
6. the SiO after modification being handled 2Gel/glass wool composite block carries out constant pressure and dry to be handled, and promptly each heat preservation and dryness 2h under 50 ℃, 70 ℃, 90 ℃, 110 ℃, 130 ℃, 150 ℃ obtains SiO 2Gas gel/glass wool composite block.
Through measuring this SiO 2Gas gel/dried quality of glass wool composite thermal insulation felt is 29.036g, and volume is 126.03cm 3, be 0.23g/cm through calculating its density 3, thermal conductivity is 0.029Wm -1℃ -1
Embodiment 3
Preparation density is 0.27g/cm 3SiO 2Gas gel/glass wool composite thermal insulation felt
1. prepare alumina sol: 1. with embodiment 1 step;
2. prepare silicon acid solution:
Measure 40ml service water glass (modulus=3.38, mSiO 2%=26, ρ=1.37g/ml) mix with the 160ml deionized water, IX is carried out through strongly acidic styrene's Zeo-karb in the back that stirs, and obtains the silicic acid of pH=2～3.
3. the pre-treatment of glass wool:
The glass wool of 16.957g is placed in the high temperature sintering furnace to descend to burn 2h at 500 ℃, and the taking-up weigh is 15.846g; Get on the glass wool after the alumina sol 110ml for preparing is poured on pre-burning, make it abundant absorption, unnecessary alumina sol is extruded in extruding gently then, then pretreated glass wool is put into baking oven, dry 2h under 80 ℃.
4. silicate solution and glass wool is compound:
Get the silicate solution 160ml for preparing, add the preparatory properties-correcting agent SWS-F 221 of 40ml, after stirring it is poured on the pretreated glass wool, make it abundant absorption, the glass wool complex body is placed under 60 ℃ of environment makes its gelling, obtain SiO 2Gel/inorganic cotton composite block.
5. SiO 2The ageing of gel/inorganic cotton composite block and modification:
To SiO 2Gel/glass wool composite block carries out modification to be handled, and modification liquid is made up of properties-correcting agent trimethylchlorosilane and normal hexane, and the volume ratio of used properties-correcting agent trimethylchlorosilane total amount and silicate solution is about 1: 1, and it is 48h that total time is handled in modification; Modification is carried out at twice, and every at a distance from the 24h modification once the add-on of properties-correcting agent is about about 1/3 of total colloidal sol amount for the first time, and the add-on of properties-correcting agent is about about 2/3 of total colloidal sol amount for the second time; The glass wool complex body of back after with normal hexane cleaning modification accomplished in modification.
6. the gel after modification being handled carries out constant pressure and dry to be handled, and promptly each heat preservation and dryness 2h under 50 ℃, 70 ℃, 90 ℃, 110 ℃, 130 ℃, 150 ℃ obtains SiO 2Gas gel/glass wool composite thermal insulation felt.
Through measuring this SiO 2The quality of gas gel/glass wool composite thermal insulation felt is 34.028g, and volume is 126.03cm 3, be 0.27g/cm through calculating its density 3, thermal conductivity is 0.023Wm -1℃ -1
Embodiment 4
Preparation density is 0.27g/cm 3SiO 2Gas gel/glass wool composite thermal insulation felt
1. prepare alumina sol: 1. with embodiment 1 step;
2. prepare silicon acid solution:
Measure 40ml service water glass (modulus=3.38, mSiO 2%=26, ρ=1.37g/ml) mix with the 160ml deionized water, IX is carried out through strongly acidic styrene's Zeo-karb in the back that stirs, and obtains the silicic acid of pH=2～3.
3. the pre-treatment of glass wool:
The glass wool of 13.306g is placed in the high temperature sintering furnace to descend to burn 2h at 500 ℃, and the taking-up weigh is 12.221g; Get on the glass wool after the alumina sol 150ml for preparing is poured on pre-burning, make it abundant absorption, unnecessary alumina sol is extruded in extruding gently then, then pretreated inorganic cotton is put into baking oven, dry 2h under 80 ℃.
4. silicate solution and glass wool is compound:
Get the silicate solution 140ml for preparing, be poured on the pretreated glass wool, make it abundant absorption, the glass wool complex body is placed under 60 ℃ of environment makes its gelling, obtain SiO 2Gel/inorganic cotton composite block.
5. SiO 2The ageing of gel/inorganic cotton composite block and modification:
To SiO 2Gel/glass wool composite block carries out modification to be handled, and modification liquid is made up of properties-correcting agent trimethylchlorosilane and normal hexane, and the add-on of normal hexane is not for just can there be SiO in the modifying process 2Gel/glass wool composite block, the volume ratio of used properties-correcting agent trimethylchlorosilane total amount and silicate solution is about 1: 1, and it is 72h that total time is handled in modification; Modification divides to be carried out for three times, and every at a distance from the 24h modification once the properties-correcting agent add-on is about 1/3 of a silicic acid volume for the first time, and the properties-correcting agent add-on is about 1/2 of a silicic acid volume for the second time, and the properties-correcting agent add-on is about 1/6 of a silicic acid volume for the third time; The glass wool complex body of back after with normal hexane cleaning modification accomplished in modification.
6. the gel after modification being handled carries out constant pressure and dry to be handled, and promptly each heat preservation and dryness 2h under 50 ℃, 70 ℃, 90 ℃, 110 ℃, 130 ℃, 150 ℃ obtains SiO 2Gas gel/glass wool composite thermal insulation felt.
Through measuring this SiO 2The quality of gas gel/glass wool composite thermal insulation felt is 23.919g, and volume is 88.59cm 3, be 0.27g/cm through calculating its density 3, thermal conductivity is 0.022Wm -1℃ -1
Embodiment 5
Preparation density is 0.19g/cm 3SiO 2Gas gel/glass wool composite thermal insulation felt
1. prepare alumina sol: 1. with embodiment 1 step;
2. prepare silicon acid solution:
Measure 40ml service water glass (modulus=3.38, mSiO 2%=26, ρ=1.37g/ml) mix with the 160ml deionized water, IX is carried out through strongly acidic styrene's Zeo-karb in the back that stirs, and obtains the silicic acid of pH=2～3.
3. the pre-treatment of glass wool:
The glass wool of 13.011g is placed in the high temperature sintering furnace to descend to burn 2h at 500 ℃, and the taking-up weigh is 11.968g; Get on the glass wool after the alumina sol 150ml for preparing is poured on pre-burning, make it abundant absorption, unnecessary alumina sol is extruded in extruding gently then, then pretreated inorganic cotton is put into baking oven, dry 2h under 80 ℃.
4. silicate solution and glass wool is compound:
Get the silicate solution 160ml for preparing and be poured on the pretreated glass wool, make it abundant absorption, the glass wool complex body is placed under 60 ℃ of environment makes its gelling, obtain SiO 2Gel/inorganic cotton composite block.
5. SiO 2The ageing of gel/inorganic cotton composite block and modification:
To SiO 2Gel/glass wool composite block carries out modification to be handled, and modification liquid is made up of properties-correcting agent trimethylchlorosilane and normal hexane, and the add-on of normal hexane is not for just can there be SiO in the modifying process 2Gel/glass wool composite block, the volume ratio of used properties-correcting agent trimethylchlorosilane total amount and silicate solution is about 1: 1, and it is 72h that total time is handled in modification; The glass wool complex body of back after with normal hexane cleaning modification accomplished in modification.Concrete modification operating process is 6. identical with embodiment 1 step.
6. the gel after modification being handled carries out constant pressure and dry to be handled, and promptly each heat preservation and dryness 2h under 50 ℃, 70 ℃, 90 ℃, 110 ℃, 130 ℃, 150 ℃ obtains SiO 2Gas gel/glass wool composite thermal insulation felt.
Through measuring this SiO 2The quality of gas gel/glass wool composite thermal insulation felt is 18.504g, and volume is 97.39cm 3, be 0.19g/cm through calculating its density 3, thermal conductivity is 0.021Wm -1℃ -1
Embodiment 6
Preparation density is 0.16g/cm 3SiO 2Gas gel/glass wool composite thermal insulation felt
1. prepare silicon acid solution:
Measure 60ml service water glass (modulus=3.38, mSiO 2%=26, ρ=1.37g/ml) mix with the 240ml deionized water, IX is carried out through strongly acidic styrene's Zeo-karb in the back that stirs, and obtains the silicic acid of pH=2～3.
2. silicate solution and glass wool is compound:
Getting the silicate solution 400ml for preparing, to be poured on diameter be that 13.29cm, weight are on the glass wool without any processing of 15.216g, makes it abundant absorption, the glass wool complex body is placed under 60 ℃ of environment makes its gelling, obtains SiO 2Gel/glass wool composite block.
3. SiO 2The ageing and the modification of gel/glass wool composite block:
To SiO 2Gel/glass wool composite block carries out modification to be handled, and modification liquid is made up of properties-correcting agent trimethylchlorosilane and normal hexane, and the add-on of normal hexane was not for just there be SiO in the modifying process 2Gel/glass wool composite block, the volume ratio of used properties-correcting agent trimethylchlorosilane total amount and silicate solution is about 1: 1, and it is 72h that total time is handled in modification; Accomplish the glass wool complex body of back after with alkanes reagent cleaning modification.Concrete modification operating process is 6. identical with embodiment 1 step.
4. the gel after modification being handled carries out constant pressure and dry to be handled, and promptly each heat preservation and dryness 2h under 50 ℃, 70 ℃, 90 ℃, 110 ℃, 130 ℃, 150 ℃ obtains SiO 2Gas gel-glass wool complex body.
Through measuring this SiO 2The quality of gas gel-glass wool composite thermal insulation material is 38.157g, and volume is 238.48cm 3, be 0.16g/cm through calculating its density 3, thermal conductivity is 0.011Wm -1℃ -1
Embodiment 7
Preparation density is 0.19g/cm 3SiO 2Gas gel/glass wool composite thermal insulation felt
1. prepare silicon acid solution:
Measure 10ml service water glass (modulus=3.38, mSiO 2%=26, ρ=1.37g/ml) mix with the 40ml deionized water, IX is carried out through strongly acidic styrene's Zeo-karb in the back that stirs, and obtains the silicic acid of pH=2～3.
2. silicate solution and glass wool is compound:
Get and prepare silicate solution 100ml to be poured on diameter be that 13.29cm, weight are on the glass wool without any processing of 4.672g, make it abundant absorption, the glass wool complex body is placed under 60 ℃ of environment makes its gelling, obtain SiO 2Gel/glass wool composite block.
3. the ageing of glass wool complex body and modification:
To SiO 2Gel/glass wool composite block carries out modification to be handled, and modification liquid is made up of properties-correcting agent trimethylchlorosilane and normal hexane, and the add-on of normal hexane was not for just there be SiO in the modifying process 2Gel/glass wool composite block, the volume ratio of used properties-correcting agent trimethylchlorosilane total amount and silicate solution is about 1: 1, and it is 72h that total time is handled in modification; The glass wool complex body of back after with alkanes reagent cleaning modification accomplished in modification.Concrete modification operating process is 6. identical with embodiment 1 step.
4. the gel after modification being handled carries out constant pressure and dry to be handled, and promptly each heat preservation and dryness 2h under 50 ℃, 70 ℃, 90 ℃, 110 ℃, 130 ℃, 150 ℃ obtains SiO 2Gas gel-glass wool complex body.
Through measuring this SiO 2The quality of gas gel-glass wool composite thermal insulation material is 13.395g, and volume is 70.50cm 3, be 0.19g/cm through calculating its density 3, thermal conductivity is 0.017Wm -1℃ -1

Claims (10)

1. SiO 2The preparation method of gas gel/inorganic cotton composite thermal insulation felt comprises the steps:
1. prepare silicon acid solution;
2. silicic acid sol and inorganic cotton carry out compoundly, obtain SiO 2Gel/inorganic cotton composite block;
3. to SiO 2Gel/inorganic cotton composite block carries out ageing, and modification and solvent replacing are handled; Described properties-correcting agent comprises organosilane and alkanes reagent; Accomplish the plural gel block of back after with alkanes reagent cleaning modification;
4. the SiO after modification being handled 2Gel/inorganic cotton composite block carries out constant pressure and dry to be handled, and obtains SiO 2Gas gel/inorganic cotton composite thermal insulation felt.
2. SiO according to claim 1 2The preparation method of gas gel/inorganic cotton composite thermal insulation felt, it is characterized in that silicic acid sol and inorganic cotton are compound before, also comprise the step of silicic acid sol being carried out preparatory modification; Described step is for to join preparatory modifying agent in the silicate solution; Wherein, described preparatory modifying agent is SWS-F 221, trimethylethoxysilane, Union carbide A-162 or methyltrimethoxy silane.
3. SiO according to claim 1 and 2 2The preparation method of gas gel/inorganic cotton composite thermal insulation felt is characterized in that the inorganic cotton during described step 2. is glass wool, rock wool, mineral wool or refractory fibre.
4. SiO according to claim 3 2The preparation method of gas gel/inorganic cotton composite thermal insulation felt, it is characterized in that inorganic cotton and silicic acid sol are compound before, also comprise inorganic cotton is coated processed steps in advance; Described step concrete grammar is following: a. handles 2～3h with inorganic cotton down at 450～500 ℃; Be cooled to room temperature; B. the inorganic cotton after will handling is immersed in alumina sol, titanium oxide sol or the silica sol; C. do not have later fully and take out, the extruding excess liquid is at 100 ℃ of down dry 2～4h.
5. SiO according to claim 4 2The preparation method of gas gel/inorganic cotton composite thermal insulation felt is characterized in that also comprising alcohols in the described step properties-correcting agent 3.; Described alcohols is selected from ethanol and Virahol.
6. SiO according to claim 5 2The preparation method of gas gel/inorganic cotton composite thermal insulation felt is characterized in that the organosilane during described step 3. is selected from one or more mixtures in trimethylchlorosilane, Union carbide A-162, trimethylethoxysilane and the methyltrimethoxy silane; Alkanes reagent is selected from normal hexane, hexanaphthene and heptane.
7. according to claim 1,4 or 6 described SiO 2The preparation method of gas gel/inorganic cotton composite thermal insulation felt is characterized in that the ageing during described step 3. is under 20～50 ℃, to carry out 1～24h.
8. SiO according to claim 7 2The preparation method of gas gel/inorganic cotton composite thermal insulation felt is characterized in that the exsiccant concrete operation method during described step 4. is: successively at 50 ℃, 70 ℃, 90 ℃, 110 ℃, 130 ℃, 150 ℃ following each heat preservation and dryness 1.5h～2h or at 50 ℃, 80 ℃, 100～120 ℃, 150 ℃ following each heat preservation and dryness 2h.
9. according to claim 1 or 8 described SiO 2The preparation method of gas gel/inorganic cotton composite thermal insulation felt is characterized in that the compound method of the silicic acid sol during described step 1. is following: the service water glass of modulus=3.38 is pressed V with deionized water Service water glass: V Deionized water=1: 4～1: 5 dilution proportion, carry out IX with strongly acidic styrene's Zeo-karb then, get the silicate solution of pH=2～3.
10. the SiO for preparing of the described method of claim 1 2Gas gel/inorganic cotton composite thermal insulation felt, the density that it is characterized in that this material is 0.10～0.30g/cm 3, thermal conductivity is 0.010～0.029Wm -1℃ -1
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