CN102701700B - 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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CN102701700B
CN102701700B CN201210118104.3A CN201210118104A CN102701700B CN 102701700 B CN102701700 B CN 102701700B CN 201210118104 A CN201210118104 A CN 201210118104A CN 102701700 B CN102701700 B CN 102701700B
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inorganic cotton
sio
thermal insulation
insulation felt
mineral wool
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CN102701700A (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 2aerogel/inorganic cotton compound thermal insulation felt and preparation method
Technical field
The present invention relates to the SiO of a kind of low-density, low thermal conductivity 2aerogel/inorganic cotton compound thermal insulation felt and constant pressure and dry preparation method thereof.
Background technology
Building energy-saving heat-insulating material mainly comprises the insulation material that polystyrene is primary raw material, as extrusion molding polystyrol plastic foam plate (XPS), molded polystyrene foams plastic plate (EPS), spraying polystyrene (SPS), and the insulation material such as polyurethane foam (PUR).But there is the problems such as poor fire, chance give off heavy smoke time fiery in the heat preserving and insulating materials such as existing polyphenyl, polyurethane.
Silica (SiO 2) aeroge is a kind of novel light nano-porous materials, has the features such as high-specific surface area, high porosity and lower thermal conductivity, has excellent thermal and insulating performance.For obtaining the SiO of loose structure 2aeroge, adopted more method to be supercritical drying process in the past, but supercritical drying process needs to use autoclave, complex process, cost are high, and have certain danger.Constant pressure and dry technique is adopted more to be conducive to accomplishing scale production and practical application.
At present, in order to realize SiO 2aeroge in the practical application of heat preservation and insulation field, SiO 2aeroge and fiber composite and SiO 2the research of airsetting collodion felt is existing to be reported.In document (fabrics for industrial use, 2009,11:9-12), report is base material and SiO with fibrofelt 2aeroge compound, surface modification and constant pressure and dry make fibrofelt composite S iO 2aeroge heat preserving and insulating material, concrete preparation process is: adopt multi-polysiloxane to be silicon source, obtain SiO by hydrolysis-condensation 2gel; With wet gel dipping, make gel penetrate in fibrofelt base material, obtain fibrofelt/SiO 2gel complex; Then aging in ethanol, soak a couple of days with hexamethyldisiloxane (oxygen alkane), trim,ethylchlorosilane is modified, and finally obtains hydrophobic fibrofelt composite S iO at 200 DEG C or infrared lamp constant pressure and dry 2aeroge.The National University of Defense technology is that colloidal sol prepared by raw material with ethyl orthosilicate, carries out supercritical drying and prepared flexible heat-insulation composite material (Rare Metals Materials and engineering, 2008,37 (suppl.2): 170-173) after impregnated flexible fibrofelt.J.Chandradass etc. utilize industrial waterglass for raw material, have prepared SiO by constant pressure and dry 2aeroge/blanket of glass wool, the document is raw materials used identical with this patent with mineral wool, but concrete technology link is different, adopts ethyl orthosilicate (TEOS)/SiO in document 2/ alcohol solution dipping mineral wool, technics comparing is loaded down with trivial details, and modified solution is different from this patent, baking temperature higher (230 DEG C), there is no thermal conductivity test result data (Journal ofNon-Crystalline Solid, 2008,354:4115-4119).
Utilize SiO 2aeroge high porosity, lower thermal conductivity feature, prepare a kind of lower thermal conductivity, have the New Si O of excellent heat insulating effect and fire protecting performance 2aerogel/inorganic cotton compound thermal insulation material, will play a great role in heat preservation and insulation field, the market prospects become reconciled in the field of having a wide range of applications.
Summary of the invention
The object of the present invention is to provide a kind of by SiO 2the high-efficiency insulated heat-barrier material with clean environment firendly, lower thermal conductivity of aeroge and inorganic cotton compound, and provide the cheap raw material of industry of utilization to prepare this SiO by constant pressure and dry technique 2the low cost preparation method of aerogel/inorganic cotton compound thermal insulation felt.
SiO of the present invention 2aerogel/inorganic cotton compound thermal insulation felt, with the industrial waterglass of cheapness or Ludox for raw material, prepares the SiO of lower thermal conductivity by the constant pressure and dry technique of novel fast solvent exchange/surface modification 2aerogel/inorganic cotton compound thermal insulation felt, manufacturing cycle is shorter, is suitable for large-scale production and commercialization practical application.
SiO of the present invention 2the preparation method of aerogel/inorganic cotton compound thermal insulation felt, comprises the steps:
1. silicate solution is prepared;
2. silica sol and inorganic cotton carry out compound, obtain SiO 2gel/inorganic cotton composite block;
3. to SiO 2gel/inorganic cotton composite block carries out ageing, and process replaced by modification and solvent; Described modifier comprises organosilan and alkanes reagent; Modified plural gel block is cleaned with alkanes reagent after completing;
4. to the SiO after modification 2gel/inorganic cotton composite block carries out constant pressure and dry process, obtains SiO 2aerogel/inorganic cotton compound thermal insulation felt.
Wherein, in above-mentioned preparation method, before inorganic cotton and silica sol compound, also comprise the step of inorganic cotton pre-coated modification, concrete operation step is: former inorganic cotton is calcined 2 ~ 3h at 450 ~ 500 DEG C, be cooled to room temperature, then soak with alumina sol, titanium oxide sol or silica sol, carry out surperficial pre-coated modification.In the present invention, in order to accelerate the modification speed of plural gel block, shorten the production cycle, pre-modifier is added in silica sol, described pre-modifier is HMDO, trimethylethoxysilane, MTES or MTMS.
And in the present invention, inorganic cotton is preferably mineral wool, rock wool, mineral wool or refractory fibre.Step 3. in also comprise alcohols in the modified solution that adopts, alcohols is preferably ethanol or isopropyl alcohol; Organosilan is preferably one or more mixtures in trim,ethylchlorosilane, MTES, trimethylethoxysilane or MTMS, and the volume ratio of modifier and alkanes reagent is about 1: 0.5 ~ 1: 1, and be preferably n-hexane, cyclohexane or heptane for the alkanes reagent cleaning gel.Step 4. in dry concrete operation step be: successively at 50 DEG C, 70 DEG C, 90 DEG C, 110 DEG C, 130 DEG C, 150 DEG C each heat preservation and dryness 1.5 ~ 2h or at 50 DEG C, 80 DEG C, 100 ~ 120 DEG C, 150 DEG C each heat preservation and dryness 2h.
In preparation method of the present invention, the detailed process of the compound method of silicate solution is: first by the industrial waterglass deionized water of modulus=3.38 by V industrial waterglass: V deionized water=1: 4 ~ 1: 5 dilution proportion, then carry out ion-exchange with strongly acidic styrene's cationic ion-exchange resin, obtain the silicate solution of pH=2 ~ 3.
In preparation method of the present invention, described step is middle SiO 2. 2the preparation method of gel/inorganic cotton composite block is: by step 1. in obtained silicate solution carry out compound with inorganic cotton by a certain percentage, require according to different heat-insulating properties the silicate solution adding different amount.
Conduct further description the method for the invention described above, more specifically, the method should comprise following operating procedure:
1. aluminium oxide, titanium oxide or silica sol is prepared:
The preparation of alumina sol: weigh a certain amount of aluminium isopropoxide, join in a certain amount of deionized water, stir at 80 DEG C, until aluminium isopropoxide dissolves completely, then appropriate red fuming nitric acid (RFNA) is added, can obtain alumina sol after continuing stirring 2 ~ 4h, in the alumina sol prepared, the concentration of aluminium isopropoxide is 1.25 ~ 5mol/L, and the concentration of red fuming nitric acid (RFNA) is 0.125 ~ 0.75mol/L.
The preparation of titanium oxide sol: take butyl titanate as titanium source, prepares TiO with reference to sol-gel process 2film pertinent literature carries out preparing (silicate journal, 2001,29 (4): 350-354).
The preparation of silica sol: with ethyl orthosilicate (TEOS) for silicon source, prepares SiO with reference to sol-gel process 2colloidal sol pertinent literature carries out preparing (silicate journal, 2001,29 (4): 350-354); Or be raw material with industrial waterglass, after obtaining the silicic acid of pH=2 ~ 3 as stated above, adjust pH=3 ~ 5 to obtain silica sol with NaOH or ammoniacal liquor; Or be raw material with industry silicasol, do not dilute or by deionized water by V industry silicasol: V deionized waterdilute at=1: 0.5 ~ 1: 1, obtains silica sol.
2. silicate solution is prepared:
The industrial waterglass of modulus=3.38 presses V by deionized water industrial waterglass: V deionized water=1: 4 ~ 1: 5 dilution proportion, then carry out ion-exchange with strongly acidic styrene's cationic ion-exchange resin, obtain the silicate solution of pH=2 ~ 3.
3. the silicate solution of pre-modification:
Add pre-modifier in silica sol, described pre-modifier is HMDO, trimethylethoxysilane, MTES, MTMS.
4. the pre-coated modification of inorganic cotton:
Inorganic cotton is calcined 2 ~ 3h at 450 ~ 500 DEG C, be cooled to room temperature, soak with alumina sol, titanium oxide sol or silica sol again, carry out surperficial pre-coated modification, make it abundant absorption, then extrude gently after unnecessary alumina sol or titanium oxide sol or silica sol liquid are extruded and put into baking oven, dry 2 ~ 4h at 100 DEG C.
5. the compound of silicate solution and inorganic cotton, obtains SiO 2gel/inorganic cotton composite block:
The silicate solution of pre-modification is poured on pretreated inorganic cotton, makes it abundant absorption, make its gelling under inorganic cotton complex saturated for absorption silicic acid is placed on 60 DEG C of environment, obtain SiO 2gel/inorganic cotton composite block.Can according to requirements such as different heat-insulating properties in actual production, pour the silicate solution of different amount into, the quality (g) of inorganic cotton and the volume (ml) of silicate solution are than being 1: 4 ~ 1: 20.
6. SiO 2the ageing of gel/inorganic cotton composite block and modification:
To SiO 2the condition of the ageing of gel/inorganic cotton composite block for carry out 1 ~ 24h at 20 ~ 50 DEG C; SiO 2gel/inorganic cotton composite block carries out exchange of solvent-surface modification treatment, modification liquid is made up of organosilicon alkanes, alcohols and alkanes reagent, wherein organosilicon alkanes is trim,ethylchlorosilane or MTES, alcohols is ethanol or isopropyl alcohol, also alcohols can not be added, alkane is selected from n-hexane, cyclohexane or heptane, and organosilicon alkanes modifier total amount used and the volume ratio of silicate solution are about 1: 0.8 ~ 1: 1, and the consumption of alkane solvents is just can submergence SiO 2gel/inorganic cotton composite block, modification total time is 24 ~ 72h, divides and completes for 1 ~ 3 time; After modification completes with the cleaning of alkanes reagent modified SiO 2gel/inorganic cotton composite block.
7. to the SiO after modification 2gel/inorganic cotton composite block carries out constant pressure and dry process, i.e. each heat preservation and dryness 1.5h ~ 2h at 50 DEG C, 70 DEG C, 90 DEG C, 110 DEG C, 130 DEG C, 150 DEG C successively, or at 50 DEG C, 80 DEG C, 100 ~ 120 DEG C, 150 DEG C each heat preservation and dryness 2h, obtain SiO 2aerogel/inorganic cotton compound thermal insulation felt.
Another object of the present invention is to the SiO providing above-mentioned arbitrary described method to prepare 2aerogel/inorganic cotton compound thermal insulation felt, is characterized in that the density of this material is 0.10 ~ 0.30g/cm 3, thermal conductivity factor is 0.010 ~ 0.029Wm -1dEG C -1.
SiO of the present invention 2aerogel/inorganic cotton compound thermal insulation felt has excellent thermal and insulating performance, presents extremely strong hydrophobicity, and water absorption rate is zero, can meet the insulation needs of inner wall of building insulation and other special dimension; And because of it, there is excellent fire resistance, the direct calcination of flame can be born for a long time, there will not be the situation of general fiber-like heat-barrier material fusing perforation or porous mineral plate class heat-barrier material fracture fragmentation, be therefore with a wide range of applications in inner wall of building insulation.
SiO involved in the present invention 2the preparation method of aerogel/inorganic cotton compound thermal insulation felt adopts the raw material of industry cheap and easy to get as industrial waterglass, industry silicasol and mineral wool, rock wool, mineral wool etc., production cost can be reduced, and constant pressure and dry technique is convenient and easy, simple to operate, be applicable to large-scale industrial production, product is nontoxic simultaneously, can not to environment.
Accompanying drawing explanation
Accompanying drawing 2 width of the present invention,
Fig. 1 is the SiO of embodiment 1 2aeroge/mineral wool composite thermal insulation felt and surface hydrophobic photo thereof, as seen from the figure, prepared SiO 2aeroge/mineral wool composite thermal insulation felt presents obvious hydrophobicity, and water droplet is not sprawled completely on heat insulation felt surface, illustrates that it has humidity resistance;
Fig. 2 is pure mineral wool and SiO 2aeroge/mineral wool composite thermal insulation felt is by the comparison diagram after calcination; Wherein, a is mineral wool, and b is SiO 2aeroge/mineral wool heat insulation felt.As seen from Figure 2, compared with pure mineral wool, SiO 2aeroge/mineral wool composite thermal insulation felt shows excellent fire-resistant and fire protecting performance, and pure mineral wool can be lighted, and burns; And meanwhile, SiO 2aeroge/mineral wool composite thermal insulation felt is difficult to be lighted, and can not burn.
Detailed description of the invention
Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.Below in embodiment, if no special instructions, adopt following means to prepared SiO 2the performance of aerogel/inorganic cotton compound thermal insulation felt measures.
(1) mensuration of density: the diameter (d) and the thickness (t) (each amount 4 groups, averages) that measure sample respectively with slide measure, then according to formula V=π (d/2) 2× t calculates the volume of sample; Weigh the quality m of sample with assay balance, calculate the density of sample according to formula ρ=m/V.
(2) mensuration of thermal conductivity factor or thermal conductivity: utilize YBF3 type thermal conductivity measuring apparatus to measure SiO 2the thermal conductivity of aerogel/inorganic cotton compound thermal insulation felt.Concrete test process is as follows: 1. first sample is put in up and down between two copper coins of thermal conductivity measuring apparatus, is fixed, and the temperature namely initial temperature of thermal conductivity measuring apparatus being gone up copper coin is adjusted to 100 DEG C of (V t1); 2. start timing, once play the temperature of copper coin every 15min note, until the temperature of lower copper coin reaches a fixed value (V t2), write down this fixed value; 3. removed by sample, the lower copper coin of heating, is heated to and stops heating than the temperature height about about 10 DEG C of record, then once play the temperature of copper coin every 2min record, calculates the rate of heat dispation (δ T/ δ t) of lower copper coin.Last according to formula
λ = 54 × d ( D 2 ) 2 ( V T 1 - V T 2 ) · δT δt
Calculate the thermal conductivity factor of sample.
Embodiment 1
Preparation density is 0.23g/cm 3siO 2aeroge/mineral wool composite thermal insulation felt
1. alumina sol is prepared:
Weigh the aluminium isopropoxide of 20.4g, add 200ml deionized water and stir at 80 DEG C, until aluminium isopropoxide dissolves completely, then add the red fuming nitric acid (RFNA) of 0.3ml, after continuing to stir 3h, be alumina sol.
2. silicate solution is prepared:
Measure 60ml industrial waterglass (modulus=3.38, mSiO 2%=26, ρ=1.37g/ml) mix with 240ml deionized water, carry out ion-exchange by strongly acidic styrene's cationic ion-exchange resin after stirring, obtain the silicate solution of pH=2 ~ 3.
3. the pre-coated process of mineral wool:
Be placed in high temperature sintering furnace by the mineral wool of 15.531g and calcine 2h at 500 DEG C, taking-up weigh is 14.426g; Get the alumina sol 50ml prepared be poured on pre-burning after mineral wool on, make it abundant absorption, then extrude gently after unnecessary alumina sol is extruded and put into baking oven, dry 2h at 80 DEG C.
4. the compound of silicate solution and mineral wool:
Get the silicate solution 260ml prepared to be poured on pretreated mineral wool, make it abundant absorption, make it solidify under mineral wool complex being placed on 60 DEG C of environment, after gel and ageing, obtain SiO 2gel/mineral wool composite block.
5. SiO 2the ageing of gel/mineral wool composite block and modification:
To SiO 2gel/mineral wool composite block carries out modification, and modification liquid is made up of modifier trim,ethylchlorosilane and solvent hexane, and in modifying process, n-hexane consumption is not for just can have SiO 2gel/mineral wool composite block, the volume ratio of modifier trim,ethylchlorosilane total amount used and silicate solution is about 1: 1, and modification total time is 72h; Modification divides to be carried out for three times, adds modifier once every 24h, and modifier addition is about 1/3 of total amount for the first time, and second time modifier addition is about 1/2 of total amount, and modifier addition is about 1/6 of total amount for the third time; Modified mineral wool complex is cleaned with n-hexane after modification completes.
6. to the SiO after modification 2gel/mineral wool composite block carries out constant pressure and dry process, and namely each heat preservation and dryness 2h at 50 DEG C, 70 DEG C, 90 DEG C, 110 DEG C, 130 DEG C, 150 DEG C, obtains SiO 2aeroge/mineral wool complex.
After measured, this SiO 2aeroge-dried quality of mineral wool theremal-preserving heat-insulating material is 25.973g, and volume is 112.26cm 3, density is 0.23g/cm 3, thermal conductivity factor is 0.020Wm -1dEG C -1.
Embodiment 2
Preparation density is 0.23g/cm 3siO 2aeroge-inorganic cotton composite thermal insulation felt
1. alumina sol is prepared: with embodiment 1 step 1.;
2. silicate solution is prepared:
Measure 30ml industrial waterglass (modulus=3.38, mSiO 2%=26, ρ=1.37g/ml) mix with 120ml deionized water, carry out ion-exchange by strongly acidic styrene's cationic ion-exchange resin after stirring, obtain the silicic acid of pH=2 ~ 3.
3. the pre-coated process of mineral wool:
Be placed in high temperature sintering furnace by the mineral wool of 18.890g and burn 2h at 500 DEG C, taking-up weigh is 16.854g; Get the alumina sol 80ml prepared be poured on pre-burning after mineral wool on, make it abundant absorption, then extrude gently and unnecessary alumina sol is extruded, then pretreated for alumina sol mineral wool is put into baking oven, dry 2h at 80 DEG C.
4. the compound of silicate solution and mineral wool:
Get the silicate solution 140ml prepared, toward wherein adding the pre-modifier HMDO of 40ml, being poured on after stirring on pretreated mineral wool, making it abundant absorption, under mineral wool complex being placed on 60 DEG C of environment, making its gelling, obtain SiO 2gel/inorganic cotton composite block.
5. SiO 2the ageing of gel/mineral wool composite block and modification:
To SiO 2gel/mineral wool composite block carries out modification, modification liquid is made up of modifier trim,ethylchlorosilane and n-hexane, the volume ratio of trim,ethylchlorosilane total amount and silicate solution is about 1: 0.8, and n-hexane consumption is not for can have plural gel block to be minimum standard; Modification total time is 48h, and modification is carried out at twice, and once, the addition of modifier is about about 1/3 of total amount for the first time in every 24h modification, and the addition of second time modifier is about about 2/3 of total amount; Modified SiO is cleaned with n-hexane after modification completes 2gel/mineral wool composite block.
6. to the SiO after modification 2gel/mineral wool composite block carries out constant pressure and dry process, and namely each heat preservation and dryness 2h at 50 DEG C, 70 DEG C, 90 DEG C, 110 DEG C, 130 DEG C, 150 DEG C, obtains SiO 2aeroge/mineral wool composite block.
After measured, this SiO 2aeroge/dried quality of mineral wool composite thermal insulation felt is 29.036g, and volume is 126.03cm 3, its density is 0.23g/cm as calculated 3, thermal conductivity factor is 0.029Wm -1dEG C -1.
Embodiment 3
Preparation density is 0.27g/cm 3siO 2aeroge/mineral wool composite thermal insulation felt
1. alumina sol is prepared: with embodiment 1 step 1.;
2. silicate solution is prepared:
Measure 40ml industrial waterglass (modulus=3.38, mSiO 2%=26, ρ=1.37g/ml) mix with 160ml deionized water, carry out ion-exchange by strongly acidic styrene's cationic ion-exchange resin after stirring, obtain the silicic acid of pH=2 ~ 3.
3. the pretreatment of mineral wool:
Be placed in high temperature sintering furnace by the mineral wool of 16.957g and burn 2h at 500 DEG C, taking-up weigh is 15.846g; Get the alumina sol 110ml prepared be poured on pre-burning after mineral wool on, make it abundant absorption, then extrude gently and unnecessary alumina sol is extruded, then pretreated mineral wool is put into baking oven, dry 2h at 80 DEG C.
4. the compound of silicate solution and mineral wool:
Get the silicate solution 160ml prepared, add the pre-modifier HMDO of 40ml, be poured on after stirring on pretreated mineral wool, make it abundant absorption, under mineral wool complex being placed on 60 DEG C of environment, make its gelling, obtain SiO 2gel/inorganic cotton composite block.
5. SiO 2the ageing of gel/inorganic cotton composite block and modification:
To SiO 2gel/mineral wool composite block carries out modification, and modification liquid is made up of modifier trim,ethylchlorosilane and n-hexane, and the volume ratio of modifier trim,ethylchlorosilane total amount used and silicate solution is about 1: 1, and modification total time is 48h; Modification is carried out at twice, and every 24h modification once, the addition of modifier is about about 1/3 of total colloidal sol amount for the first time, and the addition of second time modifier is about about 2/3 of total colloidal sol amount; Modified mineral wool complex is cleaned with n-hexane after modification completes.
6. carry out constant pressure and dry process to the gel after modification, namely each heat preservation and dryness 2h at 50 DEG C, 70 DEG C, 90 DEG C, 110 DEG C, 130 DEG C, 150 DEG C, obtains SiO 2aeroge/mineral wool composite thermal insulation felt.
After measured, this SiO 2the quality of aeroge/mineral wool composite thermal insulation felt is 34.028g, and volume is 126.03cm 3, its density is 0.27g/cm as calculated 3, thermal conductivity factor is 0.023Wm -1dEG C -1.
Embodiment 4
Preparation density is 0.27g/cm 3siO 2aeroge/mineral wool composite thermal insulation felt
1. alumina sol is prepared: with embodiment 1 step 1.;
2. silicate solution is prepared:
Measure 40ml industrial waterglass (modulus=3.38, mSiO 2%=26, ρ=1.37g/ml) mix with 160ml deionized water, carry out ion-exchange by strongly acidic styrene's cationic ion-exchange resin after stirring, obtain the silicic acid of pH=2 ~ 3.
3. the pretreatment of mineral wool:
Be placed in high temperature sintering furnace by the mineral wool of 13.306g and burn 2h at 500 DEG C, taking-up weigh is 12.221g; Get the alumina sol 150ml prepared be poured on pre-burning after mineral wool on, make it abundant absorption, then extrude gently and unnecessary alumina sol is extruded, then pretreated inorganic cotton is put into baking oven, dry 2h at 80 DEG C.
4. the compound of silicate solution and mineral wool:
Get the silicate solution 140ml prepared, be poured on pretreated mineral wool, make it abundant absorption, under mineral wool complex being placed on 60 DEG C of environment, make its gelling, obtain SiO 2gel/inorganic cotton composite block.
5. SiO 2the ageing of gel/inorganic cotton composite block and modification:
To SiO 2gel/mineral wool composite block carries out modification, and modification liquid is made up of modifier trim,ethylchlorosilane and n-hexane, and in modifying process, the addition of n-hexane is not for just can there to be SiO 2gel/mineral wool composite block, the volume ratio of modifier trim,ethylchlorosilane total amount used and silicate solution is about 1: 1, and modification total time is 72h; Modification divides to be carried out for three times, and every 24h modification once, modifier addition is about 1/3 of silicic acid volume for the first time, and second time modifier addition is about 1/2 of silicic acid volume, and modifier addition is about 1/6 of silicic acid volume for the third time; Modified mineral wool complex is cleaned with n-hexane after modification completes.
6. carry out constant pressure and dry process to the gel after modification, namely each heat preservation and dryness 2h at 50 DEG C, 70 DEG C, 90 DEG C, 110 DEG C, 130 DEG C, 150 DEG C, obtains SiO 2aeroge/mineral wool composite thermal insulation felt.
After measured, this SiO 2the quality of aeroge/mineral wool composite thermal insulation felt is 23.919g, and volume is 88.59cm 3, its density is 0.27g/cm as calculated 3, thermal conductivity factor is 0.022Wm -1dEG C -1.
Embodiment 5
Preparation density is 0.19g/cm 3siO 2aeroge/mineral wool composite thermal insulation felt
1. alumina sol is prepared: with embodiment 1 step 1.;
2. silicate solution is prepared:
Measure 40ml industrial waterglass (modulus=3.38, mSiO 2%=26, ρ=1.37g/ml) mix with 160ml deionized water, carry out ion-exchange by strongly acidic styrene's cationic ion-exchange resin after stirring, obtain the silicic acid of pH=2 ~ 3.
3. the pretreatment of mineral wool:
Be placed in high temperature sintering furnace by the mineral wool of 13.011g and burn 2h at 500 DEG C, taking-up weigh is 11.968g; Get the alumina sol 150ml prepared be poured on pre-burning after mineral wool on, make it abundant absorption, then extrude gently and unnecessary alumina sol is extruded, then pretreated inorganic cotton is put into baking oven, dry 2h at 80 DEG C.
4. the compound of silicate solution and mineral wool:
Get the silicate solution 160ml prepared to be poured on pretreated mineral wool, make it abundant absorption, under mineral wool complex being placed on 60 DEG C of environment, make its gelling, obtain SiO 2gel/inorganic cotton composite block.
5. SiO 2the ageing of gel/inorganic cotton composite block and modification:
To SiO 2gel/mineral wool composite block carries out modification, and modification liquid is made up of modifier trim,ethylchlorosilane and n-hexane, and in modifying process, the addition of n-hexane is not for just can there to be SiO 2gel/mineral wool composite block, the volume ratio of modifier trim,ethylchlorosilane total amount used and silicate solution is about 1: 1, and modification total time is 72h; Modified mineral wool complex is cleaned with n-hexane after modification completes.Concrete modification operating process is 6. identical with embodiment 1 step.
6. carry out constant pressure and dry process to the gel after modification, namely each heat preservation and dryness 2h at 50 DEG C, 70 DEG C, 90 DEG C, 110 DEG C, 130 DEG C, 150 DEG C, obtains SiO 2aeroge/mineral wool composite thermal insulation felt.
After measured, this SiO 2the quality of aeroge/mineral wool composite thermal insulation felt is 18.504g, and volume is 97.39cm 3, its density is 0.19g/cm as calculated 3, thermal conductivity factor is 0.021Wm -1dEG C -1.
Embodiment 6
Preparation density is 0.16g/cm 3siO 2aeroge/mineral wool composite thermal insulation felt
1. silicate solution is prepared:
Measure 60ml industrial waterglass (modulus=3.38, mSiO 2%=26, ρ=1.37g/ml) mix with 240ml deionized water, carry out ion-exchange by strongly acidic styrene's cationic ion-exchange resin after stirring, obtain the silicic acid of pH=2 ~ 3.
2. the compound of silicate solution and mineral wool:
Get the silicate solution 400ml prepared to be poured on the mineral wool without any process that diameter is 13.29cm, weight is 15.216g, make it abundant absorption, under mineral wool complex being placed on 60 DEG C of environment, make its gelling, obtain SiO 2gel/mineral wool composite block.
3. SiO 2the ageing of gel/mineral wool composite block and modification:
To SiO 2gel/mineral wool composite block carries out modification, and modification liquid is made up of modifier trim,ethylchlorosilane and n-hexane, and in modifying process, the addition of n-hexane was not for there just to be SiO 2gel/mineral wool composite block, the volume ratio of modifier trim,ethylchlorosilane total amount used and silicate solution is about 1: 1, and modification total time is 72h; Modified mineral wool complex is cleaned with alkanes reagent after completing.Concrete modification operating process is 6. identical with embodiment 1 step.
4. carry out constant pressure and dry process to the gel after modification, namely each heat preservation and dryness 2h at 50 DEG C, 70 DEG C, 90 DEG C, 110 DEG C, 130 DEG C, 150 DEG C, obtains SiO 2aeroge-mineral wool complex.
After measured, this SiO 2the quality of aeroge-mineral wool theremal-preserving heat-insulating material is 38.157g, and volume is 238.48cm 3, its density is 0.16g/cm as calculated 3, thermal conductivity factor is 0.011Wm -1dEG C -1.
Embodiment 7
Preparation density is 0.19g/cm 3siO 2aeroge/mineral wool composite thermal insulation felt
1. silicate solution is prepared:
Measure 10ml industrial waterglass (modulus=3.38, mSiO 2%=26, ρ=1.37g/ml) mix with 40ml deionized water, carry out ion-exchange by strongly acidic styrene's cationic ion-exchange resin after stirring, obtain the silicic acid of pH=2 ~ 3.
2. the compound of silicate solution and mineral wool:
Get and prepare silicate solution 100ml and be poured on the mineral wool without any process that diameter is 13.29cm, weight is 4.672g, make it abundant absorption, under mineral wool complex being placed on 60 DEG C of environment, make its gelling, obtain SiO 2gel/mineral wool composite block.
3. the ageing of mineral wool complex and modification:
To SiO 2gel/mineral wool composite block carries out modification, and modification liquid is made up of modifier trim,ethylchlorosilane and n-hexane, and in modifying process, the addition of n-hexane was not for there just to be SiO 2gel/mineral wool composite block, the volume ratio of modifier trim,ethylchlorosilane total amount used and silicate solution is about 1: 1, and modification total time is 72h; Modified mineral wool complex is cleaned with alkanes reagent after modification completes.Concrete modification operating process is 6. identical with embodiment 1 step.
4. carry out constant pressure and dry process to the gel after modification, namely each heat preservation and dryness 2h at 50 DEG C, 70 DEG C, 90 DEG C, 110 DEG C, 130 DEG C, 150 DEG C, obtains SiO 2aeroge-mineral wool complex.
After measured, this SiO 2the quality of aeroge-mineral wool theremal-preserving heat-insulating material is 13.395g, and volume is 70.50cm 3, its density is 0.19g/cm as calculated 3, thermal conductivity factor is 0.017Wm -1dEG C -1.

Claims (8)

1. a SiO 2the preparation method of aerogel/inorganic cotton compound thermal insulation felt, comprises the steps:
1. silicate solution is prepared;
2. silica sol and inorganic cotton carry out compound, obtain SiO 2gel/inorganic cotton composite block;
3. to SiO 2gel/inorganic cotton composite block carries out ageing, and process replaced by modification and solvent; Described modifier comprises organosilan and alkanes reagent; Modified plural gel block is cleaned with alkanes reagent after completing;
4. to the SiO after modification 2gel/inorganic cotton composite block carries out constant pressure and dry process, obtains SiO 2aerogel/inorganic cotton compound thermal insulation felt;
Before silica sol and inorganic cotton compound, also comprise the step of silica sol being carried out to pre-modification; Described step is for join in silicate solution by HMDO;
Described step 1. in the compound method of silica sol as follows: the industrial waterglass deionized water of modulus=3.38 is pressed V industrial waterglass: V deionized water=1:4 ~ 1:5 dilution proportion, then carries out ion-exchange with strongly acidic styrene's cationic ion-exchange resin, obtains the silicate solution of pH=2 ~ 3.
2. SiO according to claim 1 2the preparation method of aerogel/inorganic cotton compound thermal insulation felt, is characterized in that the inorganic cotton during described step is 2. mineral wool, rock wool, mineral wool or refractory fibre.
3. SiO according to claim 2 2the preparation method of aerogel/inorganic cotton compound thermal insulation felt, before it is characterized in that inorganic cotton and silica sol compound, also comprises the step of inorganic cotton being carried out to pre-coated process; Described step concrete grammar is as follows: inorganic cotton is processed 2 ~ 3h by a. at 450 ~ 500 DEG C, be cooled to room temperature, b. the inorganic cotton after process is immersed in alumina sol, titanium oxide sol or silica sol, c. take out after not having completely, extrude unnecessary liquid, dry 2 ~ 4h at 100 DEG C.
4. SiO according to claim 3 2the preparation method of aerogel/inorganic cotton compound thermal insulation felt, is characterized in that also comprising alcohols in described step modifier 3.; Described alcohols is selected from ethanol and isopropyl alcohol.
5. SiO according to claim 4 2the preparation method of aerogel/inorganic cotton compound thermal insulation felt, the organosilan that it is characterized in that during described step is 3. is selected from one or more mixtures in trim,ethylchlorosilane, MTES, trimethylethoxysilane and MTMS; Alkanes reagent is selected from n-hexane, cyclohexane and heptane.
6. the SiO according to claim 1,3 or 5 2the preparation method of aerogel/inorganic cotton compound thermal insulation felt, is characterized in that ageing during described step 3. for carry out 1 ~ 24h at 20 ~ 50 DEG C.
7. SiO according to claim 6 2the preparation method of aerogel/inorganic cotton compound thermal insulation felt, is characterized in that the concrete operation method of the drying during described step is 4. is: successively at 50 DEG C, 70 DEG C, 90 DEG C, 110 DEG C, 130 DEG C, 150 DEG C each heat preservation and dryness 1.5h ~ 2h or at 50 DEG C, 80 DEG C, 100 ~ 120 DEG C, 150 DEG C each heat preservation and dryness 2h.
8. the SiO for preparing of method according to claim 1 2aerogel/inorganic cotton compound thermal insulation felt, is characterized in that the density of this material is 0.10 ~ 0.30g/cm 3, thermal conductivity factor is 0.010 ~ 0.029Wm -1dEG C -1.
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