CN103496706A - Preparation method of aerogel composite material - Google Patents
Preparation method of aerogel composite material Download PDFInfo
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- CN103496706A CN103496706A CN201310439024.2A CN201310439024A CN103496706A CN 103496706 A CN103496706 A CN 103496706A CN 201310439024 A CN201310439024 A CN 201310439024A CN 103496706 A CN103496706 A CN 103496706A
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- 239000004964 aerogel Substances 0.000 title claims abstract description 84
- 239000002131 composite material Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 48
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 100
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000010703 silicon Substances 0.000 claims abstract description 47
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 47
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 43
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 36
- 239000012153 distilled water Substances 0.000 claims abstract description 33
- 238000003756 stirring Methods 0.000 claims abstract description 32
- 239000000835 fiber Substances 0.000 claims abstract description 25
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 238000000352 supercritical drying Methods 0.000 claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 72
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 43
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- 229910052757 nitrogen Inorganic materials 0.000 claims description 36
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 24
- 238000010792 warming Methods 0.000 claims description 16
- 239000011521 glass Substances 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000009413 insulation Methods 0.000 claims description 7
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 6
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- 239000004917 carbon fiber Substances 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 235000019353 potassium silicate Nutrition 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- PZZYQPZGQPZBDN-UHFFFAOYSA-N aluminium silicate Chemical compound O=[Al]O[Si](=O)O[Al]=O PZZYQPZGQPZBDN-UHFFFAOYSA-N 0.000 claims description 3
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims description 3
- 210000002268 wool Anatomy 0.000 claims description 3
- 230000032683 aging Effects 0.000 abstract description 15
- 230000000694 effects Effects 0.000 abstract description 4
- 238000007598 dipping method Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 22
- 229960004756 ethanol Drugs 0.000 description 19
- 238000005452 bending Methods 0.000 description 18
- 238000001816 cooling Methods 0.000 description 16
- 238000004080 punching Methods 0.000 description 16
- 229910002012 Aerosil® Inorganic materials 0.000 description 14
- 239000011259 mixed solution Substances 0.000 description 14
- 238000001879 gelation Methods 0.000 description 13
- 229910021529 ammonia Inorganic materials 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000010408 sweeping Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- TZMFJUDUGYTVRY-UHFFFAOYSA-N pentane-2,3-dione Chemical compound CCC(=O)C(C)=O TZMFJUDUGYTVRY-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
The invention relates to a preparation method of an aerogel composite material. The preparation method comprises the following steps: firstly, uniformly mixing a silicon source, a solvent and distilled water in a proportion of (1:4:2)-(1:12:4) and adjusting the pH value to 7-10, and stirring to obtain silicon dioxide sol; and then, dipping fibers in the unaged silicon dioxide sol, and carrying out supercritical drying treatment to obtain the aerogel composite material. According to the method provided by the invention, after the fibers are dipped into the silicon dioxide sol, supercritical drying treatment is directly carried out without gelatinizing and aging the sol at room temperature, so that the prepared aerogel composite material has good flexibility and excellent heat insulating effect. Meanwhile, the method provided by the invention is simple in process flow, the preparation time of the aerogel composite material can be greatly shortened, and the preparation period can be controlled within 4 hours.
Description
Technical field
The present invention relates to a kind of preparation method of aerogel composite, belong to the aerogel technical field.
Background technology
Aerogel is through certain method by the solvent in gel by air displacement out, keeps a kind of cellular solid that the gel vesicular structure is complete simultaneously.Aerogel has the character of multiple uniqueness, comprises extremely low density, high porosity, high-specific surface area, low thermal conductivity etc.
Wherein, the nano-porous structure that aerosil is unique with it, make it at aspects such as calorifics, optics, electricity, acoustics, all show unique character.Aspect calorifics, aerosil has special porous network structure, and void content generally can reach more than 90%, so its density is low.Because the proportion in whole aerogel volume of solid phase in aerosil is very little, add the exclusive crooked pore passage structure of porous network structure, thereby reduced largely the solid thermal conduction of aerosil; On the other hand, aerosil is mesoporous material, and the aperture of its pore is less than 50nm, and the mean free path of air molecule is 70nm, so air molecule is difficult to bump between the space of aerogel, thus decrease the air heat conduction of aerosil.Therefore, the low solid-phase thermal conduction that aerosil shows and hang down the gas phase thermal conduction characteristic and be doomed that it can become a kind of good lagging material.But, the characteristics such as the network structure of aerosil uniqueness, high porosity and low density also cause that itself intensity is low, poor mechanical property, therefore in some intensity to lagging material, mechanical property have the field of requirement, aerosil just can not directly be used as lagging material.In addition, envrionment temperature also plays conclusive impact to the heat exchange pattern of aerosil, when envrionment temperature is elevated to certain temperature, the heat exchange pattern of aerosil will be that main heat transfer type changes into and take the heat transfer type of radiative transfer as leading from take solid-phase thermal conduction and air heat conduction, and for radiative transfer, the structure of aerosil does not have the advantage of radiative transfer, and the heat-proof quality that obviously shows as aerosil significantly reduces.
In order to make aerosil use, and reach better effect of heat insulation at higher temperature, just need to its carry out the doping vario-property processing or with other lagging material compound uses.In prior art, by aerogel and fiber composite formation matrix material, be to improve silica dioxide gel intensity at high temperature and the effective way of heat-proof quality.
Chinese patent literature CN100398492C discloses a kind of SiO
2/ TiO
2aerogel heat-proof composite material, its preparation process comprises: (1), by tetraethoxy, dehydrated alcohol, deionized water, ammoniacal liquor 1:10:3:0.02 in molar ratio, is made into silicon sol with single stage method, aging 1 day; By butyl (tetra) titanate: dehydrated alcohol: deionized water: methyl ethyl diketone 1:10:3:0.3 preparation in molar ratio titanium colloidal sol, then silicon sol is under agitation splashed in titanium colloidal sol, make the raw material tetraethoxy: the butyl (tetra) titanate mol ratio is 1:0.25; (2) adopt and vacuumize Infiltration Technics by volume density 0.07g/cm
3ultra-fine quartz fiber felt immerse in above-mentioned silicon titanium colloidal sol and make the fiber composite silicon sol, under room temperature after this fiber composite silica sol gel in ethanolic soln under room temperature aging 2 days, put into autoclave, preliminary filling N
2to 3MPa, be heated to 270 ℃ with the speed of 1 ℃/min, constant temperature, after 1 hour, keeps temperature-resistant, with the slow relief pressure of the speed of 3MPa/ hour, to after normal pressure with N
2punching is swept autoclave 15 minutes, and powered-down, make its naturally cooling, can make SiO
2/ TiO
2aerogel heat-proof composite material.The aerogel heat-proof composite material that the method makes has excellent mechanical property, good heat-insulating property and hydrophobicity preferably.When the method prepares silicon dioxide aerogel heat-insulating composite material, at first need prepare silicon colloidal sol and silicon sol is carried out to burin-in process, and then prepare the fiber composite silicon sol, this fiber composite silicon sol is after gelation under room temperature, burin-in process, finally under imposing a condition, carry out supercritical drying, make aerogel heat-proof composite material.
At first, in aforesaid method, during preparation fiber composite silicon sol, need to first carrying out to the silicon sol prepared burin-in process, to add wherein fibrefelt to carry out again compound, why will be first to silicon sol, carry out after aging compound again, because the aging rear colloidal sol that just can form easily with fibrefelt coating, combination of silicon sol, thus the bonding strength between fortifying fibre and colloidal sol to a certain extent; Again the fiber composite silicon sol is at room temperature carried out to gelation, burin-in process afterwards;
Secondly, heat-proof quality from aerogel heat-proof composite material, need in preparation process, build from colloidal sol, gel, xerogel until form the reaction process of the xerogel with three-dimensional space network structure, only possessed three-dimensional space network structure good under the microscopic pattern, just can guarantee the heat-proof quality of the aerogel heat-proof composite material for preparing; Wherein, most importantly, the growth of three-dimensional space network structure only has at normal temperatures just can build good structural state.So, in the heat preservation technology field for above purpose, from prepare colloidal sol, collosol and gel, gel aging be before the gel to aging carries out follow-up drying treatment must be through program.Similarly, in above-mentioned Chinese patent literature CN100398492C, in order to guarantee the performance of aerogel composite, just to through the aging fiber composite silicon sol after compound of colloidal sol, having carried out further gelation, burin-in process, thereby realized further slowly polymerization formation xerogel and the formation of three-dimensional space network structure in the xerogel microtexture under the mild conditions of room temperature of colloidal sol, finally guaranteed further to process through supercritical drying the performance of the silicon dioxide aerogel heat-insulating composite material obtained.
, just because of in above-mentioned aerogel heat-proof composite material preparation, to the room temperature gelation of colloidal sol, the processing of aged at room temperature, be also necessary step, so cause the preparation process required time longer, usually need to place more than 3 days; In addition, when carrying out the snappiness detection, the aerogel composite that the method prepares easily fractures, snappiness is poor, so but any reason is caused to the problems referred to above, this area does not have the solution for this problem at present.
Summary of the invention
It is poor that the technical problem to be solved in the present invention is in prior art to prepare the snappiness of fibre-reinforced aerogel heat-insulation composite material, easily fracture, and preparation cycle is longer, thereby it is short and have a preparation method of the aerogel composite of high-flexibility to the invention provides a kind of preparation cycle.
The present invention is achieved by the following technical solutions: a kind of preparation method of aerogel composite is comprised of following steps:
(1) silicon source, solvent, distilled water are mixed for 1:4:2-1:12:4 in molar ratio, and to regulate pH value be 7-10, stirring, obtain silicon dioxide gel;
(2) fiber is immersed to not carrying out in the silicon dioxide gel of burin-in process that step (1) makes, directly carry out the supercritical drying processing, obtain aerogel composite.
In described step (1), carry out the adjusting of pH value with alkali lye.
Described alkali lye is ammoniacal liquor.
The concentration of described ammoniacal liquor is 0.03-0.3mol/L.
The mol ratio of described silicon source, solvent, distilled water is 1:8:4-1:10:4.
Described silicon source is one or more the mixture in tetraethoxy, methyl silicate, trimethylchlorosilane, water glass.
Described solvent is one or more the mixture in ethanol, methyl alcohol, Virahol, acetone.
Described fiber is one or more the mixture in glass mat, aluminium silicate wool, carbon fiber felt.
The step that supercritical drying described in described step (2) is processed is as follows: first preliminary filling 5-10MPa nitrogen, be warming up to 350-400 ℃ with heat-up rate 5-15 ℃/min, and control pressure is 10-20MPa, insulation 30min, again with the speed pressure release of 0.3-0.6MPa/min, finally with nitrogen purging 5-15min.
Described heat-up rate is 6-8 ℃/min.
Technique scheme of the present invention has the following advantages compared to existing technology:
(1) preparation method of aerogel composite of the present invention, form the fiber composite silicon dioxide gel after first fiber being immersed to silicon dioxide gel, to directly be placed in without the fiber composite silicon dioxide gel of burin-in process afterwards autoclave carries out supercritical drying and processes and to obtain aerogel composite, the present invention proposes colloidal sol not to be carried out any such as gelation to the complete reservation of colloidal sol first, aging processing, again the colloidal sol without any processing is directly carried out to follow-up drying treatment, by selecting suitable supercritical drying condition, guaranteed that colloidal sol is without gel, burin-in process is when directly carrying out drying treatment, also still can guarantee the heat-proof quality of the aerogel composite for preparing,
Compared to existing technology, present method has not only been saved and at room temperature colloidal sol has been carried out to aging step, also saved colloidal sol gelation under room temperature, burin-in process is converted into the step of xerogel, thereby simplified technical process, significantly shortened the preparation time of described aerogel composite, most critical be, its aerogel composite prepared has better snappiness compared to prior art, and effect of heat insulation excellence, avoided in prior art needing first the fiber composite silicon dioxide gel at room temperature being carried out to gelation, carry out again the supercritical drying processing after burin-in process, length consuming time but also to prepare the snappiness of aerogel material matrix material very poor not only, the problem easily fractureed.
(2) preparation method of aerogel composite of the present invention, not only save silicon sol and at room temperature carried out gelation, aging operation steps, further, when the described fiber composite silicon sol to without burin-in process carries out supercritical drying, also concrete control condition is: first preliminary filling 5-10MPa nitrogen, heat-up rate with 5-15 ℃/min is warming up to 350-380 ℃, and control pressure is 10-20MPa, insulation 30min, again with the speed pressure release of 0.3-0.6MPa/min, finally with nitrogen purging 5-15min; The processing condition of processing by above-mentioned supercritical drying is set, silicon sol of the present invention does not need to carry out the aged at room temperature processing, and do not need through the gelation under room temperature, burin-in process after forming described fiber composite silicon sol, process the formation aerogel composite with regard to directly carrying out described supercritical drying, not only still there is three-dimensional space network structure good under microscopic pattern in described aerogel composite, also make the bonding strength between fiber and silicon sol increase, thereby present snappiness and excellent effect of heat insulation preferably.
Embodiment
Embodiment 1
The preparation method of the described aerogel composite of the present embodiment, its step is as follows:
(1) take tetraethoxy as the silicon source, ethanol is solvent, get tetraethoxy 440mL, ethanol 720mL, distilled water 108mL, and control tetraethoxy: ethanol: the mol ratio of distilled water is 1:6:3, joins it in container, electric stirring 10min mixes it, take to the weak ammonia 150mL that adds 0.03mol/L in mixed solution that to regulate pH value be 7, after continuing stirring 10min, obtain silicon dioxide gel;
(2) glass mat is immersed in the silicon dioxide gel that step (1) makes, put into afterwards autoclave, after be evacuated to-0.03MPa, be filled with nitrogen to 4MPa, with the heat-up rate of 5 ℃/min, be warming up to 350 ℃, and control pressure is 10MPa, after keeping supercritical state 30min, with the speed pressure release of 0.3MPa/min, 5min is swept in the nitrogen that is finally 0.5L/min with flow velocity punching, open autoclave after cooling, obtain aerogel blanket.
Embodiment 2
The preparation method of the described aerogel composite of the present embodiment, its step is as follows:
(1) take tetraethoxy, methyl silicate, the trimethylchlorosilane mixture that 1:1:1 forms in molar ratio is the silicon source, ethanol is solvent, get silicon source mixture 440mL, ethanol 960mL, distilled water 108mL, and control silicon source mixture: ethanol: the mol ratio of distilled water is 1:8:3, add successively in container, electric stirring 10min mixes it, take to the weak ammonia 160mL that adds 0.08mol/L in mixed solution that to regulate the pH value be 8, after continuing to stir 10min, obtain silicon dioxide gel;
(2) glass mat is immersed in the silicon dioxide gel that step (1) makes, put into afterwards autoclave, after be evacuated to-0.03MPa, be filled with nitrogen to 10MPa, with the heat-up rate of 15 ℃/min, be warming up to 400 ℃, and control pressure is 20MPa, after keeping supercritical state 30min, with the speed pressure release of 0.6MPa/min, 5min is swept in the nitrogen that is finally 0.6L/min with flow velocity punching, open autoclave after cooling, obtain aerogel blanket.
Embodiment 3
The preparation method of the described aerogel composite of the present embodiment, its step is as follows:
(1) take tetraethoxy as the silicon source, ethanol is solvent, get tetraethoxy 440mL, ethanol 1440mL, distilled water 108mL, and control tetraethoxy: ethanol: the mol ratio of distilled water is 1:12:3, add successively in container, electric stirring 10min mixes it, take to the weak ammonia 170mL that adds 0.3mol/L in mixed solution that to regulate the pH value be 9, after continuing to stir 10min, obtain silicon dioxide gel;
(2) carbon fiber felt is immersed in the silicon dioxide gel that step (1) makes, put into afterwards autoclave, after be evacuated to-0.03MPa, rush nitrogen to 8MPa, with the heat-up rate of 10 ℃/min, be warming up to 380 ℃, and control pressure is 15MPa, after keeping supercritical state 30min, with the speed pressure release of 0.4MPa/min, autoclave 15min is swept in the nitrogen that is finally 0.6L/min with flow velocity punching, open autoclave after cooling, obtain aerogel blanket.
Embodiment 4
The preparation method of the described aerogel composite of the present embodiment, its step is as follows:
(1) take tetraethoxy as the silicon source, isopropyl acetone is solvent, get tetraethoxy 440mL, Virahol 920mL, distilled water 81mL, and control tetraethoxy: Virahol: the mol ratio of distilled water is 1:6:4, add successively in container, electric stirring 10min mixes it, take to the weak ammonia 150mL that adds 0.03mol/L in mixed solution that to regulate the pH value be 9, after continuing to stir 10min, obtain silicon dioxide gel;
(2) glass mat is immersed in the silicon dioxide gel that step (1) makes, put into afterwards autoclave, after be evacuated to-0.03MPa, be filled with nitrogen to 6MPa, with the heat-up rate of 8 ℃/min, be warming up to 360 ℃, now pressure is 12MPa, after keeping supercritical state 30min, with the speed pressure release of 0.6MPa/min, 15min in autoclave is swept in the nitrogen that is finally 0.6L/min with flow velocity punching, open autoclave after cooling, obtain aerogel blanket.
Embodiment 5
The preparation method of the described aerogel composite of the present embodiment, its step is as follows:
(1) take tetraethoxy as the silicon source, isopropyl acetone is solvent, get tetraethoxy 440mL, Virahol 1380mL, distilled water 81mL, and control tetraethoxy: Virahol: the mol ratio of distilled water is 1:8:4, adds successively in container, electric stirring 10min mixes it, take to the ammoniacal liquor 160mL that adds 0.13mol/L in mixed solution that to regulate pH value be 8, after continuing stirring 10min, obtain silicon dioxide gel;
(2) glass mat is immersed in the silicon dioxide gel that step (1) makes, put into afterwards autoclave, after be evacuated to-0.03MPa, be filled with nitrogen to 8MPa, with the heat-up rate of 6 ℃/min, be warming up to 380 ℃, and control pressure is 12MPa, after keeping above-critical state 30min, with the speed pressure release of 0.45MPa/min, 10min in autoclave is swept in the nitrogen that is finally 0.6L/min with flow velocity punching, open autoclave after cooling, obtain aerogel blanket.
Embodiment 6
The preparation method of the described aerogel composite of the present embodiment, its step is as follows:
(1) take tetraethoxy as the silicon source, isopropyl acetone is solvent, get tetraethoxy 440mL, Virahol 1840mL, distilled water 81mL, and control tetraethoxy: Virahol: the mol ratio of distilled water is 1:12:4, adds successively in container, electric stirring 10min mixes it, take to the weak ammonia 170mL that adds 0.2mol/L in mixed solution that to regulate pH value be 10, after continuing stirring 10min, obtain silicon dioxide gel;
(2) glass mat is immersed in the silicon dioxide gel that step (1) makes, put into afterwards autoclave, after be evacuated to-0.03MPa, be filled with nitrogen to 5MPa, with the heat-up rate of 15 ℃/min, be warming up to 400 ℃, and control pressure is 20MPa, after keeping above-critical state 30min, with the speed pressure release of 0.5MPa/min, 10min in autoclave is swept in the nitrogen that is finally 0.6L/min with flow velocity punching, open autoclave after cooling, obtain aerogel blanket.
Embodiment 7
The preparation method of the described aerogel composite of the present embodiment, its step is as follows:
(1) take tetraethoxy as the silicon source, methyl alcohol is solvent, get tetraethoxy 300mL, methyl alcohol 465mL, distilled water 110mL, and control methyl silicate: methyl alcohol: the mol ratio of distilled water is 1:6:3, adds successively in container, electric stirring 10min mixes it, take to the weak ammonia 150mL that adds 0.03mol/L in mixed solution that to regulate pH value be 9, after continuing stirring 10min, obtain silicon dioxide gel;
(2) glass mat is immersed in the silicon dioxide gel that step (1) makes, put into afterwards autoclave, after be evacuated to-0.03MPa, be filled with nitrogen to 10MPa, with the heat-up rate electricity of 5 ℃/min, be warming up to 350 ℃, and control pressure is 12MPa, after keeping above-critical state 30min, with the speed pressure release of 0.55MPa/min, 15min in autoclave is swept in the nitrogen that is finally 0.6L/min with flow velocity punching, open autoclave after cooling, obtain aerogel blanket.
Embodiment 8
The preparation method of the described aerogel composite of the present embodiment, its step is as follows:
(1) take tetraethoxy as the silicon source, methyl alcohol is solvent, get tetraethoxy 300mL, methyl alcohol 697.5mL, distilled water 110mL, and control methyl silicate: methyl alcohol: the mol ratio of distilled water is 1:10:4, adds successively in container, electric stirring 10min mixes it, take to the weak ammonia 160mL that adds 0.03mol/L in mixed solution that to regulate pH value be 9, after continuing stirring 10min, obtain silicon dioxide gel;
(2) carbon fiber felt is immersed in the silicon dioxide gel that step (1) makes, put into afterwards autoclave, after be evacuated to-0.03MPa, be filled with nitrogen to 9MPa, with the heat-up rate of 8 ℃/min, be warming up to 360 ℃, and control pressure is 15MPa, after keeping supercritical state 30min, with the speed pressure release of 0.6MPa/min, 10min in autoclave is swept in the nitrogen that is finally 0.6L/min with flow velocity punching, open autoclave after cooling, obtain aerogel blanket.
Embodiment 9
The preparation method of the described aerogel composite of the present embodiment, its step is as follows:
(1) take tetraethoxy as the silicon source, methyl alcohol is solvent, get tetraethoxy 300mL, methyl alcohol 930mL, distilled water 110mL, and control methyl silicate: methyl alcohol: the mol ratio of distilled water is 1:12:3, adds successively in container, electric stirring 10min mixes it, take to the weak ammonia 170mL that adds 0.03mol/L in mixed solution that to regulate pH value be 9, after continuing stirring 10min, obtain silicon dioxide gel;
(2) glass mat is immersed in the silicon dioxide gel that step (1) makes, put into afterwards autoclave, after be evacuated to-0.03MPa, be filled with nitrogen to 8MPa, with the heat-up rate of 5 ℃/min, be warming up to 350 ℃, and control pressure is 10MPa, after keeping above-critical state 30min, with the speed pressure release of 0.45MPa/min, 10min in autoclave is swept in the nitrogen that is finally 0.6L/min with flow velocity punching, open autoclave after cooling, obtain aerogel blanket.
Embodiment 10
The preparation method of the described aerogel composite of the present embodiment, its step is as follows:
(1) take trimethylchlorosilane as the silicon source, ethanol is solvent, get trimethylchlorosilane 420mL, ethanol 780mL, distilled water 120mL, and control trimethylchlorosilane: ethanol: the mol ratio of distilled water is 1:4:2, adds successively in container, electric stirring 10min mixes it, take to the ammoniacal liquor 150mL that adds 0.3mol/L in mixed solution that to regulate pH value be 8, after continuing stirring 10min, obtain silicon dioxide gel;
(2) glass mat is immersed in the silicon dioxide gel that step (1) makes, put into afterwards autoclave, after be evacuated to-0.03MPa, be filled with nitrogen to 5MPa, with the heat-up rate of 8 ℃/min, be warming up to 380 ℃, and control pressure is 12MPa, after keeping above-critical state 30min, with the pressure release speed pressure release of 0.5MPa/min, 10min in autoclave is swept in the nitrogen that is finally 0.6L/min with flow velocity punching, open autoclave after cooling, obtain aerogel blanket.
Embodiment 11
The preparation method of the described aerogel composite of the present embodiment, its step is as follows:
(1) take trimethylchlorosilane as the silicon source, ethanol, methyl alcohol, Virahol, the acetone mixed solvent that 1:1:1:1 forms in molar ratio is solvent, get trimethylchlorosilane 420mL, mixed solvent 1560mL, distilled water 180mL, and control trimethylchlorosilane: mixed solvent: the mol ratio of distilled water is 1:8:3, add successively in container, electric stirring 10min mixes it, take to the weak ammonia 160mL that adds 0.13mol/L in mixed solution that to regulate the pH value be 8, after continuing to stir 10min, obtain silicon dioxide gel;
(2) aluminium silicate wool is immersed in the silicon dioxide gel that step (1) makes, put into afterwards autoclave, after be evacuated to-0.03MPa, be filled with nitrogen to 10MPa, with the heat-up rate of 15 ℃/min, be warming up to 400 ℃, and control pressure is 20MPa, after keeping above-critical state 30min, with the speed pressure release of 0.55MPa/min, 10min in autoclave is swept in the nitrogen that is finally 0.6L/min with flow velocity punching, open autoclave after cooling, obtain aerogel blanket.
Embodiment 12
The preparation method of the described aerogel composite of the present embodiment, its step is as follows:
(1) take trimethylchlorosilane as the silicon source, acetone is solvent, get trimethylchlorosilane 420mL, acetone 2320mL, distilled water 180mL, and control trimethylchlorosilane: acetone: the mol ratio of distilled water is 1:12:3, add successively in container, electric stirring 10min mixes it, take to the weak ammonia 170mL that adds 0.5mol/L in mixed solution that to regulate the pH value be 9, after continuing to stir 10min, obtain silicon dioxide gel;
(2) glass mat is immersed in the silicon dioxide gel that step (1) makes, put into afterwards autoclave, after be evacuated to-0.03MPa, be filled with nitrogen to 12MPa, with the heat-up rate of 4 ℃/min, be warming up to 320 ℃, and control pressure is 6MPa, after keeping above-critical state 30min, with the speed pressure release of 0.8MPa/min, 10min in autoclave is swept in the nitrogen that is finally 0.6L/min with flow velocity punching, open autoclave after cooling, obtain aerogel blanket.
Embodiment 13
The preparation method of the described aerogel composite of the present embodiment, its step is as follows:
(1) take water glass as the silicon source, ethanol is solvent, water intaking glass 300mL, ethanol 465mL, distilled water 55mL, and control water glass: ethanol: the mol ratio of distilled water is 1:6:2, adds successively in container, electric stirring 10min mixes it, take to the weak ammonia 100mL that adds 0.01mol/L in mixed solution that to regulate pH value be 7, after continuing stirring 10min, obtain silicon dioxide gel;
(2) glass mat is immersed in the silicon dioxide gel that step (1) makes, put into afterwards autoclave, after be evacuated to-0.03MPa, be filled with nitrogen to 4MPa, with the heat-up rate of 16 ℃/min, be warming up to 420 ℃, and control pressure is 8MPa, after keeping above-critical state 30min, with the speed pressure release of 0.25MPa/min, 10min in autoclave is swept in the nitrogen that is finally 0.6L/min with flow velocity punching, open autoclave after cooling, obtain aerogel blanket.
Comparative Examples 1
This Comparative Examples provides a kind of preparation method of aerogel composite, and its step is as follows:
(1) take tetraethoxy as the silicon source, isopropyl acetone is solvent, get tetraethoxy 440mL, Virahol 1380mL, distilled water 81mL, and control tetraethoxy: Virahol: the mol ratio of distilled water is 1:8:4, adds successively in container, electric stirring 10min mixes it, take to the ammoniacal liquor 160mL that adds 0.13mol/L in mixed solution that to regulate pH value be 8, after continuing stirring 10min, obtain silicon dioxide gel;
(2) glass mat is adopted the mechanical high-speed dispersed with stirring in described silicon dioxide gel, supersound process disperses to obtain uniform fiber silicon sol suspension again, under room temperature, after its gelation, under room temperature, in ethanol, carry out aging 2 days, put into autoclave, pre-inflated with nitrogen is to 3MPa, the intensification of 1 ℃/min of take is heated to temperature as 270 ℃, after constant temperature 1 hour, keep temperature-resistant, with the pressure release of 3L/min speed, to sweeping autoclave 15min with the nitrogen punching after normal pressure, open autoclave after cooling, obtain aerogel blanket.
Comparative Examples 2
This Comparative Examples provides a kind of preparation method of aerogel composite, and its step is as follows:
(1) by tetraethoxy, dehydrated alcohol, deionized water, ammoniacal liquor 1:10:3:0.02 in molar ratio, be made into silicon sol with single stage method, aging 1 day;
(2) glass mat is immersed in the silicon dioxide gel of step (1) after aging, supersound process disperses to obtain uniform fiber silicon sol suspension again, under room temperature, after its gelation, under room temperature, in ethanol, carry out aging 2 days, put into autoclave, pre-inflated with nitrogen is to 3MPa, the intensification of 1 ℃/min of take is heated to temperature as 270 ℃, after constant temperature 1 hour, keep temperature-resistant, with the pressure release of 3L/min speed, to sweeping autoclave 15min with the nitrogen punching after normal pressure, open autoclave after cooling, obtain aerogel blanket.
Test case
The above-mentioned aerogel composite prepared is carried out to flexible detection:
By preparing the aerogel composite number consecutively in embodiment 1-13 and Comparative Examples 1-2, be A-O, respectively to bending test to estimate its snappiness.
| Numbering | Snappiness detects |
| A | Do not fracture after bending, and can return to original-shape |
| B | Do not fracture after bending, and can return to original-shape |
| C | Do not fracture after bending, and can return to original-shape |
| D | Do not fracture after bending, and can return to original-shape |
| E | Without folding line, do not fracture, and can return to original-shape fully after bending |
| F | Do not fracture after bending, and can return to original-shape |
| G | Do not fracture after bending, and can return to original-shape |
| H | Without folding line, do not fracture, and can return to original-shape fully after bending |
| I | Do not fracture after bending, and can return to original-shape |
| J | Do not fracture after bending, and can return to original-shape |
| K | Do not fracture after bending, and can return to original-shape |
| L | Folding line is arranged after bending |
| M | Folding line is arranged after bending |
| N | After bending, fracture |
| O | There is obvious folding line, frangibility after bending |
Result shows, for aerogel composite described in embodiment 1-13, owing to adopting the described silicon sol of the inventive method without gelation under room temperature, burin-in process, present snappiness preferably with regard to directly being placed in the aerogel composite that super critical condition of the present invention carries out preparing after drying, can not fracture after bending.Yet, for the method in Comparative Examples 1, after preparation obtains silicon sol, need first gel, burin-in process under room temperature, carry out again afterwards the supercritical drying processing, prepare thus the aerogel composite snappiness very poor, easily fracture; Preparation method in Comparative Examples 2, although after preparation obtains silicon sol, also without gelation, burin-in process, just directly adopt super critical condition of the prior art to carry out drying to it, the aerogel material snappiness finally prepared is not still fine, there is obvious folding line after bending, frangibility.
Obviously, above-described embodiment is only for example clearly is described, and is not the restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without also giving all embodiments.And the apparent variation of being extended out thus or change are still among the protection domain in the invention.
Claims (10)
1. the preparation method of an aerogel composite is comprised of following steps:
(1) silicon source, solvent, distilled water are mixed for 1:4:2-1:12:4 in molar ratio, and to regulate pH value be 7-10, stirring obtains silicon dioxide gel;
(2) fiber is immersed to not carrying out in the silicon dioxide gel of burin-in process that step (1) makes, directly carry out the supercritical drying processing, obtain aerogel composite.
2. the preparation method of aerogel composite according to claim 1, is characterized in that, in described step (1), carries out the adjusting of pH value with alkali lye.
3. the preparation method of aerogel composite according to claim 2, is characterized in that, described alkali lye is ammoniacal liquor.
4. the preparation method of aerogel composite according to claim 3, is characterized in that, the concentration of described ammoniacal liquor is 0.03-0.3mol/L.
5. according to the preparation method of the arbitrary described aerogel composite of claim 1-4, it is characterized in that, the mol ratio of described silicon source, solvent, distilled water is 1:8:4-1:10:4.
6. according to the preparation method of the arbitrary described aerogel composite of claim 1-5, it is characterized in that, described silicon source is one or more the mixture in tetraethoxy, methyl silicate, trimethylchlorosilane, water glass.
7. according to the preparation method of the arbitrary described aerogel composite of claim 1-6, it is characterized in that, described solvent is one or more the mixture in ethanol, methyl alcohol, Virahol, acetone.
8. according to the preparation method of the arbitrary described aerogel composite of claim 1-7, it is characterized in that, described fiber is one or more the mixture in glass mat, aluminium silicate wool, carbon fiber felt.
9. according to the preparation method of the arbitrary described aerogel composite of claim 1-8, it is characterized in that, the step that supercritical drying described in described step (2) is processed is as follows: first preliminary filling 5-10MPa nitrogen, heat-up rate with 5-15 ℃/min is warming up to 350-400 ℃, and control pressure is 10-20MPa, insulation 30min, then with the pressure release of 0.3-0.6MPa/min speed, finally with nitrogen purging 5-15min.
10. the preparation method of aerogel composite according to claim 9, is characterized in that, described heat-up rate is 6-8 ℃/min.
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