CN104961135A - Preparation method of silicon dioxide aerogel - Google Patents
Preparation method of silicon dioxide aerogel Download PDFInfo
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- CN104961135A CN104961135A CN201510376342.8A CN201510376342A CN104961135A CN 104961135 A CN104961135 A CN 104961135A CN 201510376342 A CN201510376342 A CN 201510376342A CN 104961135 A CN104961135 A CN 104961135A
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Abstract
The invention provides a preparation method of silicon dioxide aerogel, which can reduce the cost and prolong the service life of equipment. The preparation method comprises the following steps: (1) preparing sol; (2) gelatinizing silicon sol; (3) alcoholizing; (4) carrying out the surface hydrophobic modification; (5) drying at the normal pressure. According to the preparation method of the silicon dioxide aerogel, industrial waste slag-coal powder which is low in price and rich in resource is used as a raw material to substitute an organic silicon source high in price, so that the application cost is greatly reduced; the normal-pressure drying substitutes the supercritical drying, so that on one hand, the requirement of the entire process on the equipment is greatly lowered, the safety performance is greatly improved, and on the other hand, the operation cost is greatly reduced; moreover, the corrosion to the equipment is reduced, the requirement on the equipment is greatly lowered, the water washing is not needed, the energy consumption is reduced, the water resource is saved, and more energy conservation and environmental protection can be realized.
Description
Technical field
The present invention relates to one, especially a kind of preparation method of aerosil.
Background technology
Aerosil is the porous material of a kind of low density, high-specific surface area, lower thermal conductivity, there is continuous print network structure, pore size and particle diameter range are all at Nano grade, aerosil has unique mechanics, calorifics, optics, acoustical behavior, therefore has broad application prospects in heat preserving and insulating material, field of photocatalytic material.
For obtaining the aerosil of vesicular structure, the method of current employing is mainly silicon source with tetraethoxy, obtain by sol-gel and supercritical process, this preparation method also exists the problems such as raw materials cost is high, complex process, danger are large, restricts its large-scale industrial production and the use in all fields.
China is coal production state maximum in the world and country of consumption, the output of industrial flyash is huge, and quantum of output is on the increase, increasing seems to the research and development of the comprehensive utilization of flyash and exploitation and becomes more and more important, utilize coal ash for manufacturing significant for high value-added product, while solution environmental pollution, more turn waste into wealth, improve the utility value of flyash.The main component of flyash is the oxide compounds such as silicon, aluminum oxide and a small amount of calcium, iron, and wherein the content of silicon oxide can reach more than 30%, therefore can provide silicon source, as the main raw preparing aerosil.But the aerogel foreign matter content that existing flyash is prepared is larger, there is no the foreign ion in good method removing gel, and gel-strength is not enough, be not enough to prepare satisfactory aerogel particle, the aerogel of preparation is more not enough to the application meeting other field.
A kind of existing method taking flyash as Feedstock Atmospheric drying and prepare silicon-aluminium aerogel, its preparation process is as follows: 1, prepare silicon-aluminum sol, by flyash: sodium carbonate be 1:2-2: 1 mass ratio get flyash and sodium carbonate, after combined grinding, at the temperature of 830 DEG C-1000 DEG C, be incubated calcining 60min-120min, obtain sintered material; In every 5Kg sintered material add 5-30L hydrochloric acid ratio, by sintered material and mixed in hydrochloric acid, stirring reaction 30-100min at the temperature of room temperature-60 DEG C, the concentration of described hydrochloric acid soln is 3mol/L-8mol/L, again by reacted material suction filtration, by filtrate with salt acid for adjusting pH value to 2-10, i.e. obtained silicon-aluminum sol; 2, silicon-aluminum sol gelation: silicon-aluminum sol leaves standstill 2h-240h (hour), forms silica-alumina gel at the temperature of room temperature-60 DEG C, then at the temperature of room temperature-60 DEG C aging 10h-90h, namely obtained aging after silica-alumina gel; 3, dechlorinate: with flowing water soak aging after silica-alumina gel, remove aging after silicon-aluminum sol in the chlorion that contains, soaking temperature lower than 50 DEG C, soak time 5h-48h, the silica-alumina gel after obtained aging dechlorination; 4, solvent replacing: with the silica-alumina gel after the aging dechlorination of solvent soaked in absolute ethyl alcohol, to displace the water in the silica-alumina gel after aging dechlorination, soaking temperature is room temperature-60 DEG C, soaking number of times is 1-20 time, each soak time is 2h-50h, during each immersion, the volumetric usage of solvent dehydrated alcohol is 1-5 times, the rear elimination solvent dehydrated alcohol of immersion of the silica-alumina gel volume after aging dechlorination, the silica-alumina gel after obtained solvent replacing; 5, surface hydrophobicity process: the surface hydrophobicity agent silicoorganic compound mixing of the silica-alumina gel after solvent replacing is soaked, 10h-120h is soaked at the temperature of 40 DEG C-150 DEG C, soaking number of times is 1-20 times, each volume ratio 0.2-2:1 of silica-alumina gel when soaking after silicoorganic compound and solvent replacing, elimination silicoorganic compound after soaking, to carry out surface hydrophobicity modification; 6, constant pressure and dry: by the constant pressure and dry 2h-10h at the temperature of 40-150 DEG C of the silica-alumina gel after surface hydrophobicity process, obtained product silicon-aluminium aerogel.
The shortcoming of above-mentioned preparation method is as follows:
1, the technical program experimental installation requires high, and have corrodibility to container, need dechlorinate, the operating time is long, and needs a large amount of flowing waters except in chlorine process, adds energy consumption, wastes resource.
2, in the technical program, in flyash, other foreign ions can not be removed, and gel is impure.
3, the aerogel gel content prepared of the technical program is low, and gel-strength is not enough, and aerogel particle specific surface area is little, poor-performing.
4, the technical program preparation time is long, and realizability is poor.
Summary of the invention
The invention provides a kind ofly to reduce costs, the preparation method of the aerosil that increases service life of equipment.
Realize the preparation method of the aerosil of the object of the invention, comprise the steps:
(1) colloidal sol is prepared
Get flyash or coal gangue, mix with carbonate, then carry out mechanical disintegration, carry out insulation calcining, obtain calcinate;
Add sulphuric acid soln toward calcined material, calcined material is mixed with sulphuric acid soln, reacts at ambient temperature, the material of reaction is carried out suction filtration, obtains filtrate;
(2) silica sol gel
Silicon sol is left standstill under water-bath and forms Silica hydrogel, then aging under water-bath, the Silica hydrogel after obtained aging;
(3) refine
Silica hydrogel after aging is mixed with ethanolic soln, then leaves standstill under water-bath;
(4) surface hydrophobicity modification
Silica hydrogel surface hydrophobicity agent organic silicon solution step (3) obtained soaks;
(5) constant pressure and dry
Silica hydrogel after surface hydrophobicity process is carried out constant pressure and dry, obtained product---aerosil.
In described step (1), flyash or coal gangue, be 1:0.3 ~ 1:0.6 with the mass ratio of carbonate; Described carbonate is sodium carbonate, salt of wormwood or calcium carbonate.
The calcining temperature of described step (1) is more than 870 DEG C, and insulation calcination time is 240min ~ 300min, obtains calcinate;
Add the ratio of 10L ~ 30L sulphuric acid soln in described step (1) in every 1Kg calcined material, calcined material mixed with sulphuric acid soln, react 10min ~ 20min at ambient temperature, described sulfuric acid concentration is 2mol/l ~ 5mol/l; Described alkaline solution can be sodium hydroxide solution or water glass solution.
In described step (1), filtrate is processed by decationizing exchange resin,
In described step (1), by the filtrate after the process of decationizing exchange resin, regulate pH value to 4 ~ 6 or 8 ~ 10 by alkaline solution.
Described step (2), by silicon sol under the water-bath of 50 DEG C ~ 80 DEG C leave standstill 0.2h ~ 2h, formed Silica hydrogel, then aging 2h ~ 24h under the water-bath of 50 DEG C ~ 80 DEG C, can obtain aging after Silica hydrogel.
Described step (3), mixes by every 1kg Silica hydrogel 2L ~ 3L ethanolic soln, under 50 DEG C ~ 80 DEG C water-baths, leave standstill 2h ~ 12h.
In the middle ethanolic soln of described step (3), add sulfuric acid or phosphoric acid, the weight ratio of described ethanol and sulfuric acid or phosphoric acid is 2:1 ~ 8:1.
In described step (4), Silica hydrogel is soaked 4h ~ 12h at the temperature of 40 DEG C ~ 80 DEG C, the volume ratio 2:1 ~ 5:1 of organic silicon solution and Silica hydrogel during immersion; Described organic silicon solution needs hydrofluoric acid to carry out activity activator.
In described step (5), by the constant pressure and dry 0.5h ~ 5h at the temperature of 60 ~ 100 DEG C of the Silica hydrogel after surface hydrophobicity process, obtained product---aerosil.
The beneficial effect of the preparation method of aerosil of the present invention is as follows:
The preparation method of aerosil of the present invention, utilizes cheapness, resourceful industrial residue---flyash is raw material, replace expensive organosilicon source, cost is reduced greatly; Constant pressure and dry replaces supercritical drying, make on the one hand that the requirement of whole technique to equipment reduces greatly, safety performance promotes greatly, also running cost is made greatly to decline on the other hand, The present invention reduces the corrodibility to equipment simultaneously, the requirement of equipment is reduced greatly, without the need to washing, reduces energy consumption, save water resources, more energy-conserving and environment-protective.
Accompanying drawing explanation
Fig. 1 is the schema of the preparation method of aerosil of the present invention.
Embodiment
As shown in Figure 1, the preparation method of aerosil of the present invention, comprises the steps:
(1) colloidal sol is prepared
By flyash (or coal gangue): the mass ratio that sodium carbonate (or calcium carbonate, salt of wormwood) is 1:0.3 ~ 1:0.6 gets flyash and sodium carbonate, mechanical disintegration after mixing, at temperature more than 870 DEG C, insulation calcining 240min ~ 300min, obtains calcinate;
The ratio of 10L ~ 30L sulphuric acid soln is added in every 1Kg calcined material, calcined material is mixed with sulphuric acid soln, react 10min ~ 20min at ambient temperature, described sulfuric acid concentration is 2mol/l ~ 5mol/l, the material of reaction is carried out suction filtration, obtains filtrate, filtrate is processed by decationizing exchange resin, gained solution regulates pH value to 4 ~ 6 or 8 ~ 10 by alkaline solution, and can obtain silicon sol, described alkaline solution also can be water glass solution for sodium hydroxide solution.
2. silica sol gel
By silicon sol under the water-bath of 50 DEG C ~ 80 DEG C leave standstill 0.2h ~ 2h, formed Silica hydrogel, then aging 2h ~ 24h under the water-bath of 50 DEG C ~ 80 DEG C, can obtain aging after Silica hydrogel.
3. acid alcohol
By the mixed solution of every 1kg wet gel 2L ~ 3L ethanol and sulfuric acid, the ratio of ethanol and sulfuric acid is 2:1 ~ 8:1, under 50 DEG C ~ 80 DEG C water-baths, leave standstill 2h ~ 12h, and this stage main purpose reduces the moisture in gel, strengthens the intensity of gel.
4. surface hydrophobicity modification
Silica hydrogel after solvent replacing surface hydrophobicity agent organic silicon solution is soaked, at the temperature of 40 DEG C ~ 80 DEG C, soaks 4h ~ 12h, the volume ratio 2:1 ~ 5:1 of silica-alumina gel during immersion after organic silicon solution and solvent replacing; Organic silicon solution used needs hydrofluoric acid to carry out activity activator.
5. constant pressure and dry
By the constant pressure and dry 0.5h ~ 5h at the temperature of 60 ~ 100 DEG C of the Silica hydrogel after surface hydrophobicity process, obtained product---aerosil.
The preparation method of aerosil of the present invention, substitutes hydrochloric acid by sulfuric acid and calcined material is reacted, and not chloride ion-containing in reaction solution, reduces the corrosion to steel container, without the need to dechlorination, reduce energy consumption, economize on resources, reduce requirement to equipment, thus reduce old, extension device work-ing life.
The preparation method of aerosil of the present invention, carries out process by decationizing exchange resin to colloidal sol and removes other foreign ions in colloidal sol thus obtain highly purified aerosil.
The preparation method of aerosil of the present invention, regulates pH value by alkaline solution titration, thus increases the intensity of gel, and when pH value is 4 ~ 6, when 8 ~ 10, gel state is best.
The preparation method of aerosil of the present invention, carries out solvent exchange by the mixed solution of ethanol and sulfuric acid or phosphoric acid to gel, strengthens gel internal structure, thus strengthens the intensity of gel, the ratio 3:1 of ethanol and sulfuric acid or phosphoric acid, and during 4:1, state is best.
The preparation method of aerosil of the present invention, surface hydrophobicity agent is mainly trimethylchlorosilane and cyclohexane mixtures, hexamethyldisiloxane, the silane coupling agents such as hexamethyldisilazane, before using, activity activator is carried out to it, can modified effect be improved, shorten modification time, the porosity of gained aerosil is high, pore size distribution is more even, and quality product is more excellent, and production efficiency is higher simultaneously.
The preparation method of aerosil of the present invention, utilizes cheapness, resourceful industrial residue---flyash is raw material, replace expensive organosilicon source, cost is reduced greatly; Constant pressure and dry replaces supercritical drying, make on the one hand that the requirement of whole technique to equipment reduces greatly, safety performance promotes greatly, also running cost is made greatly to decline on the other hand, The present invention reduces the corrodibility to equipment simultaneously, the requirement of equipment is reduced greatly, without the need to washing, reduces energy consumption, save water resources, more energy-conserving and environment-protective;
Aerosil prepared by the present invention, through performance test, specific surface area can reach 700m
2about/g, contained aperture is nano level, and porosity can reach 99.9%, pore size distribution range 15-25nm, mean pore size 16-18nm, and can control aerogel said structure parameter as required; Have excellent mechanical properties and low heat conductivity, will be widely used in heat preserving and insulating material field prospect.
Embodiment 1:
The preparation method of aerosil of the present invention, comprises the steps:
(1) colloidal sol is prepared
By flyash: sodium carbonate is that the mass ratio of 1:0.3 gets flyash and sodium carbonate, mechanical disintegration after mixing, at the temperature more than 870 DEG C, insulation calcining 240min, obtains calcinate;
The ratio of 10L sulphuric acid soln is added in every 1Kg calcined material, calcined material is mixed with sulphuric acid soln, react 10min at ambient temperature, described sulfuric acid concentration is 2mol/l, the material of reaction is carried out suction filtration, obtains filtrate, filtrate is processed by decationizing exchange resin, gained solution regulates pH value to 4 by alkaline solution, and can obtain silicon sol, described alkaline solution also can be water glass solution for sodium hydroxide solution.
2. silica sol gel
By silicon sol under the water-bath of 50 DEG C leave standstill 0.2h, formed Silica hydrogel, then aging 2h under the water-bath of 50 DEG C, can obtain aging after Silica hydrogel.
3. acid alcohol
By the mixed solution of every 1kg wet gel 2L ethanol and sulfuric acid, the ratio of ethanol and sulfuric acid is 2:1, under 50 DEG C of water-baths, leave standstill 2h, and this stage main purpose reduces the moisture in gel, strengthens the intensity of gel.
4. surface hydrophobicity modification
Silica hydrogel after solvent replacing surface hydrophobicity agent organic silicon solution is soaked, at the temperature of 40 DEG C, soaks 4h, the volume ratio 2:1 of silica-alumina gel during immersion after organic silicon solution and solvent replacing; Organic silicon solution used needs hydrofluoric acid to carry out activity activator.
5. constant pressure and dry
By the constant pressure and dry 0.5h at the temperature of 60 DEG C of the Silica hydrogel after surface hydrophobicity process, obtained product---aerosil.
Embodiment 2:
The preparation method of aerosil of the present invention, comprises the steps:
(1) colloidal sol is prepared
By coal gangue: calcium carbonate is that the mass ratio of 1:0.4 gets coal gangue and calcium carbonate, mechanical disintegration after mixing, at the temperature more than 870 DEG C, insulation calcining 260min, obtains calcinate;
The ratio of 20L sulphuric acid soln is added in every 1Kg calcined material, calcined material is mixed with sulphuric acid soln, react 15min at ambient temperature, described sulfuric acid concentration is 4mol/l, the material of reaction is carried out suction filtration, obtains filtrate, filtrate is processed by decationizing exchange resin, gained solution regulates pH value to 6 by alkaline solution, and can obtain silicon sol, described alkaline solution also can be water glass solution for sodium hydroxide solution.
2. silica sol gel
By silicon sol under the water-bath of 60 DEG C leave standstill 1h, formed Silica hydrogel, then aging 10h under the water-bath of 70 DEG C, can obtain aging after Silica hydrogel.
3. acid alcohol
By the mixed solution of every 1kg wet gel 2.5L ethanol and sulfuric acid, the ratio of ethanol and sulfuric acid is 5:1, under 65 DEG C of water-baths, leave standstill 6h, and this stage main purpose reduces the moisture in gel, strengthens the intensity of gel.
4. surface hydrophobicity modification
Silica hydrogel after solvent replacing surface hydrophobicity agent organic silicon solution is soaked, at the temperature of 60 DEG C, soaks 8h, the volume ratio 4:1 of silica-alumina gel during immersion after organic silicon solution and solvent replacing; Organic silicon solution used needs hydrofluoric acid to carry out activity activator.
5. constant pressure and dry
By the constant pressure and dry 3h at the temperature of 80 DEG C of the Silica hydrogel after surface hydrophobicity process, obtained product---aerosil.
Embodiment 3:
The preparation method of aerosil of the present invention, comprises the steps:
(1) colloidal sol is prepared
By flyash: salt of wormwood) get flyash and salt of wormwood for the mass ratio of 1:0.6, mechanical disintegration after mixing, at the temperature more than 870 DEG C, 300min is calcined in insulation, obtains calcinate;
The ratio of 30L sulphuric acid soln is added in every 1Kg calcined material, calcined material is mixed with sulphuric acid soln, react 20min at ambient temperature, described sulfuric acid concentration is 5mol/l, the material of reaction is carried out suction filtration, obtains filtrate, filtrate is processed by decationizing exchange resin, gained solution regulates pH value to 10 by alkaline solution, and can obtain silicon sol, described alkaline solution also can be water glass solution for sodium hydroxide solution.
2. silica sol gel
By silicon sol under the water-bath of 80 DEG C leave standstill 2h, formed Silica hydrogel, then aging 24h under the water-bath of 80 DEG C, can obtain aging after Silica hydrogel.
3. acid alcohol
By the mixed solution of every 1kg wet gel 3L ethanol and sulfuric acid, the ratio of ethanol and sulfuric acid is 8:1, under 80 DEG C of water-baths, leave standstill 12h, and this stage main purpose reduces the moisture in gel, strengthens the intensity of gel.
4. surface hydrophobicity modification
Silica hydrogel after solvent replacing surface hydrophobicity agent organic silicon solution is soaked, at the temperature of 80 DEG C, soaks 12h, the volume ratio 5:1 of silica-alumina gel during immersion after organic silicon solution and solvent replacing; Organic silicon solution used needs hydrofluoric acid to carry out activity activator.
5. constant pressure and dry
By the constant pressure and dry 5h at the temperature of 100 DEG C of the Silica hydrogel after surface hydrophobicity process, obtained product---aerosil.
Embodiment recited above is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; do not departing under the present invention designs spiritual prerequisite; the various distortion that the common engineering technical personnel in this area make technical solution of the present invention and improvement, all should fall in protection domain that claims of the present invention determine.
Claims (10)
1. a preparation method for aerosil, comprises the steps:
(1) colloidal sol is prepared:
Get flyash or coal gangue, mix with carbonate, then carry out mechanical disintegration, carry out insulation calcining, obtain calcinate;
Add sulphuric acid soln toward calcined material, calcined material is mixed with sulphuric acid soln, reacts at ambient temperature, the material of reaction is carried out suction filtration, obtains filtrate;
(2) silica sol gel:
Silicon sol is left standstill under water-bath and forms Silica hydrogel, then aging under water-bath, the Silica hydrogel after obtained aging;
(3) refine:
Silica hydrogel after aging is mixed with ethanolic soln, then leaves standstill under water-bath;
(4) surface hydrophobicity modification:
Silica hydrogel surface hydrophobicity agent organic silicon solution step (3) obtained soaks;
(5) constant pressure and dry:
Silica hydrogel after surface hydrophobicity process is carried out constant pressure and dry, obtained product---aerosil.
2. the preparation method of aerosil according to claim 1, is characterized in that: flyash or coal gangue in described step (1) are 1:0.3 ~ 1:0.6 with the mass ratio of carbonate; Described carbonate is sodium carbonate, salt of wormwood or calcium carbonate.
3. the preparation method of aerosil according to claim 1, is characterized in that: the calcining temperature of described step (1) is more than 870 DEG C, and insulation calcination time is 240min ~ 300min, obtains calcinate.
4. the preparation method of aerosil according to claim 1, it is characterized in that: the ratio adding 10L ~ 30L sulphuric acid soln in described step (1) in every 1Kg calcined material, calcined material is mixed with sulphuric acid soln, react 10min ~ 20min at ambient temperature, described sulfuric acid concentration is 2mol/l ~ 5mol/l; Described alkaline solution can be sodium hydroxide solution or water glass solution.
5., according to the preparation method of the arbitrary described aerosil of claim 1 ~ 4, it is characterized in that: in described step (1), filtrate is processed by decationizing exchange resin.
6. the preparation method of aerosil according to claim 5, is characterized in that: in described step (1), by the filtrate after the process of decationizing exchange resin, regulates pH value to 4 ~ 6 or 8 ~ 10 by alkaline solution.
7. the preparation method of aerosil according to claim 1, it is characterized in that: described step (2), silicon sol is left standstill 0.2h ~ 2h under the water-bath of 50 DEG C ~ 80 DEG C, form Silica hydrogel, then aging 2h ~ 24h under the water-bath of 50 DEG C ~ 80 DEG C, can obtain aging after Silica hydrogel.
8. the preparation method of aerosil according to claim 1, is characterized in that: described step (3), mixes by every 1kg Silica hydrogel 2L ~ 3L ethanolic soln, under 50 DEG C ~ 80 DEG C water-baths, leave standstill 2h ~ 12h.
9. the preparation method of the aerosil according to claim 1 or 8, is characterized in that: in the middle ethanolic soln of described step (3), add sulfuric acid or phosphoric acid, and the weight ratio of described ethanol and sulfuric acid or phosphoric acid is 2:1 ~ 8:1;
In described step (4), Silica hydrogel is soaked 4h ~ 12h at the temperature of 40 DEG C ~ 80 DEG C, the volume ratio 2:1 ~ 5:1 of organic silicon solution and Silica hydrogel during immersion;
In described step (5), by the constant pressure and dry 0.5h ~ 5h at the temperature of 60 ~ 100 DEG C of the Silica hydrogel after surface hydrophobicity process, obtained product---aerosil.
10. the preparation method of aerosil according to claim 1, is characterized in that: the organic silicon solution in described step (4) needs hydrofluoric acid to carry out activity activator before using.
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