CN106395873A - Preparation method of ultra-light blocky aluminum oxide aerogel - Google Patents
Preparation method of ultra-light blocky aluminum oxide aerogel Download PDFInfo
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- CN106395873A CN106395873A CN201610856015.7A CN201610856015A CN106395873A CN 106395873 A CN106395873 A CN 106395873A CN 201610856015 A CN201610856015 A CN 201610856015A CN 106395873 A CN106395873 A CN 106395873A
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- ultralight
- graphene oxide
- dehydrated alcohol
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
Abstract
The invention discloses a preparation method of ultra-light blocky aluminum oxide aerogel. Graphene oxide is doped in a process of preparing the graphene oxide by a sol-gel method; then, the graphene oxide is removed through roasting; the ultra-light aluminum oxide aerogel with good block degree can be obtained. After the aluminum oxide aerogel prepared by the method is roasted at 500 DEG C, the specific surface area can still reach up to 444m<2>/g, and the density is lowered to 0.151g/cm<3>. The synthetic method has great reference value for industrially producing the ultra-light blocky aluminum oxide aerogel in a large scale; meanwhile, great significance is realized for promoting the practical application of the aluminum oxide aerogel.
Description
Technical field
The present invention relates to inorganic oxide aerogel preparation field, the system of specifically a kind of ultralight lump alumina aerogel
Preparation Method.
Background technology
Aeroge is a kind of nanoporous network structure mutually assembling composition with ultramicron or high-polymer molecular, and
It is full of a kind of high dispersive solid material of gaseous state disperse medium in hole, its porosity may be up to 99.8%, and pore-size distribution exists
Nanometer scale (1nm～100nm).It is condensed state material the lightest in the world, and density can as little as 0.002g/cm3, by people's shape
Referred to as " the solid-state cigarette " of elephant；It is the current best solid material of heat-proof quality in the world, room temperature in vacuo thermal conductivity can be as little as
0.001W/(m·K).In addition, also having much excellent characteristic, such as low coefficient of refraction, low electrical conductivity, in a low voice spread speed,
Fireclay insulating refractory, catalyst and catalyst carrier, silencing and damping material, novel high-energy particle detector, gas and water net
The aspects such as agent, special glass presoma have boundless application prospect.Basic research about aeroge and application are ground
Study carefully the extensive concern being increasingly subject to Chinese scholars, the aeroge application possessing unique excellent properties is more and more extensive, becomes
Study hotspot in current Material Field.In numerous aeroges, Al2O3Aeroge thermal conductivity low (30 DEG C, 1 atmospheric pressure intermittent fever
The coefficient of conductivity be only 0.029W/ (m K), 400 DEG C, 1 atmospheric pressure when the coefficient of heat conduction be only 0.098W/ (m K), 800 DEG C,
During 1 atmospheric pressure, the coefficient of heat conduction is 0.298W/ (m K), is preferable high temperature insulating material.Due to Al2O3The height of aeroge
Warm stability is superior compared with aerosil, as high temperature insulating material and excellent catalyst and catalyst carrier side
Face has obtained wider concern.Al2O3Aeroge is because having superpower resistance to elevated temperatures (being resistant to 2000 DEG C of high temperature), efficiently
Catalytic performance and absorption property etc., become the splendid candidate material of heat-barrier material, high temperature catalyst and its carrier.
However, it is poor to prepare alumina aerogels big lumpy degree at this stage, easily rupturable and density is larger, these defects
Limit it to be widely applied.Although can solve these defects using supercritical drying, the difficult control of its condition, to equipment requirements
High, operating difficultiess, and time-consuming, dangerous height, efficiency are low, significantly limit the large-scale production of aeroge.Therefore,
Finding a kind of drying meanss simple to operate, low cost and obtaining the alumina aerogels that block degree is good, density is extremely low becomes present
The focus of research.
Content of the invention
It is an object of the invention to provide a kind of preparation method of ultralight lump alumina aerogel, to solve in prior art
Preparation alumina aerogels density big, specific surface area is little, easily rupturable the problems such as.
For achieving the above object, the technical solution used in the present invention is：
A kind of preparation method of ultralight lump alumina aerogel, comprises the steps：
Step one, take graphene oxide, be added in deionized water, in being cleaned by ultrasonic instrument ultrasonic to being completely dissolved, obtain
To graphene oxide solution；
Step 2, take dehydrated alcohol, be subsequently adding in the graphene oxide solution that step one obtains and be warming up to design temperature,
Add aluminum soluble salt, react at a set temperature；
Step 3, treat in step 2 that reaction finishes and be cooled to room temperature that Deca epoxide under the conditions of ice-water bath drips
Proceed to standing in 40 DEG C of thermostatic drying chambers after finishing and form gel；
Add dehydrated alcohol fluid-tight after forming gel in step 4, step 3, put into aging a couple of days in thermostatic drying chamber, often
24h replaces a dehydrated alcohol；
Step 5, the wet gel of end aging in step 4 is dried, then by dried sample roasting, that is, obtains ultralight
Lump alumina aerogel.
In the graphene oxide solution of step one, the concentration of graphene oxide is 0.05-5.00mg/ml.
In step 2, dehydrated alcohol is 0.1-9 with the volume ratio of graphene oxide solution.
In step 2, described aluminum soluble salt is Aluminium chloride hexahydrate, ANN aluminium nitrate nonahydrate or Patent alum
A kind of.
In step 2, described aluminum soluble salt is 400-1000 with the mass ratio of contained graphene oxide in step one.
In step 3, described epoxide is oxirane, expoxy propane or epoxychloropropane.
In step 5, the drying meanss of employing are constant pressure and dry, vacuum drying or supercritical drying.
Beneficial effect：The preparation method of the ultralight lump alumina aerogel that the present invention provides, by sol-gel legal system
Graphene oxide is mixed, simple to operate, effect substantially, contrasts unadulterated aeroge, gas during standby alumina aerogels
Gel density is by 0.933g/cm3It is reduced to 0.151g/cm3, and in aging not easy to crack with dry run, experiment discovery doping
Graphene oxide can effectively reduce contraction in ageing process and dry run for the wet gel, and roasting removes graphene oxide
The mechanical strength of sample strengthens afterwards.
Brief description
Fig. 1 is the alumina aerogels obtaining after roasting after drying.
Specific embodiment
With reference to embodiment, the present invention is done and further explain.The following example is merely to illustrate the present invention, but
It is not used to limit the practical range of the present invention.
A kind of preparation method of ultralight lump alumina aerogel, with Aluminium chloride hexahydrate as raw material, using sol-gel
Method mixes graphene oxide during preparing alumina aerogels, leads to after the composite alumina aeroge sample obtaining doping again
Cross roasting to go out graphene oxide therein, that is, obtain ultralight lump alumina aerogel, specifically include following steps：
Step one, take by modified Hummer method preparation graphene oxide, be added in deionized water, be cleaned by ultrasonic instrument
In ultrasonic obtain graphene oxide solution to being completely dissolved, the concentration of graphene oxide is 0.05-5.00mg/ml；
Step 2, take dehydrated alcohol, be subsequently adding the graphene oxide solution that step one obtains, be warming up to design temperature,
Add aluminum soluble salt, react at a set temperature；
Wherein, dehydrated alcohol and the volume ratio of graphene oxide solution are 0.1-9；
Aluminum soluble salt is one kind of Aluminium chloride hexahydrate, ANN aluminium nitrate nonahydrate or Patent alum；
Aluminum soluble salt is 400-1000 with the mass ratio of contained graphene oxide in step one；
Step 3, treat in step 2 that reaction finishes and be cooled to room temperature that Deca epoxide under the conditions of ice-water bath drips
Proceed to standing in 40 DEG C of thermostatic drying chambers after finishing and form gel；
Wherein, epoxide is oxirane, expoxy propane or epoxychloropropane；
Add dehydrated alcohol fluid-tight after forming gel in step 4, step 3, put into aging a couple of days in thermostatic drying chamber, often
24h replaces a dehydrated alcohol；
Step 5, the wet gel of end aging in step 4 is dried, then the roasting one at 500 DEG C by dried sample
The section time obtains alumina aerogels ultralight, that block degree is good；
Wherein, the drying meanss of employing are constant pressure and dry, vacuum drying or supercritical drying.
Graphene oxide used in the present invention is to be prepared using modified Hummer method, and its preparation method is as follows：
The preparation of graphene oxide：Weigh 5g natural flake graphite and 2.5g sodium nitrate is added in 130ml concentrated sulphuric acid,
2h is stirred, this stage is pre-oxidizing the stage under condition of ice bath；After pre-oxidation finishes, it is slowly added to the potassium permanganate of 15g, and in ice
Continue reaction 2h, this stage is the low-temp reaction stage under the conditions of bath；Remove ice bath, above-mentioned reactant is transferred to 35 DEG C of water-baths
In, continue reaction 1h, this stage is the middle temperature stage of reaction；It is slowly added to 230mL deionized water in above-mentioned reaction system, subsequently
It is warming up to 98 DEG C, and reacts 30min at such a temperature, this stage is the pyroreaction stage；After the pyroreaction stage terminates, add
400ml deionized water and 10ml hydrogen peroxide, and stir 1h, reaction terminates.After graphite oxide preparation finishes, by centrifuge washing
Mode remove foreign ion therein, such as potassium ion, manganese ion and sulfate ion.After washing finishes, will be obtained
Graphite oxide slurry carry out forced air drying under the conditions of 60 DEG C, standby.
Embodiment 1
Step one, take the oxidized graphite flake that 0.1g prepared by modified Hummer method, be added in 100ml deionized water,
Be cleaned by ultrasonic instrument in ultrasonic to being completely dissolved, obtain concentration be 1mg/ml graphene oxide solution；
Step 2, take the dehydrated alcohol of 40ml, be subsequently adding the graphene oxide solution that 40ml step one obtains, be warming up to
80 DEG C, add the Aluminium chloride hexahydrate of 24.143g, react 2h at 80 DEG C；
Step 3, treat in step 2 that reaction finishes and be cooled to room temperature that Deca 70mL expoxy propane under the conditions of ice-water bath drips
Add and after finishing, proceed to standing formation gel in 40 DEG C of thermostatic drying chambers；
Add dehydrated alcohol fluid-tight after forming gel in step 4, step 3, put into aging 3-4 in 40 DEG C of thermostatic drying chambers
My god, every 24h replaces a dehydrated alcohol；
Step 5, the drying in 60 DEG C of vacuum drying ovens by the wet gel of end aging in step 4, then will be dried
Sample roasting 4h at 500 DEG C obtains alumina aerogels ultralight, that block degree is good.
Embodiment 2
Step one, take the oxidized graphite flake that 0.15g prepared by modified Hummer method, be added in 100ml deionized water,
Be cleaned by ultrasonic instrument in ultrasonic to being completely dissolved, obtain concentration be 1.5mg/ml graphene oxide solution；
Step 2, take the dehydrated alcohol of 30ml, be subsequently adding the graphene oxide solution that 50ml step one obtains, be warming up to
80 DEG C, add the ANN aluminium nitrate nonahydrate of 24g, react 2h at 80 DEG C；
Step 3, treat in step 2 that reaction finishes and be cooled to room temperature that Deca 70ml oxirane under the conditions of ice-water bath drips
Add and after finishing, proceed to standing formation gel in 40 DEG C of thermostatic drying chambers；
Add dehydrated alcohol fluid-tight after forming gel in step 4, step 3, put into aging 3-4 in 40 DEG C of thermostatic drying chambers
My god, every 24h replaces a dehydrated alcohol；
Step 5, by the wet gel constant pressure and dry of end aging in step 4, more dried sample is roasted at 500 DEG C
Burn 4h and obtain alumina aerogels ultralight, that block degree is good.
Embodiment 3
Step one, take the oxidized graphite flake that 0.1g prepared by modified Hummer method, be added in 100ml deionized water,
Be cleaned by ultrasonic instrument in ultrasonic to being completely dissolved, obtain concentration be 1mg/ml graphene oxide solution；
Step 2, take the dehydrated alcohol of 50ml, be subsequently adding the graphene oxide solution that 30ml step one obtains, be warming up to
80 DEG C, add the Aluminium chloride hexahydrate of 24.143g, react 2h at 80 DEG C；
Step 3, treat in step 2 that reaction finishes and be cooled to room temperature that Deca 70ml oxirane under the conditions of ice-water bath drips
Add and after finishing, proceed to standing formation gel in 40 DEG C of thermostatic drying chambers；
Add dehydrated alcohol fluid-tight after forming gel in step 4, step 3, put into aging 3-4 in 40 DEG C of thermostatic drying chambers
My god, every 24h replaces a dehydrated alcohol；
Step 5, the wet gel of end aging in step 4 is adopted supercritical drying, then by dried sample 500
At DEG C, roasting 4h obtains alumina aerogels ultralight, that block degree is good.
Embodiment 4
Step one, take the oxidized graphite flake that 0.05g prepared by modified Hummer method, be added in 100ml deionized water,
Be cleaned by ultrasonic instrument in ultrasonic to being completely dissolved, obtain concentration be 0.5mg/ml graphene oxide solution；
Step 2, take the dehydrated alcohol of 40ml, be subsequently adding the graphene oxide solution that 40ml step one obtains, be warming up to
80 DEG C, add the Aluminium chloride hexahydrate of 24.143g, react 2h at 80 DEG C；
Step 3, treat in step 2 that reaction finishes and be cooled to room temperature, Deca 70ml epoxychloropropane under the conditions of ice-water bath,
Proceed to standing in 40 DEG C of thermostatic drying chambers after completion of dropping and form gel；
Add dehydrated alcohol fluid-tight after forming gel in step 4, step 3, put into aging 3-4 in 40 DEG C of thermostatic drying chambers
My god, every 24h replaces a dehydrated alcohol；
Step 5, the drying in 60 DEG C of vacuum drying ovens by the wet gel of end aging in step 4, then will be dried
Sample roasting 4h at 500 DEG C obtains alumina aerogels ultralight, that block degree is good.
Comparative example 1
Step one, take the oxidized graphite flake that 0.1g prepared by modified Hummer method, be added in 100ml deionized water,
Be cleaned by ultrasonic instrument in ultrasonic obtain the graphene oxide solution of concentration 1mg/ml to being completely dissolved, with acidometer measure oxidation stone
The pH of black alkene solution；
Step 2, take the dehydrated alcohol of 40ml, be subsequently adding 40ml deionized water, adjust pH and step one with dilute hydrochloric acid
The graphene oxide solution arriving is identical, is warming up to 80 DEG C, adds the Aluminium chloride hexahydrate of 24.143g, reacts 2h at 80 DEG C；
Step 3, treat in step 2 that reaction finishes and be cooled to room temperature that Deca 70ml expoxy propane under the conditions of ice-water bath drips
Add and after finishing, proceed to standing formation gel in 40 DEG C of thermostatic drying chambers；
Add dehydrated alcohol fluid-tight after forming gel in step 4, step 3, put into aging 3-4 in 40 DEG C of thermostatic drying chambers
My god, every 24h replaces a dehydrated alcohol；
Step 5, the drying in 60 DEG C of vacuum drying ovens by the wet gel of end aging in step 4, then will be dried
Sample roasting 4h at 500 DEG C obtains alumina aerogels ultralight, that block degree is good.
Fig. 1 is the alumina aerogels obtaining after roasting after drying, the Al being respectively obtained by comparative example 12O3Gas
Gel sample (left)；The Al that the composite aerogel sample being obtained by embodiment 1 obtains after roasting2O3Aeroge sample (right).
Can slowly shrink so that volume can diminish with gel in dry run aging, contrast two figures can be seen that airsetting after compound GO
Colloid amass big, that is, shrink little, the density of rough calculation aeroge is by 0.933g/cm3It is reduced to 0.151g/cm3, and block
Shape degree improves, and illustrates that compound GO prepares ultralight bulk Al2O3The method of aeroge is feasible, and effect is obvious.
The above be only the preferred embodiment of the present invention it should be pointed out that：Ordinary skill people for the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (7)
1. a kind of preparation method of ultralight lump alumina aerogel it is characterised in that：Comprise the steps：
Step one, take graphene oxide, be added in deionized water, in being cleaned by ultrasonic instrument ultrasonic to being completely dissolved, obtain oxygen
Graphite alkene solution；
Step 2, take dehydrated alcohol, be subsequently adding in the graphene oxide solution that step one obtains and be warming up to design temperature, then plus
Enter aluminum soluble salt, react at a set temperature；
Step 3, treat in step 2 that reaction finishes and be cooled to room temperature, Deca epoxide under the conditions of ice-water bath, after completion of dropping
Proceed to standing in 40 DEG C of thermostatic drying chambers and form gel；
Add dehydrated alcohol fluid-tight after forming gel in step 4, step 3, put into aging a couple of days in thermostatic drying chamber, every 24h
Replace a dehydrated alcohol；
Step 5, the wet gel of end aging in step 4 is dried, then by dried sample roasting, that is, obtains ultralight bulk
Alumina aerogels.
2. ultralight lump alumina aerogel according to claim 1 preparation method it is characterised in that：The oxygen of step one
In graphite alkene solution, the concentration of graphene oxide is 0.05-5.00mg/ml.
3. ultralight lump alumina aerogel according to claim 1 preparation method it is characterised in that：In step 2,
Dehydrated alcohol is 0.1-9 with the volume ratio of graphene oxide solution.
4. ultralight lump alumina aerogel according to claim 1 preparation method it is characterised in that：In step 2,
Described aluminum soluble salt is one kind of Aluminium chloride hexahydrate, ANN aluminium nitrate nonahydrate or Patent alum.
5. the ultralight lump alumina aerogel according to claim 1 or 4 preparation method it is characterised in that：Step 2
In, described aluminum soluble salt is 400-1000 with the mass ratio of contained graphene oxide in step one.
6. ultralight lump alumina aerogel according to claim 1 preparation method it is characterised in that：In step 3,
Described epoxide is oxirane, expoxy propane or epoxychloropropane.
7. ultralight lump alumina aerogel according to claim 1 preparation method it is characterised in that：In step 5,
Using drying meanss be constant pressure and dry, vacuum drying or supercritical drying.
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Cited By (3)
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| CN113480875A (en) * | 2021-07-27 | 2021-10-08 | 雷索新材料(苏州)有限公司 | Aluminum oxide modified graphene, graphene heat dissipation coating and preparation method thereof |
| CN113717718A (en) * | 2021-08-10 | 2021-11-30 | 常州大学 | Preparation method and application of terbium ion-doped three-dimensional porous-structure alumina aerogel fluorescent powder |
| CN113754462A (en) * | 2021-08-30 | 2021-12-07 | 常州大学 | Preparation of ultralight Cr capable of being rapidly cooled2O3-Al2O3Method for producing ceramic aerogels |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113754462A (en) * | 2021-08-30 | 2021-12-07 | 常州大学 | Preparation of ultralight Cr capable of being rapidly cooled2O3-Al2O3Method for producing ceramic aerogels |
| CN113754462B (en) * | 2021-08-30 | 2022-07-26 | 常州大学 | Preparation of ultralight Cr capable of being rapidly cooled 2 O 3 -Al 2 O 3 Method for producing ceramic aerogels |
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