CN106186035A - A kind of block La2o3siO2the preparation method of composite aerogel - Google Patents
A kind of block La2o3siO2the preparation method of composite aerogel Download PDFInfo
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- CN106186035A CN106186035A CN201610523827.XA CN201610523827A CN106186035A CN 106186035 A CN106186035 A CN 106186035A CN 201610523827 A CN201610523827 A CN 201610523827A CN 106186035 A CN106186035 A CN 106186035A
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- 239000004964 aerogel Substances 0.000 title claims abstract description 42
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 84
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 83
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 83
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 83
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 83
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 83
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000352 supercritical drying Methods 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 18
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 9
- 150000002603 lanthanum Chemical class 0.000 claims abstract description 8
- 230000002378 acidificating effect Effects 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 44
- 239000000203 mixture Substances 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims description 12
- 239000011240 wet gel Substances 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 238000006073 displacement reaction Methods 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229960004756 ethanol Drugs 0.000 claims description 4
- ZHIMWHGEMSAQBS-UHFFFAOYSA-N lanthanum sulfuric acid Chemical compound [La].S(O)(O)(=O)=O ZHIMWHGEMSAQBS-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- RLDBHKUGRPXFBF-UHFFFAOYSA-N lanthanum;hydrate Chemical compound O.[La] RLDBHKUGRPXFBF-UHFFFAOYSA-N 0.000 claims description 2
- 230000036571 hydration Effects 0.000 claims 1
- 238000006703 hydration reaction Methods 0.000 claims 1
- 150000002576 ketones Chemical class 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 239000011148 porous material Substances 0.000 abstract description 7
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 5
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 5
- 150000002910 rare earth metals Chemical class 0.000 abstract description 3
- 238000005352 clarification Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 15
- 230000032683 aging Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000499 gel Substances 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004965 Silica aerogel Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229960001422 aluminium chlorohydrate Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- LVYZJEPLMYTTGH-UHFFFAOYSA-H dialuminum chloride pentahydroxide dihydrate Chemical compound [Cl-].[Al+3].[OH-].[OH-].[Al+3].[OH-].[OH-].[OH-].O.O LVYZJEPLMYTTGH-UHFFFAOYSA-H 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000007783 nanoporous material Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- 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
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/16—Preparation of silica xerogels
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- 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
- C01P2006/12—Surface area
-
- 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
- C01P2006/16—Pore diameter
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Materials Engineering (AREA)
- Composite Materials (AREA)
- Dispersion Chemistry (AREA)
- Catalysts (AREA)
- Silicon Compounds (AREA)
Abstract
The present invention relates to a kind of block La2O3‑SiO2The preparation method of composite aerogel, by tetraethyl orthosilicate, hydrated inorganic lanthanum salt, acidic catalyst, deionized water, dehydrated alcohol are pressed certain mol proportion uniform stirring, ammonia regulation pH value in reaction, obtains the La of colourless clarification2O3‑SiO2Complex sol solution, then be statically placed in uniform temperature environment, wait gel.Finally utilize CO2Supercritical drying is dried process and obtains block La sample2O3‑SiO2Composite aerogel, this preparation process is simple to operation, the La prepared2O3‑SiO2Composite aerogel has the advantages such as uniform nano-pore structure, specific surface area is high, thermal conductivity is low, density is low, substantially increases pure SiO2Aeroge uses temperature.This not only had nanoporous aerogel structure but also possessed the La of characteristic of rare earth oxide2O3‑SiO2Composite aerogel will have more preferable application prospect in terms of high temperature insulating, heavy metal ion adsorbed, catalyst and catalyst carrier.
Description
Technical field
The invention belongs to the technical field that there is high-specific surface area, prepared by efficient absorption feature inorganic nano material, relate to
A kind of block La2O3-SiO2The preparation method of composite aerogel, especially with the block La of supercritical drying preparation2O3-SiO2Multiple
Close the preparation method of aeroge.
Background technology
Aeroge is mutually to be coalesced, by colloidal particle or high-polymer molecular, the one constituted to have three-dimensional manometer network structure,
It it is a kind of novel nano-porous materials.It has high specific surface area, high porosity, low-refraction, extremely-low density, superpower suction
The features such as attached property, so being all with a wide range of applications at aspects such as calorifics, optics, electricity, acoustics.In terms of calorifics, gas
The nanoporous network structure of gel can effectively suppress solid-phase thermal conduction and gaseous heat transfer, has the heat insulation characteristics of excellence, is
The solid-state material that thermal conductivity is minimum in the world at present, has wide answering in fields such as space flight and aviation, chemical industry metallurgical, energy saving buildings
Use prospect.
Research shows, rare earth element all obtains in fields such as oil, chemical industry, metallurgy, weaving, pottery, glass, permanent magnet materials
It is widely applied.The oxide of rare earth element has the spies such as high heat stability, strong heavy metal ion adsorbed property, high catalytic property
Point, but rare earth oxide aeroge difficult forming, it is difficult to become bulk.SiO2Aeroge is the aeroge being most widely used at present
One of material, possesses numerous such as the excellent characteristic such as high-specific surface area, high porosity, and especially it is blockiness easily and Stability Analysis of Structures,
And technique is the most ripe.
So it is this with SiO2Aeroge is as structure carrier, with La2O3It is combined and can obtain complete block La2O3-
SiO2Composite aerogel, this composite not only has nano-oxide porous aerogel structure but also possesses rare earth oxide
Characteristic, it will have broad application prospects in fields such as heat insulation, heavy metal ion adsorbed, catalyst and catalyst carriers.
Summary of the invention
The invention aims to improve La2O3The global formation problem of aerogel particle, combines technique and simply becomes
Ripe, and blockiness easy, Stability Analysis of Structures SiO2Aeroge, is prepared for complete block La2O3-SiO2Composite aerogel, Ke Yigeng
The good good characteristic playing rare earth oxide, it is provided that a kind of technique is simple, molding is easy, heavy metal ion adsorbed ability
By force, catalytic effect preferably block La2O3-SiO2The preparation method of composite aerogel.
The technical scheme is that a kind of block La2O3-SiO2The preparation method of composite aerogel, its concrete steps are such as
Under:
(1) by tetraethyl orthosilicate, acidic catalyst, deionized water, dehydrated alcohol be in molar ratio 1:(0.02～
0.2): (2～10): (5～20) mix homogeneously wiring solution-forming, mix and blend 30～60min at 40～50 DEG C；Obtain transparent
SiO2Sol solution；
(2) to the transparent SiO of step (1)2Sol solution adds hydrated inorganic lanthanum salt, continues mixed at 50 DEG C～60 DEG C
Close stirring 30～60min, until mixed solution is water white transparency shape；Wherein, tetraethyl orthosilicate is massaged with hydrated inorganic lanthanum salt
Your ratio is 1:(0.05～0.5) configuration；
(3) adding ammonia regulation pH value in the mixed solution that step (2) obtains is 5～8；Obtain colourless transparent solution；
(4) clear solution that step (3) obtains is poured in mould, be placed in isothermal reaction in baking oven and obtain water white transparency
La2O3-SiO2Compound wet gel；
(5) in step (4), in mould, sample addition organic solvent carries out solvent displacement to wet gel, obtains water white transparency
La2O3-SiO2Compound alcogel；
(6) by the water white transparency La in step (5)2O3-SiO2Compound alcogel carries out CO2Supercritical drying processes；Obtain
Block La2O3-SiO2Composite aerogel.
Acidic catalyst described in preferred steps (1) is the one in hydrochloric acid, nitric acid or acetic acid.
Hydrated inorganic lanthanum salt described in preferred steps (2) is in hydrated lanthanum chloride, hydrated sulfuric acid lanthanum or nitric hydrate lanthanum
One.
Oven temperature in preferred steps (4) is 40～60 DEG C, and the time of isothermal reaction is 1～5 hour.
Organic solvent described in preferred steps (5) is the one in ethanol, acetone or isopropanol.
In preferred steps (5), the number of times of solvent displacement is 2～5 times, and the time of displacement is 12～24h every time.
CO described in preferred steps (6)2Supercritical drying process is: sample is at CO2Under gas shield, reaction temperature is
45～55 DEG C, autoclave Stress control is 8～12MP, and the response time is 8～12h.
By the above-mentioned La prepared2O3-SiO2Composite aerogel is heat treatment test high high-temp stability under aerobic conditions
The pure SiO of document report2Aerogel material maximum operation (service) temperature is only 650 DEG C, the temperature that oversteps the extreme limit 800 DEG C, former
Some three-dimensional net structures almost cave in, specific surface area as little as 50m2/ below g, porosity is extremely low, loses aerogel material
Numerous good characteristics.And La2O3-SiO2Sample after 1000 DEG C of heat treatment 2h is still under aerobic conditions for composite aerogel
There is higher specific surface area (350～400m2/ g), higher porosity (more than 90%).
Beneficial effect:
1, the present invention uses CO2Supercritical Drying Technology is prepared for block DEG C composite aerogel.First pass through the most molten
Sol-gel prepares block La2O3-SiO2Compound wet gel, it is uniform that recycling Supercritical Drying Technology prepares hole, compares table
The block La that area is high2O3-SiO2Composite aerogel.
2, block La prepared by the present invention2O3-SiO2Composite aerogel, not only nanoporous aerogel excellent characteristic is (with just
Tetraethyl orthosilicate, acidic catalyst, deionized water, dehydrated alcohol are 1:0.1:6:16, aluminium chlorohydrate and hydrated inorganic lanthanum salt
As a example by being 1:0.3 in molar ratio, under aerobic conditions, after 1000 DEG C of heat treatment 2h, specific surface area is 385.62m2/ g), logical
Cross the SEM photograph of example 1 sample it can be seen that there is presently no pertinent literature report.
At present, the silica aerogel material life-time service temperature more in the application of heat insulation field is less than 650 DEG C, logical
Cross rare earth doped compound, successfully inhibit original SiO2The high temperature sintering phenomenon of aeroge, so this invention has in research
Under the conditions of oxygen, have on the aerogel material of more operation at high temperature and there is profound significance, La can be opened up further simultaneously2O3-
SiO2The application of self property of composite aerogel middle rare earth, as superhigh temperature resistant, strong heavy metal ion are inhaled
Attached ability, strong catalytic etc..
Accompanying drawing explanation
Fig. 1 is the block La prepared by embodiment 12O3-SiO2The SEM photograph of composite aerogel.
Detailed description of the invention
Example 1
It is that 1:0.1:6:16 mixes at 45 DEG C in molar ratio by tetraethyl orthosilicate, hydrochloric acid, deionized water, dehydrated alcohol
Uniform stirring 60min, obtains transparent SiO2Sol solution.Again to SiO2Sol solution adds hydrated lanthanum chloride, continues at 50 DEG C
Continuous mix and blend 30min, until mixed solution is water white transparency shape, tetraethyl orthosilicate and hydrated lanthanum chloride are 1 in molar ratio:
0.3 configuration.Adding ammonia regulation mixed solution pH value again in clear solution is that 6.5,50 DEG C of continuation uniform stirring 30min obtain
Colourless transparent solution.The La that will obtain2O3-SiO2Complex sol solution is poured into and is placed isothermal reaction 3h in 50 DEG C of baking ovens in mould
Obtain water white transparency La2O3-SiO2Compound wet gel.In mould, sample addition ethanol Ageing solution carries out burin-in process, solvent again
Replace 3 times, each 18h, finally give water white transparency La2O3-SiO2Compound alcogel.Again by La2O3-SiO2Compound alcogel is put
Enter in autoclave, utilize CO2Sample is dried by supercritical drying, wherein CO2Stress control, at 10MPa, controls temperature
Degree is at 50 DEG C, and the supercritical drying time is 10h, obtains block La2O3-SiO2Composite aerogel.Through sample is carried out aerobic bar
Lower 1300 DEG C of high-temperature heat treatment 2h of part, obtain the block La after heat treatment2O3-SiO2Composite aerogel.Find through characterizing, should
The specific surface area of aeroge is 385.62m2/ g, porosity is 92%, and average pore size is 42nm.Prepared block La2O3-
SiO2The SEM photograph of composite aerogel is as it is shown in figure 1, can be seen that from figure obtained composite aerogel is porous three dimensional
Network structure.
Example 2
It is that 1:0.02:2:5 mixes at 50 DEG C in molar ratio by tetraethyl orthosilicate, nitric acid, deionized water, dehydrated alcohol
Uniform stirring 30min, obtains transparent SiO2Sol solution.Again to SiO2Sol solution adds hydrated lanthanum chloride, continues at 50 DEG C
Continuous mix and blend 60min, until mixed solution is water white transparency shape, tetraethyl orthosilicate and hydrated lanthanum chloride are 1 in molar ratio:
0.1 configuration.Adding ammonia regulation mixed solution pH value again in clear solution is that 7.5,50 DEG C of continuation uniform stirring 30min obtain
Colourless transparent solution.The La that will obtain2O3-SiO2Complex sol solution is poured into and is placed isothermal reaction 5h in 40 DEG C of baking ovens in mould
Obtain water white transparency La2O3-SiO2Compound wet gel.In mould, sample addition acetone Ageing solution carries out burin-in process, solvent again
Replace 5 times, each 12h, finally give water white transparency La2O3-SiO2Compound alcogel.Again by La2O3-SiO2Compound alcogel is put
Enter in autoclave, utilize CO2Sample is dried by supercritical drying, wherein CO2Stress control, at 8MPa, controls temperature
Degree is at 45 DEG C, and the supercritical drying time is 12h, obtains block La2O3-SiO2Composite aerogel.Through sample is carried out aerobic bar
Lower 900 DEG C of high-temperature heat treatment 2h of part, obtain the block La after heat treatment2O3-SiO2Composite aerogel.Find through characterizing, this gas
The specific surface area of gel is 430.26m2/ g, porosity is 94%, and average pore size is 34nm.
Example 3
It is that 1:0.2:10:20 is mixed at 50 DEG C in molar ratio by tetraethyl orthosilicate, acetic acid, deionized water, dehydrated alcohol
Close uniform stirring 50min, obtain transparent SiO2Sol solution.Again to SiO2Sol solution adds hydrated sulfuric acid lanthanum, at 50 DEG C
Continuing mix and blend 45min, until mixed solution is water white transparency shape, tetraethyl orthosilicate and hydrated lanthanum chloride are in molar ratio
1:0.5 configuration.Adding ammonia regulation mixed solution pH value again in clear solution is that 5,50 DEG C of continuation uniform stirring 30min obtain
Colourless transparent solution.The La that will obtain2O3-SiO2Complex sol solution is poured into and is placed isothermal reaction 1h in 60 DEG C of baking ovens in mould
Obtain water white transparency La2O3-SiO2Compound wet gel.In mould, sample addition ethanol Ageing solution carries out burin-in process, solvent again
Replace 4 times, each 18h, finally give water white transparency La2O3-SiO2Compound alcogel.Again by La2O3-SiO2Compound alcogel is put
Enter in autoclave, utilize CO2Sample is dried by supercritical drying, wherein CO2Stress control, at 12MPa, controls temperature
Degree is at 55 DEG C, and the supercritical drying time is 10h, obtains block La2O3-SiO2Composite aerogel.Through sample is carried out aerobic bar
Lower 1000 DEG C of high-temperature heat treatment 2h of part, obtain the block La after heat treatment2O3-SiO2Composite aerogel.Find through characterizing, should
The specific surface area of aeroge is 367.44m2/ g, porosity is 91%, and average pore size is 43nm.
Example 4
It is that 1:0.15:8:10 is mixed at 50 DEG C in molar ratio by tetraethyl orthosilicate, nitric acid, deionized water, dehydrated alcohol
Close uniform stirring 40min, obtain transparent SiO2Sol solution.Again to SiO2Sol solution adds hydrated sulfuric acid lanthanum, at 50 DEG C
Continuing mix and blend 40min, until mixed solution is water white transparency shape, tetraethyl orthosilicate and hydrated lanthanum chloride are in molar ratio
1:0.4 configuration.Adding ammonia regulation mixed solution pH value again in clear solution is that 6.0,50 DEG C of continuation uniform stirring 30min obtain
To colourless transparent solution.The La that will obtain2O3-SiO2Complex sol solution is poured into and is placed isothermal reaction in 50 DEG C of baking ovens in mould
3h obtains water white transparency La2O3-SiO2Compound wet gel.In mould, sample addition isopropanol Ageing solution carries out burin-in process again,
Solvent is replaced 3 times, and each 18h finally gives water white transparency La2O3-SiO2Compound alcogel.Again by La2O3-SiO2Compound alcohol coagulates
Glue is put in autoclave, utilizes CO2Sample is dried by supercritical drying, wherein CO2Stress control is in 8MPa, control
Temperature processed is at 48 DEG C, and the supercritical drying time is 10h, obtains block La2O3-SiO2Composite aerogel.Through sample is had
900 DEG C of high-temperature heat treatment 2h under the conditions of oxygen, obtain the block La after heat treatment2O3-SiO2Composite aerogel.Find through characterizing,
The specific surface area of this aeroge is 418.91m2/ g, porosity is 93%, and average pore size is 36nm.
Example 5
It is that 1:0.08:7:12 is mixed at 50 DEG C in molar ratio by tetraethyl orthosilicate, acetic acid, deionized water, dehydrated alcohol
Close uniform stirring 30min, obtain transparent SiO2Sol solution.Again to SiO2Sol solution adds hydrated lanthanum chloride, at 50 DEG C
Continuing mix and blend 60min, until mixed solution is water white transparency shape, tetraethyl orthosilicate and hydrated lanthanum chloride are in molar ratio
1:0.2 configuration.Adding ammonia regulation mixed solution pH value again in clear solution is that 8.0,50 DEG C of continuation uniform stirring 30min obtain
To colourless transparent solution.The La that will obtain2O3-SiO2Complex sol solution is poured into and is placed isothermal reaction in 60 DEG C of baking ovens in mould
2h obtains water white transparency La2O3-SiO2Compound wet gel.In mould, sample addition acetone Ageing solution carries out burin-in process again, molten
Agent is replaced 3 times, and each 12h finally gives water white transparency La2O3-SiO2Compound alcogel.Again by La2O3-SiO2Compound alcogel
Put in autoclave, utilize CO2Sample is dried by supercritical drying, wherein CO2Stress control, at 10MPa, controls
Temperature is at 48 DEG C, and the supercritical drying time is 10h, obtains block La2O3-SiO2Composite aerogel.Through sample is carried out aerobic
Under the conditions of 1000 DEG C of high-temperature heat treatment 2h, obtain the block La after heat treatment2O3-SiO2Composite aerogel.Find through characterizing,
The specific surface area of this aeroge is 378.46m2/ g, porosity is 92%, and average pore size is 41nm.
Example 6
It is that 1:0.18:9:15 is mixed at 50 DEG C in molar ratio by tetraethyl orthosilicate, hydrochloric acid, deionized water, dehydrated alcohol
Close uniform stirring 40min, obtain transparent SiO2Sol solution.Again to SiO2Sol solution adds hydrated lanthanum chloride, at 60 DEG C
Continuing mix and blend 50min, until mixed solution is water white transparency shape, tetraethyl orthosilicate and hydrated lanthanum chloride are in molar ratio
1:0.25 configuration.Adding ammonia regulation mixed solution pH value again in clear solution is 5.5,50 DEG C of continuation uniform stirring 30min
Obtain colourless transparent solution.The La that will obtain2O3-SiO2Complex sol solution pours that to place constant temperature in 50 DEG C of baking ovens in mould anti-into
3h is answered to obtain water white transparency La2O3-SiO2Compound wet gel.In mould, sample addition isopropanol Ageing solution carries out aging place again
Reason, solvent displacement 2 times, each 24h, finally give water white transparency La2O3-SiO2Compound alcogel.Again by La2O3-SiO2Compound
Alcogel is put in autoclave, utilizes CO2Sample is dried by supercritical drying, wherein CO2Stress control exists
12MPa, control temperature is at 45 DEG C, and the supercritical drying time is 8h, obtains block La2O3-SiO2Composite aerogel.Through to sample
Product carry out lower 900 DEG C of high-temperature heat treatment 2h of aerobic conditions, obtain the block La after heat treatment2O3-SiO2Composite aerogel.Pass through
Characterizing and find, the specific surface area of this aeroge is 451.46m2/ g, porosity is 95%, and average pore size is 31nm.
Claims (7)
1. a block La2O3-SiO2The preparation method of composite aerogel, it specifically comprises the following steps that
(1) by tetraethyl orthosilicate, acidic catalyst, deionized water, dehydrated alcohol it is 1:(0.02～0.2 in molar ratio): (2
～10): (5～20) mix homogeneously wiring solution-forming, mix and blend 30～60min at 40～50 DEG C；Obtain transparent SiO2Colloidal sol
Solution；
(2) to the transparent SiO of step (1)2Sol solution adds hydrated inorganic lanthanum salt, at 50 DEG C～60 DEG C, continues mixing stir
Mix 30～60min, until mixed solution is water white transparency shape；Wherein, tetraethyl orthosilicate is with hydrated inorganic lanthanum salt in molar ratio
For 1:(0.05～0.5) configuration；
(3) adding ammonia regulation pH value in the mixed solution that step (2) obtains is 5～8；Obtain colourless transparent solution；
(4) clear solution that step (3) obtains is poured in mould, be placed in isothermal reaction in baking oven and obtain water white transparency La2O3-
SiO2Compound wet gel；
(5) in step (4), in mould, sample addition organic solvent carries out solvent displacement to wet gel, obtains water white transparency
La2O3-SiO2Compound alcogel；
(6) by the water white transparency La in step (5)2O3-SiO2Compound alcogel carries out CO2Supercritical drying processes；Obtain bulk
La2O3-SiO2Composite aerogel.
Preparation method the most according to claim 1, it is characterised in that the acidic catalyst described in step (1) be hydrochloric acid,
One in nitric acid or acetic acid.
Preparation method the most according to claim 1, it is characterised in that the hydrated inorganic lanthanum salt described in step (2) is hydration
One in lanthanum chloride, hydrated sulfuric acid lanthanum or nitric hydrate lanthanum.
Preparation method the most according to claim 1, it is characterised in that the oven temperature in step (4) is 40～60 DEG C, permanent
The time of temperature reaction is 1～5 hour.
Preparation method the most according to claim 1, it is characterised in that the organic solvent described in step (5) be ethanol, third
One in ketone or isopropanol.
Preparation method the most according to claim 1, it is characterised in that in step (5), the number of times of solvent displacement is 2～5 times,
The time of displacement is 12～24h every time.
Preparation method the most according to claim 1, it is characterised in that the CO described in step (6)2Supercritical drying process
For: sample is at CO2Under gas shield, reaction temperature is 45～55 DEG C, and autoclave Stress control is 8～12MP, during reaction
Between be 8～12h.
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Cited By (6)
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| CN110563435A (en) * | 2018-06-06 | 2019-12-13 | 厦门稀土材料研究所 | Rare earth-based aerogel material with radiation shielding effect and heat insulation performance as well as preparation and application thereof |
| CN111013566A (en) * | 2019-12-31 | 2020-04-17 | 弘大科技（北京）股份公司 | Novel rare earth modified aerogel denitration flue gas catalyst and preparation method thereof |
| CN112320833A (en) * | 2020-11-06 | 2021-02-05 | 湖南荣岚智能科技有限公司 | High temperature resistant SiO2-Gd2O3Composite aerogel and preparation method thereof |
| CN113289598A (en) * | 2021-04-27 | 2021-08-24 | 南京工业大学 | FePO4-SiO2Preparation method of aerogel catalyst material |
| CN115140772A (en) * | 2022-05-20 | 2022-10-04 | 大连工业大学 | VO (volatile organic compound) 2 -SiO 2 Preparation method of composite aerogel |
| WO2023040966A1 (en) * | 2021-09-17 | 2023-03-23 | 中科润资(重庆)节能科技有限公司 | Thermal insulation material, and preparation method therefor and use thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110563435A (en) * | 2018-06-06 | 2019-12-13 | 厦门稀土材料研究所 | Rare earth-based aerogel material with radiation shielding effect and heat insulation performance as well as preparation and application thereof |
| CN110563435B (en) * | 2018-06-06 | 2022-07-01 | 厦门稀土材料研究所 | Rare earth-based aerogel material with radiation shielding effect and heat insulation performance as well as preparation and application thereof |
| CN111013566A (en) * | 2019-12-31 | 2020-04-17 | 弘大科技（北京）股份公司 | Novel rare earth modified aerogel denitration flue gas catalyst and preparation method thereof |
| CN111013566B (en) * | 2019-12-31 | 2023-01-06 | 弘大科技（北京）股份公司 | Novel rare earth modified aerogel denitration flue gas catalyst and preparation method thereof |
| CN112320833A (en) * | 2020-11-06 | 2021-02-05 | 湖南荣岚智能科技有限公司 | High temperature resistant SiO2-Gd2O3Composite aerogel and preparation method thereof |
| CN112320833B (en) * | 2020-11-06 | 2022-08-02 | 湖南荣岚智能科技有限公司 | High temperature resistant SiO 2 -Gd 2 O 3 Composite aerogel and preparation method thereof |
| CN113289598A (en) * | 2021-04-27 | 2021-08-24 | 南京工业大学 | FePO4-SiO2Preparation method of aerogel catalyst material |
| WO2023040966A1 (en) * | 2021-09-17 | 2023-03-23 | 中科润资(重庆)节能科技有限公司 | Thermal insulation material, and preparation method therefor and use thereof |
| CN115140772A (en) * | 2022-05-20 | 2022-10-04 | 大连工业大学 | VO (volatile organic compound) 2 -SiO 2 Preparation method of composite aerogel |
| CN115140772B (en) * | 2022-05-20 | 2023-08-22 | 大连工业大学 | VO (Voice over Internet protocol) 2 -SiO 2 Preparation method of composite aerogel |
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