CN104986994B - A kind of preparation method of block zirconium carbon aerogel composite - Google Patents
A kind of preparation method of block zirconium carbon aerogel composite Download PDFInfo
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Abstract
The invention belongs to the preparation technology field of nano-porous materials, is related to a kind of preparation method of block zirconium carbon aerogel composite.The present invention is with resorcinol, formaldehyde as carbon source, inorganic zirconium salts zirconium oxychloride is zirconium source, deionized water is hydrolytic reagent, alcohols is solvent, epoxide is gel accelerator, wet gel is prepared by solgel reaction in the presence of base catalyst, wet gel obtains shape high temperature resistant zirconium carbon aerogel composite through the displacement of aging, solvent, supercritical drying, high-temperature heat treatment.Material obtained in cheap inorganic zirconium salts as raw material of the invention has low-density, bigger serface, high intensity, high-temperature stability, structural integrity, and the system has good prospect in high temperature insulating and in terms of doing catalytic carrier.
Description
Technical field
The invention belongs to the preparation technology field of nano-porous materials, is related to a kind of system of the compound airsetting hot material of carbon-zirconium
Preparation Method.A kind of CO is used especially2Supercritical methanol technology prepares the preparation method of block zirconium-carbon aerogel composite.
Background technology
Aeroge is the nano-porous materials that a kind of nano-particle is mutually assembled, and has high-specific surface area and porosity,
Therefore common solid-state material is all different from aspects such as calorifics, acoustics, optics, be that a kind of lightweight nanometer with extensive use is more
Porous materials.The high porosity that aerogel material possesses can reduce solid thermal conduction, and nano-porous structure can suppress gas conduction of heat,
The infrared light screening agent of introducing can reduce radiant heat transfer, and this causes aeroge to have excellent heat-proof quality, be generally acknowledged heat conduction at present
The minimum solid material of coefficient.It is many to the comparison of carbon-silicon, carbon-aluminum architectural study both at home and abroad at present, to the compound gas of carbon-zirconium system
The research of gel is not also concrete to be reported.Therefore the preparation and research of block carbon-zirconium system aeroge is for the property of optimization material
The application of energy and reinforcement material has far-reaching influence.
The content of the invention
The invention aims to improve the deficiencies in the prior art and provide a kind of block zirconium-carbon aerogel composite
Preparation method, the method materials and process is simple be with low cost, this material can be used for high temperature insulating, and as urging
Change carrier.
The technical scheme is that：A kind of preparation method of block zirconium-carbon aerogel composite, its concrete steps is such as
Under：
(1) inorganic zirconium salts are dissolved in configuration in solvent to be obtained concentration being that 0.1mol/L～0.5mol/L inorganic zirconium salts are molten
Liquid, then in solution, add Polyethylene Glycol and Methanamide to stir, obtain ZrO2Colloidal sol；Wherein Polyethylene Glycol and inorganic zirconium salts
Mol ratio be (0.2～1)：1, Methanamide is (0.2～1) with the mol ratio of inorganic zirconium salts：1；Simultaneously by resorcinol, first
Aldehyde, water, base catalyst, according to formaldehyde：Water：The mol ratio of resorcinol is 2：(33～55)：1, resorcinol：Base catalysis
The mol ratio of agent is 80～120 ratio mixing, is uniformly mixing to obtain RF organosols；
(2) ZrO that will be obtained in step (1)2Colloidal sol and RF organosols according to inorganic zirconium salts and resorcinol mole
Than for 1：(1～4) mix, be stirring evenly and then adding into expoxy propane, be placed in mould after being stirred for uniformly and treat its gel, obtain
ZrO2/ RF gels；
(3) then in mould in step (2) gel add Ageing solution, and be put in 40～70 DEG C of baking oven carry out it is aging
Process and replace foreign ion；
(4) ZrO that will be obtained after burin-in process in step (3)2The compound wet gels of/RF carry out supercritical drying process, obtain
To block ZrO2/ RF composite aerogels；
(5) ZrO that will be obtained in step (4)2/ RF composite aerogels heat treatment under atmosphere protection, obtains block resistance to height
Warm carbon-zirconium aerogel material.
It is 1 according to volume ratio that solvent described in preferred steps (1) is water and ethanol：The mixed solvent that (3～5) configure.
Inorganic zirconium salts described in preferred steps (1) be eight hydration zirconium oxychlorides or the one kind in six nitric hydrate oxygen zirconiums or
Its mixture.
Base catalyst in preferred steps (1) is in natrium carbonicum calcinatum, sodium hydroxide, calcium hydroxide or potassium carbonate
Kind.
The addition of preferred steps (2) expoxy propane is to control the mol ratio of expoxy propane and inorganic zirconium salts for (1～4)：
1。
Ageing solution described in preferred steps (3) is the one kind in ethanol, normal hexane or tetraethyl orthosilicate or its mixing
Thing；Burin-in process and replace foreign ion displacement number of times be 5～10 times, each time swap be 12～24h.
Supercritical drying described in preferred steps (4) is CO2Supercritical drying, with CO2As dried medium, reaction temperature
Spend for 45～60 DEG C, in autoclave, pressure is 8～12MPa, and drying time is 8～14h.
Atmosphere described in preferred steps (5) is the one kind in nitrogen, argon or helium.
In preferred steps (5), heat treatment temperature is 800 DEG C～1500 DEG C, and heat treatment time is 3～10h.
The apparent density of aerogel material obtained in preferred steps (5) is 0.15～0.6g/cm3, specific surface area 330～
500m2/ g, pore-size distribution is in 5～50nm.
Beneficial effect：
The inventive method and there are following features by the method bulk high temperature resistant zirconium-carbon aerogel composite：
(1) raw material is inexpensive, reduces cost.What in this method, zirconium source selected is inorganic zirconium salts, has abandoned the process of being typically prepared
Organic alcohol zirconium of middle employing, and the price of inorganic zirconium salts is low, greatly reduces production cost.
(2) density is low, and block high temperature resistant zirconium-carbon aerogel composite density prepared by the invention is 0.15～0.6g/
cm2, density is significantly less than conventional high temperature insulating material.
(3) block high temperature resistant zirconium-carbon aerogel composite, the carbon reactant in sol-gel process obtained in the method
It is not independent reaction with zirconium reactant, the wet gel for obtaining is nor the mixing of simple carbon and zirconium, but reacts each other
So that the network structure of wet gel is interleaved with each other, more firmly.Therefore aeroge good moldability, intensity are big, can have well
Purposes.
Description of the drawings
In kind photos of the Fig. 1 for shape high temperature resistant zirconium-carbon aerogel composite obtained in embodiment 1；
Nitrogen adsorption desorption curves of the Fig. 2 for carbon-zirconium composite aerogel obtained in embodiment 1；
Fig. 3 is that the SEM of block carbon-zirconium composite aerogel prepared by embodiment 3 shines.
Specific embodiment
Example 1
It is 1 according to eight hydration zirconium oxychlorides and resorcinol mol ratio：2 are respectively configured ZrO2Colloidal sol and RF colloidal sols, by eight
It is 1 that hydration zirconium oxychloride is dissolved in ethanol with water volume ratio:In 4 mixed solvent cause its concentration be 0.5mol/L, thereto plus
The mol ratio for entering Macrogol 1000, Methanamide, Macrogol 1000 and Methanamide and eight hydration zirconium oxychlorides is 0.5：1,
Mixing and stirring, obtains ZrO2Colloidal sol.Formaldehyde：Water：Resorcinol=2：55:1, resorcinol：Sodium carbonate=100 mole
Organosol (RF colloidal sols) is obtained after than uniformly mixing and being sufficiently stirred for.The mixing of above-mentioned 2 kinds of colloidal sol is stirred, then
After be added thereto to zirconium oxychloride mol ratio be 1:The expoxy propane of 1 amount, pours in mould after stirring 15min, 6h or so
Gel.RF/ZrO is obtained by above-mentioned2After gel puts 12h at room temperature, ethanol is added to replace as Ageing solution miscellaneous in wet gel
Matter ion, is then put in 50 DEG C of baking oven, replaces 8 times, each 24h.RF/ZrO after again will be aging2Compound wet gel is put into
In high temperature and high pressure kettle, using CO2Supercritical drying is dried to sample, wherein CO2Stress control is in 10MPa, temperature control
At 50 DEG C, the supercritical drying time is 9h, so as to the block RF/ZrO of good forming ability is obtained2Composite aerogel.Again will be organic
Aeroge heat treatment 3h at 1500 DEG C under the protection of argon obtains required block carbon-zirconium aerogel composite.It is obtained
Shape high temperature resistant zirconium-carbon aerogel composite photo in kind it is as shown in Figure 1：It can be seen that the composite aerogel is whole blocks
Body, surface flawless, and possess certain mechanical strength, and its nitrogen adsorption desorption curve is as shown in Figure 2：It can be seen that the song
Line is typical IV type curve, shows material for typical mesoporous material, and specific surface area is big, advantageous as a kind of high temperature resistant every
Hot material is used.Jing is characterized and is found its density 0.41g/cm2, specific surface area is 420.1m2/ g, pore-size distribution is in 5～30nm.
Example 2
It is 1 according to eight hydration zirconium oxychlorides and resorcinol mol ratio：1 is respectively configured ZrO2Colloidal sol and RF colloidal sols, by eight
It is 1 that hydration zirconium oxychloride is dissolved in ethanol with water volume ratio:In 3 mixed solvent cause its concentration be 0.5mol/L, thereto plus
The mol ratio for entering Macrogol 600, Methanamide, Macrogol 600 and Methanamide and eight hydration zirconium oxychlorides is 0.2：1, mix
Conjunction stirs, and obtains ZrO2Colloidal sol.Formaldehyde：Water：Resorcinol=2：55:1, resorcinol：The mol ratio of potassium carbonate=100
Uniformly mix and obtain after being sufficiently stirred for organosol (RF colloidal sols).The mixing of above-mentioned 2 kinds of colloidal sol is stirred, Ran Houhou
It is 1 to be added thereto to zirconium oxychloride mol ratio:The expoxy propane of 1 amount, pours in mould after stirring 10min, and 8h or so coagulates
Glue.RF/ZrO is obtained by above-mentioned2After gel puts 12h at room temperature, add ethanol that the impurity in wet gel is replaced as Ageing solution
Ion, is then put in 40 DEG C of baking oven, replaces 10 times, each 24h.RF/ZrO after again will be aging2Compound wet gel is put into
In high temperature and high pressure kettle, using CO2Supercritical drying is dried to sample, wherein CO2Stress control is in 8MPa, temperature control
At 60 DEG C, the supercritical drying time is 12h, so as to the block RF/ZrO of good forming ability is obtained2Composite aerogel.Again will be organic
Aeroge heat treatment 10h at 1500 DEG C under the protection of argon obtains required block carbon-zirconium aerogel composite.It is obtained
Composite aerogel density 0.51g/cm2, specific surface area is 338.4m2/ g, pore-size distribution is in 10～40nm.
Example 3
It is 1 according to eight hydration zirconium oxychlorides and resorcinol mol ratio：4 are respectively configured ZrO2Colloidal sol and RF colloidal sols, by eight
It is 1 that hydration zirconium oxychloride is dissolved in ethanol with water volume ratio:In 5 mixed solvent cause its concentration be 0.5mol/L, thereto plus
The mol ratio for entering Macrogol 1000, Methanamide, Macrogol 1000 and Methanamide and eight hydration zirconium oxychlorides is 0.8：1,
Mixing and stirring, obtains ZrO2Colloidal sol.Formaldehyde：Water：Resorcinol=2：55:1, resorcinol：Sodium carbonate=100 mole
Organosol (RF colloidal sols) is obtained after than uniformly mixing and being sufficiently stirred for.The mixing of above-mentioned 2 kinds of colloidal sol is stirred, then
After be added thereto to zirconium oxychloride mol ratio be 1:The expoxy propane of 1 amount, pours in mould after stirring 15min, 5h or so
Gel.RF/ZrO is obtained by above-mentioned2After gel puts 12h at room temperature, ethanol is added to replace as Ageing solution miscellaneous in wet gel
Matter ion, is then put in 70 DEG C of baking oven, replaces 5 times, each 12h.RF/ZrO after again will be aging2Compound wet gel is put into
In high temperature and high pressure kettle, using CO2Supercritical drying is dried to sample, wherein CO2Stress control is in 12MPa, temperature control
At 45 DEG C, the supercritical drying time is 8h, so as to the block RF/ZrO of good forming ability is obtained2Composite aerogel.Again will be organic
Aeroge heat treatment 3h at 1500 DEG C under the protection of argon obtains required block carbon-zirconium aerogel composite.It is made
The SEM figures of standby carbon-zirconium aerogel composite are as shown in figure 3, the compound airsetting of the block carbon-zirconium for as can be seen from the figure obtaining
Glue is porous network structure, and Jing is characterized and found its density 0.24g/cm2, specific surface area is 429.0m2/ g, pore-size distribution 5～
40nm。
Example 4
It is 1 according to zirconium oxychloride and resorcinol mol ratio：2 are respectively configured ZrO2Colloidal sol and RF colloidal sols, are hydrated oxygen by eight
It is 1 that zirconium chloride is dissolved in ethanol with water volume ratio:Cause its concentration to be 0.1mol/L in 4 mixed solvent, be added thereto to poly- second
The mol ratio of glycol 600, Methanamide, Macrogol 600 and Methanamide and eight hydration zirconium oxychlorides is 1：1, mix equal
It is even, obtain ZrO2Colloidal sol.Formaldehyde：Water：Resorcinol=2：55:1, resorcinol：The mol ratio of sodium carbonate=80 uniformly mixes
And after being sufficiently stirred for, obtain organosol (RF colloidal sols).By above-mentioned 2 kinds of colloidal sol mixing stir, then after thereto plus
It is 3 to enter with zirconium oxychloride mol ratio:The expoxy propane of 1 amount, pours in mould after stirring 10min, 3h or so gels.Will be above-mentioned
Obtain RF/ZrO2After gel puts 12h at room temperature, add ethanol that the foreign ion in wet gel is replaced as Ageing solution, then
It is put in 50 DEG C of baking oven, replaces 7 times, each 24h.RF/ZrO after again will be aging2Compound wet gel is put into high temperature and high pressure kettle
It is interior, using CO2Supercritical drying is dried to sample, wherein CO2In 10MPa, temperature control surpasses Stress control at 50 DEG C
Critical drying time is 10h, so as to the block RF/ZrO of good forming ability is obtained2Composite aerogel.Again organic aerogel is existed
Block carbon-zirconium aerogel composite needed for heat treatment 5h is obtained at 1500 DEG C under the protection of helium.Obtained compound gas
Gel density 0.17g/cm2, specific surface area is 490.1m2/ g, pore-size distribution is in 10～50nm.
Example 5
It is 1 according to six nitric hydrate oxygen zirconiums and resorcinol mol ratio：2 are respectively configured ZrO2Colloidal sol and RF colloidal sols, by six
It is 1 that nitric hydrate oxygen zirconium is dissolved in ethanol with water volume ratio:In 4 mixed solvent cause its concentration be 0.5mol/L, thereto plus
The mol ratio for entering Macrogol 1000, Methanamide, Macrogol 1000 and Methanamide and six nitric hydrate oxygen zirconiums is 0.5：1,
Mixing and stirring, obtains ZrO2Colloidal sol.Formaldehyde：Water：Resorcinol=2：33:1, resorcinol：Sodium carbonate=120 mole
Organosol (RF colloidal sols) is obtained after than uniformly mixing and being sufficiently stirred for.The mixing of above-mentioned 2 kinds of colloidal sol is stirred, then
After be added thereto to zirconium oxychloride mol ratio be 1:The expoxy propane of 1 amount, pours in mould after stirring 10min, 6h or so
Gel.RF/ZrO is obtained by above-mentioned2After gel puts 12h at room temperature, normal hexane is added as in Ageing solution displacement wet gel
Foreign ion, is then put in 50 DEG C of baking oven, replaces 8 times, each 24h.RF/ZrO after again will be aging2Compound wet gel is put
Enter in high temperature and high pressure kettle, using CO2Supercritical drying is dried to sample, wherein CO2Stress control is in 10MPa, temperature control
At 50 DEG C, the supercritical drying time is 14h to system, so as to the block RF/ZrO of good forming ability is obtained2Composite aerogel.To have again
Machine aeroge heat treatment 3h at 800 DEG C under the protection of nitrogen obtains required block carbon-zirconium aerogel composite.It is obtained
Composite aerogel density 0.58g/cm2, specific surface area is 377.2m2/ g, pore-size distribution is in 5～20nm.
Example 6
It is 1 according to eight hydration zirconium oxychlorides and resorcinol mol ratio：2 are respectively configured ZrO2Colloidal sol and RF colloidal sols, by eight
It is 1 that hydration zirconium oxychloride is dissolved in ethanol with water volume ratio:In 4 mixed solvent cause its concentration be 0.3mol/L, thereto plus
The mol ratio for entering Macrogol 600, Methanamide, Macrogol 600 and Methanamide and eight hydration zirconium oxychlorides is 0.5：1, mix
Conjunction stirs, and obtains ZrO2Colloidal sol.Formaldehyde：Water：Resorcinol=2：55:1, resorcinol：The mol ratio of sodium carbonate=100
Uniformly mix and obtain after being sufficiently stirred for organosol (RF colloidal sols).The mixing of above-mentioned 2 kinds of colloidal sol is stirred, Ran Houhou
It is 2.5 to be added thereto to zirconium oxychloride mol ratio:The expoxy propane of 1 amount, pours in mould after stirring 10min, 3h or so
Gel.RF/ZrO is obtained by above-mentioned2After gel puts 12h at room temperature, ethanol is added to replace as Ageing solution miscellaneous in wet gel
Matter ion, is then put in 50 DEG C of baking oven, replaces 10 times, each 24h.RF/ZrO after again will be aging2Compound wet gel is put
Enter in high temperature and high pressure kettle, using CO2Supercritical drying is dried to sample, wherein CO2Stress control is in 10MPa, temperature control
At 50 DEG C, the supercritical drying time is 11h to system, so as to the block RF/ZrO of good forming ability is obtained2Composite aerogel.To have again
Machine aeroge heat treatment 3h at 1500 DEG C under the protection of argon obtains required block carbon-zirconium aerogel composite.System
Composite aerogel density 0.26g/cm for obtaining2, specific surface area is 488.7m2/ g, pore-size distribution is in 5～40nm.
Example 7
It is 1 according to eight hydration zirconium oxychlorides and resorcinol mol ratio：1.5 are respectively configured ZrO2Colloidal sol and RF colloidal sols, will
It is 1 that eight hydration zirconium oxychlorides are dissolved in ethanol with water volume ratio:Its concentration is caused to be 0.5mol/L in 4 mixed solvent, thereto
Macrogol 1000, Methanamide, Macrogol 1000 and Methanamide and the mol ratio of eight hydration zirconium oxychlorides is added to be 0.5：
1, mixing and stirring obtains ZrO2Colloidal sol.Formaldehyde：Water：Resorcinol=2：55:1, resorcinol：Sodium hydroxide=100
Mol ratio uniformly mixes and organosol (RF colloidal sols) is obtained after being sufficiently stirred for.The mixing of above-mentioned 2 kinds of colloidal sol is stirred,
Then it is 1 to be added thereto to afterwards with zirconium oxychloride mol ratio:The expoxy propane of 1 amount, pours in mould after stirring 12min, 7h
Left and right gel.RF/ZrO is obtained by above-mentioned2After gel puts 12h at room temperature, ethanol is added as in Ageing solution displacement wet gel
Foreign ion, be then put in 50 DEG C of baking oven, replace 8 times, each 24h.RF/ZrO after again will be aging2Compound wet gel
It is put in high temperature and high pressure kettle, using CO2Supercritical drying is dried to sample, wherein CO2Stress control is in 12MPa, temperature
At 45 DEG C, the supercritical drying time is 8h for control, so as to the block RF/ZrO of good forming ability is obtained2Composite aerogel.Again will
Organic aerogel heat treatment 5h at 1500 DEG C under the protection of argon obtains required block carbon-zirconium aerogel composite.
Obtained composite aerogel density 0.48g/cm2, specific surface area is 338.8m2/ g, pore-size distribution is in 5～30nm.
Claims (9)
1. a kind of preparation method of block zirconium-carbon aerogel composite, which comprises the following steps that：
(1) inorganic zirconium salts are dissolved in configuration in solvent to be obtained concentration being 0.1mol/L～0.5mol/L inorganic zirconium salts solution, then
To in solution, add Polyethylene Glycol and Methanamide to stir, obtain ZrO2Colloidal sol；Wherein Polyethylene Glycol and inorganic zirconium salts rub
You are than being (0.2～1)：1, Methanamide is (0.2～1) with the mol ratio of inorganic zirconium salts：1；Simultaneously by resorcinol, formaldehyde, water,
Base catalyst, according to formaldehyde：Water：The mol ratio of resorcinol is 2：(33～55)：1, resorcinol：Base catalyst rubs
You mix than the ratio for 80～120, are uniformly mixing to obtain RF organosols；Wherein described inorganic zirconium salts are eight hydration oxygen chlorine
Change zirconium or one kind or its mixture in six nitric hydrate oxygen zirconiums；
(2) ZrO that will be obtained in step (1)2Colloidal sol and RF organosols are 1 according to the mol ratio of inorganic zirconium salts and resorcinol：
(1～4) mix, be stirring evenly and then adding into expoxy propane, be placed in mould after being stirred for uniformly and treat its gel, obtain ZrO2/RF
Gel；
(3) Ageing solution is added and then to gel in mould in step (2), and is put in 40～70 DEG C of baking oven and is carried out burin-in process
And replace foreign ion；
(4) ZrO that will be obtained after burin-in process in step (3)2The compound wet gels of/RF carry out supercritical drying process, obtain bulk
ZrO2/ RF composite aerogels；
(5) ZrO that will be obtained in step (4)2/ RF composite aerogels heat treatment under atmosphere protection, obtain block high temperature resistant carbon-
Zirconium aerogel material.
2. preparation method according to claim 1, it is characterised in that the solvent described in step (1) be water with ethanol according to
Volume ratio is 1：The mixed solvent that (3～5) configure.
3. preparation method according to claim 1, it is characterised in that the base catalyst in step (1) is Carbon Dioxide
One kind in sodium, sodium hydroxide, calcium hydroxide or potassium carbonate.
4. preparation method according to claim 1, it is characterised in that the addition of step (2) expoxy propane is control epoxy
Propane is (1～4) with the mol ratio of inorganic zirconium salts：1.
5. preparation method according to claim 1, it is characterised in that the Ageing solution described in step (3) be ethanol, just oneself
One kind or its mixture in alkane or tetraethyl orthosilicate；Burin-in process and replace foreign ion displacement number of times be 5～10 times,
Time swap is 12～24h every time.
6. preparation method according to claim 1, it is characterised in that the supercritical drying described in step (4) is CO2It is super to face
Boundary is dried, with CO2Used as dried medium, reaction temperature is 45～60 DEG C, and in autoclave, pressure is 8～12MPa, when being dried
Between be 8～14h.
7. preparation method according to claim 1, it is characterised in that the atmosphere described in step (5) be nitrogen, argon or
One kind in helium.
8. preparation method according to claim 1, it is characterised in that heat treatment temperature is 800 DEG C～1500 in step (5)
DEG C, heat treatment time is 3～10h.
9. preparation method according to claim 1, it is characterised in that the apparent density of aerogel material obtained in step (5)
For 0.15～0.6g/cm3, specific surface area is in 330～500m2/ g, pore-size distribution is in 5～50nm.
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| CN108439409A (en) * | 2018-04-18 | 2018-08-24 | 南京工业大学 | A kind of preparation method of bulk boron carbide aeroge |
| CN109020619A (en) * | 2018-09-19 | 2018-12-18 | 蚌埠星烁新材料科技有限公司 | A kind of corrosion-resistant waterproof material suitable for concrete |
| CN110818423A (en) * | 2019-11-04 | 2020-02-21 | 江苏一夫新材料产业技术研究院有限公司 | Zirconium carbide-boron carbide composite aerogel and preparation method thereof |
| CN111346678A (en) * | 2020-03-30 | 2020-06-30 | 安徽元琛环保科技股份有限公司 | Preparation method of denitration catalyst with aerogel as carrier and prepared catalyst |
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