CN109289717B - Preparation method of zirconium dioxide/titanium dioxide composite aerogel - Google Patents

Preparation method of zirconium dioxide/titanium dioxide composite aerogel Download PDF

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CN109289717B
CN109289717B CN201811125174.5A CN201811125174A CN109289717B CN 109289717 B CN109289717 B CN 109289717B CN 201811125174 A CN201811125174 A CN 201811125174A CN 109289717 B CN109289717 B CN 109289717B
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zirconium
titanium
composite aerogel
stirring
dioxide
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CN109289717A (en
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廖家轩
吴孟强
徐自强
录凯
巩峰
冯婷婷
黄雄芳
王武
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University of Electronic Science and Technology of China
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0091—Preparation of aerogels, e.g. xerogels

Abstract

A preparation method of zirconium dioxide/titanium dioxide composite aerogel belongs to the technical field of functional materials. In the preparation method of the zirconium dioxide/titanium dioxide composite aerogel provided by the invention, titanium alkoxide is used as a titanium source, and zirconyl nitrate inorganic salt is used as a zirconium source. On one hand, the selected raw materials are low in cost, stable and environment-friendly, and do not generate toxic and harmful gases; on the other hand, the zirconyl nitrate inorganic salt has the function of stabilizing titanium alkoxide, so that the hydrolysis process is controllable, gel with good transparency is obtained, and finally the gel with the specific surface area larger than 660m is prepared2Zirconium dioxide/titanium dioxide composite aerogel per gram. Meanwhile, the formation of precipitates is effectively controlled by controlling the addition amount of the propylene oxide, and the gel with excellent performance is obtained.

Description

Preparation method of zirconium dioxide/titanium dioxide composite aerogel
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to a preparation method of zirconium dioxide/titanium dioxide composite aerogel.
Background
Titanium dioxide integrates multiple functions, is called as 'gold oil', has unique photoelectric and catalytic properties, has the advantages of high activity, strong oxidizing property, high chemical stability, low cost and the like, and is well favored by various fields. However, the titanium dioxide aerogel is difficult to form a three-dimensional network structure, is easy to be powdered in the preparation process, has low strength and poor thermal stability, and the three-dimensional network structure is easy to be damaged, so that the service life and the application of the titanium dioxide aerogel are greatly limited.
The zirconium dioxide aerogel has the advantages of excellent thermal stability, chemical stability, high strength, high specific surface area, high porosity, strong environmental adaptability and the like, can be used as a catalyst and a catalyst carrier in a harsh environment, can be used as a high-temperature-resistant fireproof heat-insulating material, but has poorer catalytic activity than the titanium dioxide aerogel. Therefore, the zirconium dioxide composite titanium dioxide can greatly enhance the catalytic activity of the titanium dioxide, and the stable and firm framework structure can also enhance the thermal stability of the titanium dioxide.
At present, the main method for preparing the zirconium dioxide/titanium dioxide composite aerogel is a sol-gel method, and the zirconium dioxide/titanium dioxide composite aerogel has the advantages of low cost, high quality, uniform dispersion and the like. However, at present, the precursors for preparing the zirconium dioxide/titanium dioxide composite aerogel mainly adopt organic alkoxides of titanium and zirconium, such as tetrabutyl titanate, zirconium n-propoxide, zirconium isopropoxide and the like. On one hand, organic alkoxides of zirconium are expensive and not beneficial to industrialization; on the other hand, zirconium and titanium alkoxides are very susceptible to hydrolysis to form precipitates, which are not conducive to control of hydrolysis and polycondensation. Therefore, the need for a precursor with low cost and excellent performance is an urgent problem to be solved.
Disclosure of Invention
The invention aims to provide a preparation method of zirconium dioxide/titanium dioxide composite aerogel with low cost, stability and high specific surface area, aiming at the defects in the background technology.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the zirconium dioxide/titanium dioxide composite aerogel is characterized by comprising the following steps:
step 1, adding zirconyl nitrate hydrate into absolute ethyl alcohol, and stirring in a water bath at 40-60 ℃ until the zirconyl nitrate hydrate is completely dissolved to obtain a zirconium precursor solution with the concentration of zirconyl nitrate of 0.1-1.5 mol/L; adding titanium alkoxide into absolute ethyl alcohol, and stirring at room temperature until the titanium alkoxide is completely dissolved to obtain a titanium precursor solution, wherein the volume ratio of the titanium alkoxide to the absolute ethyl alcohol is 1: (0.5 to 10);
step 2, dropwise adding deionized water into the zirconium precursor liquid while stirring in a water bath at 40-60 ℃, continuing stirring for 1-2 min after dropwise adding, moving out of the water bath, and naturally cooling to room temperature under the stirring condition; wherein the molar ratio of the zirconyl nitrate hydrate to the dropwise added deionized water is 1: (15-120);
step 3, placing the zirconium precursor solution obtained in the step 2 in an ice bath, stirring for 5-10 min, then dropwise adding the titanium precursor solution prepared in the step 1 into the zirconium precursor solution obtained in the step 2 while stirring in the ice bath, and continuously stirring for 10-20 min after dropwise adding is completed to obtain a zirconium-titanium mixed solution; wherein the ratio n of the amounts of zirconium and titanium in the mixed solution of zirconium and titaniumZr：nTi＝1:(0.1～10)；
Step 4, under the condition of ice-bath stirring, dropwise adding epoxypropane into the zirconium-titanium mixed solution obtained in the step 3 at a dropwise adding speed of not more than 10mL/min, rapidly stirring in the dropwise adding process, and continuously stirring for 3-20 min after dropwise adding is completed to obtain zirconium-titanium sol; wherein the ratio of the sum of the amounts of zirconium and titanium species to the amount of propylene oxide species is 1: (8 to 15) i.e. (n)Zr+nTi)：nPropylene oxide＝1：(8～15)；
Step 5, standing the zirconium-titanium sol obtained in the step 4 for 10-60 min under an ice bath condition, taking out, and naturally heating to room temperature to obtain clear and transparent titanium dioxide/zirconium dioxide composite wet gel;
step 6, adding absolute ethyl alcohol into the titanium dioxide/zirconium dioxide composite wet gel obtained in the step 5 to serve as a protective aging liquid, so that the absolute ethyl alcohol can be immersed in the wet gel, and aging for 1-10 days at room temperature; soaking the wet gel in ethanol for 2-4 times for cleaning, wherein the soaking time is 12-24 h each time, and obtaining aged wet gel;
and 7, placing the aged wet gel obtained in the step 6 in a supercritical drying kettle, and performing supercritical drying to obtain the zirconium dioxide/titanium dioxide composite aerogel.
Further, the titanium alkoxide in step 1 is one of tetrabutyl titanate, isopropyl titanate and the like.
Further, in the step 1, the zirconyl nitrate hydrate is zirconyl nitrate dihydrate or zirconyl nitrate pentahydrate.
Further, in the step 7, the supercritical drying medium is carbon dioxide, the supercritical drying temperature is 35-50 ℃, and the pressure is 8-15 MPa.
Compared with the prior art, the invention has the beneficial effects that:
1. in the preparation method of the zirconium dioxide/titanium dioxide composite aerogel provided by the invention, titanium alkoxide is used as a titanium source, and zirconyl nitrate inorganic salt is used as a zirconium source. On one hand, the selected raw materials are low in cost, stable and environment-friendly, and do not generate toxic and harmful gases; on the other hand, the zirconyl nitrate inorganic salt has the function of stabilizing titanium alkoxide, so that the hydrolysis process is controllable, gel with good transparency is obtained, and finally the gel with the specific surface area larger than 660m is prepared2Zirconium dioxide/titanium dioxide composite aerogel per gram.
2. In the preparation method of the zirconium dioxide/titanium dioxide composite aerogel provided by the invention, the formation of precipitates is effectively controlled by controlling the addition amount of propylene oxide, and meanwhile, gel with excellent performance is obtained.
3. In the preparation method of the zirconium dioxide/titanium dioxide composite aerogel provided by the invention, no additional catalyst is required to be added in the preparation process of the zirconium-titanium mixed solution, so that the process flow is simplified, and the cost is further reduced.
4. In the preparation method of the zirconium dioxide/titanium dioxide composite aerogel provided by the invention, the zirconium-titanium sol is stood in ice bath and then naturally heated to room temperature, so that the temperature of a reaction system is effectively ensured, and the hydrolysis polycondensation rate is controlled; meanwhile, the performance of the gel is improved by controlling the addition amount of the propylene oxide, and finally the composite aerogel with larger specific surface area is obtained.
Drawings
FIG. 1 is a diagram illustrating the pore size distribution of a zirconium dioxide/titanium dioxide composite aerogel obtained in example 1 of the present invention;
FIG. 2 is an XRD spectrum of the zirconium dioxide/titanium dioxide composite aerogel obtained in example 1 of the present invention;
FIG. 3 is an SEM image of the zirconium dioxide/titanium dioxide composite aerogel obtained in example 1 of the present invention;
FIG. 4 is a diagram illustrating the pore size distribution of the zirconium dioxide/titanium dioxide composite aerogel obtained in example 2 of the present invention;
FIG. 5 is an XRD spectrum of the zirconium dioxide/titanium dioxide composite aerogel obtained in example 2 of the present invention;
FIG. 6 is an SEM image of a zirconium dioxide/titanium dioxide composite aerogel obtained in example 2 of the present invention;
FIG. 7 is a pore size distribution diagram of a zirconium dioxide/titanium dioxide composite aerogel obtained by a comparative example.
Detailed Description
The technical scheme of the invention is detailed below by combining the accompanying drawings and the embodiment.
Example 1
The preparation method of the zirconium dioxide/titanium dioxide composite aerogel is characterized by comprising the following steps:
step 1, adding 5.49g of zirconyl nitrate pentahydrate into 20mL of absolute ethyl alcohol, and stirring in a water bath at 60 ℃ until the zirconyl precursor is completely dissolved to obtain a zirconium precursor solution; adding 5.07mL of tetrabutyl titanate into 10mL of absolute ethyl alcohol, and stirring at room temperature until the tetrabutyl titanate is completely dissolved to obtain a titanium precursor solution;
step 2, dropwise adding 6mL of deionized water into the zirconium precursor solution obtained in the step 1 while stirring in a water bath at 60 ℃, continuing stirring for 2min after dropwise adding, moving out of the water bath, and naturally cooling to room temperature under the stirring condition;
step 3, placing the zirconium precursor solution obtained in the step 2 in an ice bath and stirring for 10min, then dropwise adding the titanium precursor solution prepared in the step 1 into the zirconium precursor solution obtained in the step 2 while stirring in the ice bath, and continuously stirring for 20min after dropwise adding is completed to obtain a zirconium-titanium mixed solution;
step 4, under the condition of ice-bath stirring, dropwise adding 20mL of propylene oxide into the zirconium-titanium mixed solution obtained in the step 3 at a dropwise adding speed of not more than 10mL/min, rapidly stirring in the dropwise adding process, and continuously stirring for 5min after dropwise adding is completed to obtain zirconium-titanium sol;
step 5, standing the zirconium-titanium sol obtained in the step 4 for 30min under an ice bath condition, and naturally heating to room temperature to obtain clear and transparent titanium dioxide/zirconium dioxide composite wet gel;
step 6, adding absolute ethyl alcohol into the titanium dioxide/zirconium dioxide composite wet gel obtained in the step 5 to serve as a protective aging liquid, so that the absolute ethyl alcohol is 1-2 cm higher than the wet gel, and aging for 2 days at room temperature; soaking the wet gel in 100mL of ethanol for 3 times for cleaning, wherein the soaking time is 24h each time, so as to obtain aged wet gel;
step 7, placing the aged wet gel obtained in the step 6 into a supercritical drying kettle, and performing supercritical drying to obtain the zirconium dioxide/titanium dioxide composite aerogel; wherein the supercritical drying medium is carbon dioxide, the supercritical drying temperature is 45 ℃, the pressure is 12MPa, the carbon dioxide flow is 10L/h, and the drying time is 12 h.
FIG. 1 is a diagram illustrating the pore size distribution of a zirconium dioxide/titanium dioxide composite aerogel obtained in example 1 of the present invention; as can be seen from FIG. 1, the zirconia/titania composite aerogel obtained in example 1 had a specific surface area of 529.3m2The pore diameter of micropores of the SF method is mostly distributed between 1nm and 1.3nm, the pore diameter of mesopores desorbed by the BJH method is mostly distributed between 8nm and 12nm, and the obtained aerogel is a nano mesoporous material.
FIG. 2 is an XRD spectrum of the zirconium dioxide/titanium dioxide composite aerogel obtained in example 1 of the present invention; as can be seen from fig. 2, the zirconium dioxide/titanium dioxide composite aerogel obtained in example 1 is an amorphous material.
FIG. 3 is an SEM image of the zirconium dioxide/titanium dioxide composite aerogel obtained in example 1 of the present invention; as can be seen from fig. 3, the surface of the zirconium dioxide/titanium dioxide composite aerogel obtained in example 1 has a porous structure.
Example 2
This example is different from example 1 in that: adding 4.28mL of isopropyl titanate into 10mL of absolute ethyl alcohol in the step 1, and stirring at room temperature until the isopropyl titanate is completely dissolved to obtain a titanium precursor solution; the rest of the procedure was the same as in example 1.
FIG. 4 shows example 2 of the present inventionThe aperture distribution map of the obtained zirconium dioxide/titanium dioxide composite aerogel; as can be seen from FIG. 2, the zirconia/titania composite aerogel obtained in example 2 had a specific surface area of 664.1m2The pore diameter of micropores of the SF method is mostly distributed between 1.5nm and 2nm, the pore diameter of mesopores desorbed by the BJH method is mostly distributed between 9nm and 15nm, and the obtained aerogel is a nano mesoporous material.
FIG. 5 is an XRD spectrum of the zirconium dioxide/titanium dioxide composite aerogel obtained in example 2 of the present invention; as can be seen from fig. 5, the zirconium dioxide/titanium dioxide composite aerogel obtained in example 2 is an amorphous material.
FIG. 6 is an SEM image of a zirconium dioxide/titanium dioxide composite aerogel obtained in example 2 of the present invention; as can be seen from fig. 6, the surface of the zirconium dioxide/titanium dioxide composite aerogel obtained in example 2 has a porous structure.
Example 3
This example is different from example 1 in that: in the step 1, 7.39g of zirconyl nitrate pentahydrate is added into 20mL of absolute ethyl alcohol, and stirred in a water bath at 60 ℃ until the zirconyl precursor solution is completely dissolved to obtain a zirconium precursor solution; adding 3.17mL of tetrabutyl titanate into 10mL of absolute ethyl alcohol, and stirring at room temperature until the tetrabutyl titanate is completely dissolved to obtain a titanium precursor solution; the rest of the procedure was the same as in example 1.
Example 3 the composite aerogel prepared has a specific surface area of 659.7m2/g。
Example 4
This example is different from example 1 in that: in the step 1, 3.17g of zirconyl nitrate pentahydrate is added into 20mL of absolute ethyl alcohol, and stirred in a water bath at 60 ℃ until the zirconyl precursor solution is completely dissolved to obtain a zirconium precursor solution; adding 7.39mL of tetrabutyl titanate into 10mL of absolute ethyl alcohol, and stirring at room temperature until the tetrabutyl titanate is completely dissolved to obtain a titanium precursor solution; the rest of the procedure was the same as in example 1.
The specific surface area of the composite aerogel prepared in example 4 is 612.4m2/g。
Example 5
This example is different from example 1 in that: in the step 1, 1.07g of zirconyl nitrate pentahydrate is added into 20mL of absolute ethyl alcohol, and stirred in a water bath at 60 ℃ until the zirconyl precursor solution is completely dissolved to obtain a zirconium precursor solution; adding 9.5mL of isopropyl titanate into 10mL of absolute ethyl alcohol, and stirring at room temperature until the isopropyl titanate is completely dissolved to obtain a titanium precursor solution; the rest of the procedure was the same as in example 1.
Example 6
This example is different from example 1 in that: in the step 1, 9.51g of zirconyl nitrate pentahydrate is added into 20mL of absolute ethyl alcohol, and stirred in a water bath at 60 ℃ until the zirconyl precursor solution is completely dissolved to obtain a zirconium precursor solution; adding 1.1mL of isopropyl titanate into 10mL of absolute ethyl alcohol, and stirring at room temperature until the isopropyl titanate is completely dissolved to obtain a titanium precursor solution; the rest of the procedure was the same as in example 1.
Comparative example
The comparative example is different from example 1 in that: the procedure of example 1 was repeated except that "dehydrated alcohol" in step 1 was changed to "ethylene glycol methyl ether".
FIG. 7 is a diagram showing the pore size distribution of a zirconium dioxide/titanium dioxide composite aerogel obtained by a comparative example of the present invention; as can be seen from FIG. 7, the zirconia/titania composite aerogel obtained in the comparative example had a specific surface area of only 422.4m2/g。
The above-described embodiments are merely illustrative of the principles of the present invention and the results thereof, and are not intended to limit the scope of the practice of the invention.
In the preparation method of the zirconium dioxide/titanium dioxide composite aerogel provided by the invention, the zirconyl nitrate inorganic salt is used as a zirconium source, so that the raw material cost is low, the method is stable and environment-friendly, and toxic and harmful gases are not generated; meanwhile, the zirconyl nitrate inorganic salt has the function of stabilizing titanium alkoxide, so that the hydrolysis process is controllable, gel with good transparency is obtained, and the final preparation method obtains the gel with the specific surface area of more than 660m2Zirconium dioxide/titanium dioxide composite aerogel per gram.

Claims (4)

1. The preparation method of the zirconium dioxide/titanium dioxide composite aerogel is characterized by comprising the following steps:
step 1, adding zirconyl nitrate hydrate into absolute ethyl alcohol, and stirring in a water bath at 40-60 ℃ until the zirconyl nitrate hydrate is completely dissolved to obtain a zirconium precursor solution with the concentration of 0.1-1.5 mol/L; adding titanium alkoxide into absolute ethyl alcohol, and stirring at room temperature until the titanium alkoxide is completely dissolved to obtain a titanium precursor solution, wherein the volume ratio of the titanium alkoxide to the absolute ethyl alcohol is 1: (0.5 to 10);
step 2, dropwise adding deionized water into the zirconium precursor liquid while stirring in a water bath at 40-60 ℃, continuing stirring for 1-2 min after dropwise adding, moving out of the water bath, and naturally cooling to room temperature; wherein the molar ratio of the zirconyl nitrate hydrate to the dropwise added deionized water is 1: (15-120);
step 3, placing the zirconium precursor solution obtained in the step 2 in an ice bath, stirring for 5-10 min, then dropwise adding the titanium precursor solution prepared in the step 1 into the zirconium precursor solution obtained in the step 2 while stirring in the ice bath, and continuously stirring for 10-20 min after dropwise adding is completed to obtain a zirconium-titanium mixed solution; wherein n in the mixed solution of zirconium and titaniumZr：nTi＝1:(0.1～10)；
Step 4, under the condition of ice-bath stirring, dropwise adding propylene oxide into the zirconium-titanium mixed solution obtained in the step 3 at a speed of not more than 10mL/min, and after dropwise adding is completed, continuously stirring for 3-20 min to obtain zirconium-titanium sol; wherein (n)Zr+nTi)：nPropylene oxide＝1：(8～15)；
Step 5, standing the zirconium-titanium sol obtained in the step 4 for 10-60 min under an ice bath condition, taking out, and naturally heating to room temperature to obtain clear and transparent titanium dioxide/zirconium dioxide composite wet gel;
step 6, adding absolute ethyl alcohol into the composite wet gel obtained in the step 5 to serve as a protective aging liquid, and aging for 1-10 days at room temperature; soaking the wet gel in absolute ethyl alcohol for 2-4 times for cleaning, wherein the soaking time is 12-24 h each time, and obtaining aged wet gel;
and 7, placing the aged wet gel obtained in the step 6 in a supercritical drying kettle, and performing supercritical drying to obtain the zirconium dioxide/titanium dioxide composite aerogel.
2. The method for preparing zirconium dioxide/titanium dioxide composite aerogel according to claim 1, wherein the titanium alkoxide in step 1 is tetrabutyl titanate or isopropyl titanate.
3. The method for preparing zirconium dioxide/titanium dioxide composite aerogel according to claim 1, wherein the zirconyl nitrate hydrate in step 1 is zirconyl nitrate dihydrate or zirconyl nitrate pentahydrate.
4. The preparation method of the zirconium dioxide/titanium dioxide composite aerogel according to claim 1, wherein the supercritical drying medium in the step 7 is carbon dioxide, the supercritical drying temperature is 35-50 ℃, and the pressure is 8-15 MPa.
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