CN108002431B - A kind of preparation method of richness titanium metatitanic acid alumina supporter - Google Patents
A kind of preparation method of richness titanium metatitanic acid alumina supporter Download PDFInfo
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Abstract
The preparation method of a kind of rich titanium metatitanic acid alumina supporter disclosed by the invention, comprising the following steps: step 1, prepare titanium sol solutions and nano-titanium dioxide suspension parcel-like；Step 2, Aluminum sol is put into reaction kettle, then sequentially adds nano-titanium dioxide suspension and silester, obtains mixed liquor；Mixed liquor is evaporated under reduced pressure and is reacted, viscous fluid is obtained；Step 3, porous roughcast is prepared；Step 4, plated film roughcast is prepared；Step 5, plated film roughcast is subjected to gradient sintering to get porous rich titanium aluminium titanates is arrived.Preparation method of the invention, compared to traditional carrier coating method, provide it is a kind of so that titanium elements is connected with carrier the method for priority processing, not only step is simple, and technique is easily realized；Using gradient sintering method, obtaining aluminium titanates, not only titaniferous amount is high, but also stomata is uniform, and intensity improves, and has good use value.
Description
Technical field
The invention belongs to aluminium titanates support preparation method technical fields, and in particular to a kind of preparation of richness titanium metatitanic acid alumina supporter
Method.
Background technique
With the fast development in the fields such as contemporary metal smelting, aerospace and auto industry, to the performance of ceramic material
Required standard be continuously improved, especially high temperature resistant and in terms of.Aluminium titanates (Al2TiO5) material melting point height, anti-impact
It hits and thermal shock resistance is good, these advantages make it have very big answer at higher temperature and frequent cold and hot give-and-take conditions
Use potentiality.Furthermore material of aluminum titanate also has many advantages, such as low expansion and fire resisting, anti-corrosion, alkaline-resisting, so material of aluminum titanate is also wide
General is applied to refractory brick and chemical industry.Porous alumina titanate ceramics has relative density low, and specific surface area is high, good penetrability,
And superior adsorptivity, while having many advantages, such as that material of aluminum titanate fusing point is high, shock resistance and thermal shock resistance are good, are widely applied
In following field: (1) filtering, purify, separation；(2) catalytic carrier, absorption carrier；(3) high-quality thermal insulating material, sensing material.
Noble metal catalyst is most important catalyst in petrochemical industry, using noble metal as activated centre, is had good
Catalytic effect, with the development of science and technology, double activity center's structure based on noble metal, supplemented by titanium elements becomes main research
Object.Current preparation method mainly uses carrier coating method, but the priority processing technique that titanium elements are connected with carrier is also
There is not disclosure.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of rich titanium metatitanic acid alumina supporter, improve traditional carrier plated film side
Cannot make in method titanium elements connect with carrier priority processing the problem of.
The technical scheme adopted by the invention is that a kind of preparation method of richness titanium metatitanic acid alumina supporter, comprising the following steps:
Step 1, titanium sol solutions and nano-titanium dioxide suspension parcel-like are prepared
Step 1.1, tetrabutyl titanate is added in dehydrated alcohol, dispersing agent is then added, then carry out ultrasonic reaction
Titanium sol solutions parcel-like are formed, it is spare；
Step 1.2, nano-titanium dioxide is added to absolute ethanol, then it is suspended to obtain nano-titanium dioxide for ultrasonic disperse
Liquid, it is spare；
Step 2, Aluminum sol is put into reaction kettle, the nano-titanium dioxide suspension of step 1.2 is then added, stirring is equal
Silester is added after even, ultrasonic reaction obtains mixed liquor；Mixed liquor is evaporated under reduced pressure and is reacted, viscous fluid is obtained；
Step 3, porous roughcast is prepared
Viscous fluid in step 2 is put into ultrasonic curing in mold to react, constant pressure heating reaction is then carried out, obtains porous
Roughcast；
Step 4, plated film roughcast is prepared
The porous roughcast of step 3 is immersed in the titanium colloidal sol parcel-like of step 1.1, rapid curing is then taken out, obtains
Plated film roughcast；
Step 5, the plated film roughcast of step 4 is subjected to gradient sintering to get porous rich titanium aluminium titanates is arrived.
It is of the invention to be further characterized in that,
Mass concentration of the tetrabutyl titanate in titanium sol solutions parcel-like is 10-20g/L in step 1.1, wherein dispersing agent
Specially polyvinylpyrrolidone, dispersing agent addition concentration be 0.5-1.5g/L；
Ultrasonic reaction parameter: pressure 3-5MPa, temperature are 60-80 DEG C, frequency 2.5-5.5kHz.
Mass concentration of the nano-titanium dioxide in nano-titanium dioxide suspension is 20-40g/L, ultrasound in step 1.2
Dispersion frequency is 8-16kHz.
Silester in step 2, aluminium ion in Aluminum sol, in nano-titanium dioxide suspension nano-titanium dioxide quality
Than for 0.05-0.15:1:1, ultrasonic reaction frequency is 10-20kHz, ultrasonic reaction time 10-15min.
The parameter of reaction is evaporated under reduced pressure in step 2 are as follows: time 3-5h, pressure are the 20-40% of standard atmospheric pressure, temperature
50-80℃。
Ultrasonic curing response parameter in step 3: supersonic frequency 2-8MHz, temperature are 120-150 DEG C, ultrasonic time 2-
4h；The constant pressure heating response parameter: 200-250 DEG C of temperature, pressure 0.4-0.8Mpa, time 2-3h.
Rapid curing temperature is 110-140 DEG C in step 4, curing time 10-20min.
Gradient sintering parameter in step 5 are as follows:
First gradient: 200-240 DEG C of sintering temperature, sintering time 40-60min；Second gradient: sintering temperature 400-500
DEG C, sintering time 60-80min；3rd gradient: 1000-1100 DEG C of sintering temperature, sintering time 120-150min；4th gradient:
1200-1400 DEG C of sintering temperature, sintering time 240-300min.
The beneficial effects of the present invention are: a kind of preparation method of rich titanium metatitanic acid alumina supporter of the present invention, compared to traditional load
Body coating method, provide it is a kind of so that titanium elements is connected with carrier the method for priority processing, not only step is simple, and technique is easily realized；
Using gradient sintering method, obtaining aluminium titanates, not only titaniferous amount is high, but also stomata is uniform, and intensity improves, and has and uses valence well
Value.
Specific embodiment
Below by specific embodiment, the present invention is described in detail.
A kind of preparation method of rich titanium metatitanic acid alumina supporter of the present invention, comprising the following steps:
Step 1, titanium sol solutions and nano-titanium dioxide suspension parcel-like are prepared
Step 1.1, tetrabutyl titanate is added in dehydrated alcohol, dispersing agent is then added, then carry out ultrasonic reaction
Titanium sol solutions parcel-like are formed, it is spare；Wherein mass concentration of the tetrabutyl titanate in titanium sol solutions parcel-like is 10-20g/L,
Dispersing agent be specially polyvinylpyrrolidone, dispersing agent addition concentration be 0.5-1.5g/L；Ultrasonic reaction parameter: pressure 3-
5MPa, temperature are 60-80 DEG C, frequency 2.5-5.5kHz.
Step 1.2, nano-titanium dioxide is added to absolute ethanol, then it is suspended to obtain nano-titanium dioxide for ultrasonic disperse
Liquid, it is spare；Wherein mass concentration of the nano-titanium dioxide in nano-titanium dioxide suspension is 20-40g/L, ultrasonic disperse frequency
Rate is 8-16kHz.
Step 2, Aluminum sol is put into reaction kettle, the nano-titanium dioxide suspension of step 1.2 is then added, stirring is equal
Silester is added after even, ultrasonic reaction obtains mixed liquor；Mixed liquor is evaporated under reduced pressure and is reacted, viscous fluid is obtained；Wherein silicic acid
Aluminium ion in ethyl ester, Aluminum sol, the mass ratio of nano-titanium dioxide is 0.05-0.15:1:1 in nano-titanium dioxide suspension,
Ultrasonic reaction frequency is 10-20kHz, ultrasonic reaction time 10-15min；It is evaporated under reduced pressure the parameter of reaction are as follows: time 3-5h, pressure
Power is the 20-40% of standard atmospheric pressure, 50-80 DEG C of temperature.
Step 3, porous roughcast is prepared
Viscous fluid in step 2 is put into ultrasonic curing in mold to react, constant pressure heating reaction is then carried out, obtains porous
Roughcast；Wherein ultrasonic curing response parameter: supersonic frequency 2-8MHz, temperature are 120-150 DEG C, ultrasonic time 2-4h；It is described
Constant pressure heating response parameter: 200-250 DEG C of temperature, pressure 0.4-0.8Mpa, time 2-3h.
Step 4, plated film roughcast is prepared
The porous roughcast of step 3 is immersed in the titanium colloidal sol parcel-like of step 1.1, rapid curing is then taken out, obtains
Plated film roughcast；Rapid curing temperature is 110-140 DEG C, curing time 10-20min.
Step 5, the plated film roughcast of step 4 is subjected to gradient sintering to get to porous rich titanium aluminium titanates, wherein gradient sintering
Parameter are as follows:
First gradient: 200-240 DEG C of sintering temperature, sintering time 40-60min；Second gradient: sintering temperature 400-500
DEG C, sintering time 60-80min；3rd gradient: 1000-1100 DEG C of sintering temperature, sintering time 120-150min；4th gradient:
1200-1400 DEG C of sintering temperature, sintering time 240-300min.
Embodiment 1
(1) titanium sol solutions parcel-like are prepared
Tetrabutyl titanate is added in dehydrated alcohol, polyethylene of dispersing agent pyrrolidones is then added, is then surpassed
Phonoresponse forms titanium sol solutions parcel-like, spare.
Wherein mass concentration of the tetrabutyl titanate in titanium sol solutions parcel-like is 10g/L, and the addition concentration of dispersing agent is
0.5g/L；Ultrasonic reaction parameter: pressure 3MPa, temperature are 60 DEG C, frequency 2.5kHz.
(2) nano-titanium dioxide suspension is prepared
Nano-titanium dioxide is added to absolute ethanol, then ultrasonic disperse obtains nano-titanium dioxide suspension, spare.
Wherein mass concentration of the nano-titanium dioxide in nano-titanium dioxide suspension is 20g/L, ultrasonic disperse frequency
For 8kHz.
(3) Aluminum sol is put into reaction kettle, nano-titanium dioxide suspension is then added, is stirring evenly and then adding into silicic acid
Ethyl ester, ultrasonic reaction obtain mixed liquor；Mixed liquor is evaporated under reduced pressure and is reacted, viscous fluid is obtained.
Wherein silester, aluminium ion in Aluminum sol, in nano-titanium dioxide suspension nano-titanium dioxide mass ratio
For 0.05:1:1, ultrasonic reaction frequency is 10kHz, ultrasonic reaction time 10min；It is evaporated under reduced pressure the parameter of reaction are as follows: time 3h,
Pressure is the 20% of standard atmospheric pressure, temperature 50 C.
(4) porous roughcast is prepared
Viscous fluid is put into ultrasonic curing in mold to react, constant pressure heating reaction is then carried out, obtains porous roughcast.
Wherein ultrasonic curing response parameter: supersonic frequency 2MHz, temperature are 120 DEG C, ultrasonic time 2h；Constant pressure heating is anti-
Answer parameter: 200 DEG C of temperature, pressure 0.4Mpa, time 2h.
(5) plated film roughcast is prepared
Porous roughcast is immersed in titanium colloidal sol parcel-like, rapid curing is then taken out, obtains plated film roughcast；Rapid curing
Temperature is 110 DEG C, curing time 10min.
(6) plated film roughcast is subjected to gradient sintering to get porous rich titanium aluminium titanates is arrived.
Wherein gradient sintering parameter are as follows:
First gradient: 200 DEG C of sintering temperature, sintering time 60min；
Second gradient: 400 DEG C of sintering temperature, sintering time 80min；
3rd gradient: 1000 DEG C of sintering temperature, sintering time 150min；
4th gradient: 1200 DEG C of sintering temperature, sintering time 300min.
Embodiment 2
(1) titanium sol solutions parcel-like are prepared
Tetrabutyl titanate is added in dehydrated alcohol, polyethylene of dispersing agent pyrrolidones is then added, is then surpassed
Phonoresponse forms titanium sol solutions parcel-like, spare.
Wherein mass concentration of the tetrabutyl titanate in titanium sol solutions parcel-like is 13g/L, and the addition concentration of dispersing agent is
0.8g/L；Ultrasonic reaction parameter: pressure 4.5MPa, temperature are 65 DEG C, frequency 3.5kHz.
(2) nano-titanium dioxide suspension is prepared
Nano-titanium dioxide is added to absolute ethanol, then ultrasonic disperse obtains nano-titanium dioxide suspension, spare.
Wherein mass concentration of the nano-titanium dioxide in nano-titanium dioxide suspension is 25g/L, ultrasonic disperse frequency
For 10kHz.
(3) Aluminum sol is put into reaction kettle, nano-titanium dioxide suspension is then added, is stirring evenly and then adding into silicic acid
Ethyl ester, ultrasonic reaction obtain mixed liquor；Mixed liquor is evaporated under reduced pressure and is reacted, viscous fluid is obtained.
Wherein silester, aluminium ion in Aluminum sol, in nano-titanium dioxide suspension nano-titanium dioxide mass ratio
For 0.08:1:1, ultrasonic reaction frequency is 12kHz, ultrasonic reaction time 11min；It is evaporated under reduced pressure the parameter of reaction are as follows: the time
3.5h, pressure are the 25% of standard atmospheric pressure, temperature 60 C.
(4) porous roughcast is prepared
Viscous fluid is put into ultrasonic curing in mold to react, constant pressure heating reaction is then carried out, obtains porous roughcast.
Wherein ultrasonic curing response parameter: supersonic frequency 4MHz, temperature are 130 DEG C, ultrasonic time 2.5h；Constant pressure heating
Response parameter: 210 DEG C of temperature, pressure 0.5Mpa, time 2.2h.
(5) plated film roughcast is prepared
Porous roughcast is immersed in titanium colloidal sol parcel-like, rapid curing is then taken out, obtains plated film roughcast；Rapid curing
Temperature is 120 DEG C, curing time 12min.
(6) plated film roughcast is subjected to gradient sintering to get porous rich titanium aluminium titanates is arrived.
Wherein gradient sintering parameter are as follows:
First gradient: 210 DEG C of sintering temperature, sintering time 55min；
Second gradient: 420 DEG C of sintering temperature, sintering time 75min；
3rd gradient: 1030 DEG C of sintering temperature, sintering time 140min；
4th gradient: 1250 DEG C of sintering temperature, sintering time 280min.
Embodiment 3
(1) titanium sol solutions parcel-like are prepared
Tetrabutyl titanate is added in dehydrated alcohol, polyethylene of dispersing agent pyrrolidones is then added, is then surpassed
Phonoresponse forms titanium sol solutions parcel-like, spare.
Wherein mass concentration of the tetrabutyl titanate in titanium sol solutions parcel-like is 15g/L, and the addition concentration of dispersing agent is
1g/L；Ultrasonic reaction parameter: pressure 3.5MPa, temperature are 70 DEG C, frequency 4.5kHz.
(2) nano-titanium dioxide suspension is prepared
Nano-titanium dioxide is added to absolute ethanol, then ultrasonic disperse obtains nano-titanium dioxide suspension, spare.
Wherein mass concentration of the nano-titanium dioxide in nano-titanium dioxide suspension is 30g/L, ultrasonic disperse frequency
For 10kHz.
(3) Aluminum sol is put into reaction kettle, nano-titanium dioxide suspension is then added, is stirring evenly and then adding into silicic acid
Ethyl ester, ultrasonic reaction obtain mixed liquor；Mixed liquor is evaporated under reduced pressure and is reacted, viscous fluid is obtained.
Wherein silester, aluminium ion in Aluminum sol, in nano-titanium dioxide suspension nano-titanium dioxide mass ratio
For 0.1:1:1, ultrasonic reaction frequency is 15kHz, ultrasonic reaction time 13min；It is evaporated under reduced pressure the parameter of reaction are as follows: time 4h,
Pressure is the 30% of standard atmospheric pressure, temperature 70 C.
(4) porous roughcast is prepared
Viscous fluid is put into ultrasonic curing in mold to react, constant pressure heating reaction is then carried out, obtains porous roughcast.
Wherein ultrasonic curing response parameter: supersonic frequency 6MHz, temperature are 130 DEG C, ultrasonic time 3h；Constant pressure heating is anti-
Answer parameter: 230 DEG C of temperature, pressure 0.5Mpa, time 2.5h.
(5) plated film roughcast is prepared
Porous roughcast is immersed in titanium colloidal sol parcel-like, rapid curing is then taken out, obtains plated film roughcast；Rapid curing
Temperature is 125 DEG C, curing time 15min.
(6) plated film roughcast is subjected to gradient sintering to get porous rich titanium aluminium titanates is arrived.
Wherein gradient sintering parameter are as follows:
First gradient: 230 DEG C of sintering temperature, sintering time 50min；
Second gradient: 450 DEG C of sintering temperature, sintering time 70min；
3rd gradient: 1050 DEG C of sintering temperature, sintering time 140min；
4th gradient: 1300 DEG C of sintering temperature, sintering time 260min.
Embodiment 4
(1) titanium sol solutions parcel-like are prepared
Tetrabutyl titanate is added in dehydrated alcohol, polyethylene of dispersing agent pyrrolidones is then added, is then surpassed
Phonoresponse forms titanium sol solutions parcel-like, spare.
Wherein mass concentration of the tetrabutyl titanate in titanium sol solutions parcel-like is 18g/L, and the addition concentration of dispersing agent is
1.2g/L；Ultrasonic reaction parameter: pressure 4MPa, temperature are 75 DEG C, frequency 5kHz.
(2) nano-titanium dioxide suspension is prepared
Nano-titanium dioxide is added to absolute ethanol, then ultrasonic disperse obtains nano-titanium dioxide suspension, spare.
Wherein mass concentration of the nano-titanium dioxide in nano-titanium dioxide suspension is 35g/L, ultrasonic disperse frequency
For 14kHz.
(3) Aluminum sol is put into reaction kettle, nano-titanium dioxide suspension is then added, is stirring evenly and then adding into silicic acid
Ethyl ester, ultrasonic reaction obtain mixed liquor；Mixed liquor is evaporated under reduced pressure and is reacted, viscous fluid is obtained.
Wherein silester, aluminium ion in Aluminum sol, in nano-titanium dioxide suspension nano-titanium dioxide mass ratio
For 0.12:1:1, ultrasonic reaction frequency is 18kHz, ultrasonic reaction time 14min；It is evaporated under reduced pressure the parameter of reaction are as follows: the time
4.5h, pressure are the 35% of standard atmospheric pressure, 75 DEG C of temperature.
(4) porous roughcast is prepared
Viscous fluid is put into ultrasonic curing in mold to react, constant pressure heating reaction is then carried out, obtains porous roughcast.
Wherein ultrasonic curing response parameter: supersonic frequency 6MHz, temperature are 145 DEG C, ultrasonic time 3.5h；Constant pressure heating
Response parameter: 240 DEG C of temperature, pressure 0.7Mpa, time 2.8h.
(5) plated film roughcast is prepared
Porous roughcast is immersed in titanium colloidal sol parcel-like, rapid curing is then taken out, obtains plated film roughcast；Rapid curing
Temperature is 130 DEG C, curing time 18min.
(6) plated film roughcast is subjected to gradient sintering to get porous rich titanium aluminium titanates is arrived.
Wherein gradient sintering parameter are as follows:
First gradient: 230 DEG C of sintering temperature, sintering time 45min；
Second gradient: 480 DEG C of sintering temperature, sintering time 65min；
3rd gradient: 1080 DEG C of sintering temperature, sintering time 130min；
4th gradient: 1350 DEG C of sintering temperature, sintering time 260min.
Embodiment 5
(1) titanium sol solutions parcel-like are prepared
Tetrabutyl titanate is added in dehydrated alcohol, polyethylene of dispersing agent pyrrolidones is then added, is then surpassed
Phonoresponse forms titanium sol solutions parcel-like, spare.
Wherein mass concentration of the tetrabutyl titanate in titanium sol solutions parcel-like is 20g/L, and the addition concentration of dispersing agent is
1.5g/L；Ultrasonic reaction parameter: pressure 5MPa, temperature are 80 DEG C, frequency 5.5kHz.
(2) nano-titanium dioxide suspension is prepared
Nano-titanium dioxide is added to absolute ethanol, then ultrasonic disperse obtains nano-titanium dioxide suspension, spare.
Wherein mass concentration of the nano-titanium dioxide in nano-titanium dioxide suspension is 40g/L, ultrasonic disperse frequency
For 16kHz.
(3) Aluminum sol is put into reaction kettle, nano-titanium dioxide suspension is then added, is stirring evenly and then adding into silicic acid
Ethyl ester, ultrasonic reaction obtain mixed liquor；Mixed liquor is evaporated under reduced pressure and is reacted, viscous fluid is obtained.
Wherein silester, aluminium ion in Aluminum sol, in nano-titanium dioxide suspension nano-titanium dioxide mass ratio
For 0.15:1:1, ultrasonic reaction frequency is 20kHz, ultrasonic reaction time 15min；It is evaporated under reduced pressure the parameter of reaction are as follows: time 5h,
Pressure is the 40% of standard atmospheric pressure, 80 DEG C of temperature.
(4) porous roughcast is prepared
Viscous fluid is put into ultrasonic curing in mold to react, constant pressure heating reaction is then carried out, obtains porous roughcast.
Wherein ultrasonic curing response parameter: supersonic frequency 8MHz, temperature are 150 DEG C, ultrasonic time 4h；Constant pressure heating is anti-
Answer parameter: 250 DEG C of temperature, pressure 0.8Mpa, time 3h.
(5) plated film roughcast is prepared
Porous roughcast is immersed in titanium colloidal sol parcel-like, rapid curing is then taken out, obtains plated film roughcast；Rapid curing
Temperature is 140 DEG C, curing time 20min.
(6) plated film roughcast is subjected to gradient sintering to get porous rich titanium aluminium titanates is arrived.
Wherein gradient sintering parameter are as follows:
First gradient: 240 DEG C of sintering temperature, sintering time 40min；
Second gradient: 500 DEG C of sintering temperature, sintering time 60min；
3rd gradient: 1100 DEG C of sintering temperature, sintering time 120min；
4th gradient: 1400 DEG C of sintering temperature, sintering time 240min.
The rich titanium metatitanic acid alumina supporter prepared by embodiment 1-5, not only step is simple, and technique is easily realized；It is burnt using gradient
Knot method, obtaining aluminium titanates, not only titaniferous amount is high, but also stomata is uniform, and intensity improves, and has good practical value.
Claims (8)
1. a kind of preparation method of richness titanium metatitanic acid alumina supporter, which comprises the following steps:
Step 1, titanium sol solutions and nano-titanium dioxide suspension parcel-like are prepared
Step 1.1, tetrabutyl titanate is added in dehydrated alcohol, dispersing agent is then added, then carried out ultrasonic reaction and formed
Titanium sol solutions parcel-like, it is spare；
Step 1.2, nano-titanium dioxide is added to absolute ethanol, then ultrasonic disperse obtains nano-titanium dioxide suspension,
It is spare；
Step 2, Aluminum sol is put into reaction kettle, the nano-titanium dioxide suspension of step 1.2 is then added, after mixing evenly
Silester is added, ultrasonic reaction obtains mixed liquor；Mixed liquor is evaporated under reduced pressure and is reacted, viscous fluid is obtained；
Step 3, porous roughcast is prepared
Viscous fluid in step 2 is put into ultrasonic curing in mold to react, then carries out constant pressure heating reaction, is obtained porous thick
Mould；
Step 4, plated film roughcast is prepared
The porous roughcast of step 3 is immersed in the titanium colloidal sol parcel-like of step 1.1, rapid curing is then taken out, obtains plated film
Roughcast；
Step 5, the plated film roughcast of step 4 is subjected to gradient sintering to get porous rich titanium aluminium titanates is arrived.
2. a kind of preparation method of rich titanium metatitanic acid alumina supporter according to claim 1, which is characterized in that the step 1.1
Mass concentration of the middle tetrabutyl titanate in titanium sol solutions parcel-like is 10-20g/L, and wherein dispersing agent is specially polyvinyl pyrrole
Alkanone, the addition concentration of dispersing agent are 0.5-1.5g/L；
The ultrasonic reaction parameter: pressure 3-5MPa, temperature are 60-80 DEG C, frequency 2.5-5.5kHz.
3. a kind of preparation method of rich titanium metatitanic acid alumina supporter according to claim 1, which is characterized in that the step 1.2
Mass concentration of the middle nano-titanium dioxide in nano-titanium dioxide suspension is 20-40g/L, and ultrasonic disperse frequency is 8-
16kHz。
4. a kind of preparation method of rich titanium metatitanic acid alumina supporter according to claim 1, which is characterized in that in the step 2
Aluminium ion in silester, Aluminum sol, the mass ratio of nano-titanium dioxide is 0.05-0.15 in nano-titanium dioxide suspension:
1:1, ultrasonic reaction frequency are 10-20kHz, ultrasonic reaction time 10-15min.
5. a kind of preparation method of rich titanium metatitanic acid alumina supporter according to claim 1, which is characterized in that in the step 2
It is evaporated under reduced pressure the parameter of reaction are as follows: time 3-5h, pressure are the 20-40% of standard atmospheric pressure, 50-80 DEG C of temperature.
6. a kind of preparation method of rich titanium metatitanic acid alumina supporter according to claim 1, which is characterized in that in the step 3
Ultrasonic curing response parameter: supersonic frequency 2-8MHz, temperature are 120-150 DEG C, ultrasonic time 2-4h；The constant pressure heating is anti-
Answer parameter: 200-250 DEG C of temperature, pressure 0.4-0.8Mpa, time 2-3h.
7. a kind of preparation method of rich titanium metatitanic acid alumina supporter according to claim 1, which is characterized in that in the step 4
Rapid curing temperature is 110-140 DEG C, curing time 10-20min.
8. a kind of preparation method of rich titanium metatitanic acid alumina supporter according to claim 1, which is characterized in that in the step 5
Gradient sintering parameter are as follows:
First gradient: 200-240 DEG C of sintering temperature, sintering time 40-60min；Second gradient: it 400-500 DEG C of sintering temperature, burns
Tie time 60-80min；3rd gradient: 1000-1100 DEG C of sintering temperature, sintering time 120-150min；4th gradient: sintering
1200-1400 DEG C of temperature, sintering time 240-300min.
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| CN104513062A (en) * | 2013-09-27 | 2015-04-15 | 青岛市首胜实业有限公司 | Aluminum titanate ceramic material modification production method |
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