CN108128801B - Preparation method of porous aluminum titanate carrier - Google Patents
Preparation method of porous aluminum titanate carrier Download PDFInfo
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- CN108128801B CN108128801B CN201711470194.1A CN201711470194A CN108128801B CN 108128801 B CN108128801 B CN 108128801B CN 201711470194 A CN201711470194 A CN 201711470194A CN 108128801 B CN108128801 B CN 108128801B
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- 229910000505 Al2TiO5 Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 title claims abstract description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 95
- 239000002002 slurry Substances 0.000 claims abstract description 48
- 239000000725 suspension Substances 0.000 claims abstract description 39
- 238000009835 boiling Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 17
- 239000006185 dispersion Substances 0.000 claims abstract description 15
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- 235000019441 ethanol Nutrition 0.000 claims description 66
- 239000000243 solution Substances 0.000 claims description 58
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 39
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 32
- 238000004821 distillation Methods 0.000 claims description 30
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- 239000002270 dispersing agent Substances 0.000 claims description 18
- 238000000498 ball milling Methods 0.000 claims description 16
- 229920005749 polyurethane resin Polymers 0.000 claims description 16
- 230000035484 reaction time Effects 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 15
- 229920005989 resin Polymers 0.000 claims description 15
- 239000011347 resin Substances 0.000 claims description 15
- 229910052710 silicon Inorganic materials 0.000 claims description 15
- 239000010703 silicon Substances 0.000 claims description 15
- 239000004408 titanium dioxide Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 8
- QOHMWDJIBGVPIF-UHFFFAOYSA-N n',n'-diethylpropane-1,3-diamine Chemical group CCN(CC)CCCN QOHMWDJIBGVPIF-UHFFFAOYSA-N 0.000 claims description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000005292 vacuum distillation Methods 0.000 claims 2
- 229920002050 silicone resin Polymers 0.000 claims 1
- 238000005245 sintering Methods 0.000 abstract description 6
- 238000009768 microwave sintering Methods 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 239000000969 carrier Substances 0.000 description 2
- PPQREHKVAOVYBT-UHFFFAOYSA-H dialuminum;tricarbonate Chemical compound [Al+3].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O PPQREHKVAOVYBT-UHFFFAOYSA-H 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 229910003079 TiO5 Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229940118662 aluminum carbonate Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000011540 sensing material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a preparation method of a porous aluminum titanate carrier, which comprises the following steps: step 1, preparing a dispersion system suspension alcohol solution; step 2, preparing viscous slurry; step 3, preparing prefabricated slurry; step 4, placing the prefabricated slurry into a mold for heating and curing, and then carrying out gradient microwave reaction to obtain a porous model; and 5, adding the porous model into an ethanol water solution for micro-boiling reaction, removing the model, and drying to obtain the porous aluminum titanate carrier. The preparation method comprises the steps of putting the prefabricated slurry into a mold, heating and curing, and then carrying out micro-boiling reaction to obtain a porous aluminum titanate carrier; the preparation method has the advantages that the steps are simple, the process is easy to realize, gradient microwave sintering is carried out after heating and curing, the sintering temperature is reduced, and the obtained porous aluminum titanate carrier is high in strength and porosity and has good practical value.
Description
Technical Field
The invention belongs to the technical field of preparation methods of aluminum titanate catalyst carriers, and particularly relates to a preparation method of a porous aluminum titanate carrier.
Background
With the rapid development of the fields of modern metal smelting, aerospace, automobile industry and the like, the standard of the performance requirements of ceramic materials is continuously improved, particularly in the aspects of high temperature resistance, thermal shock resistance and the like. Aluminum titanate (Al)2TiO5) The material has high melting point and good impact resistance and thermal shock resistance, and the advantages make the material have great application potential under the conditions of higher temperature and frequent cold and heat exchange. In addition, the aluminum titanate material also has the advantages of low expansibility, fire resistance, corrosion resistance, alkali resistance and the like, so the aluminum titanate material is also widely applied to the refractory bricks and the chemical industry. The porous aluminum titanate ceramic has the advantages of low relative density, high specific surface area, good permeability, excellent adsorbability, high melting point of an aluminum titanate material, good impact resistance and thermal shock resistance and the like, and is widely applied to the following fields: (1) filtering, purifying and separating; (2) a catalytic carrier, an adsorption carrier; (3) high-grade heat insulating material and sensing material.
A method for producing a porous aluminum titanate block (application No. CN 201410567885.3; published: 2015.02.18; published: CN104355614A) discloses a method for producing a porous aluminum titanate block by a sol-gel concomitant phase separation method; a method for producing porous aluminum magnesium titanate and porous aluminum magnesium titanate (application No. CN 201180012955.3; published No. 2012.11.14; published No. CN102781873A) disclose porous aluminum magnesium titanate and a method for producing the same; in conclusion, the preparation processes of the two materials have the problems of complicated process, overhigh sintering temperature, low sintering strength, low porosity and the like.
Disclosure of Invention
The invention aims to provide a preparation method of a porous aluminum titanate carrier, which solves the problems of complex process, overhigh sintering temperature, low sintering strength and low porosity in the existing preparation method.
The invention adopts the technical scheme that the preparation method of the porous aluminum titanate carrier comprises the following steps:
step 1, preparing a dispersion-based suspension alcohol solution
Step 1.1, adding alumina and titanium dioxide into a ball mill, uniformly mixing, then adding absolute ethyl alcohol, and carrying out water bath ball milling reaction to obtain a mixed suspended alcohol solution;
step 1.2, adding a dispersing agent into the mixed suspension alcohol solution obtained in the step 1.1 to carry out ultrasonic reaction to obtain a dispersion system suspension alcohol solution;
step 2, preparing viscous slurry
Putting the dispersion system suspended alcohol solution obtained in the step 1.2 into a reduced pressure distillation reaction kettle, and carrying out reduced pressure distillation reaction to obtain viscous slurry;
step 3, preparing the prefabricated slurry
Sequentially adding silicon resin, polyurethane resin and a curing agent into the viscous slurry obtained in the step (2), and carrying out ultrasonic reaction to obtain prefabricated slurry;
step 4, preparing a porous model
Placing the prefabricated slurry obtained in the step (3) into a mold for heating and curing, and then carrying out gradient microwave reaction to obtain a porous model;
and 5, adding the porous model obtained in the step 4 into an ethanol water solution for micro-boiling reaction, removing the model, and drying to obtain the porous aluminum titanate carrier.
The present invention is also characterized in that,
in the step 1.1, the mass ratio of the alumina to the titanium dioxide is 1:1.2-1.6, wherein the mass concentration of the alumina in the mixed suspension alcohol solution is 13-25 g/L;
the parameters of the water bath ball milling reaction are as follows: the reaction time is 2-4h, and the reaction temperature is not more than 60 ℃.
In the step 1.2, the dispersing agent is any one of polyvinylpyrrolidone or sodium dodecyl sulfate, wherein the mass ratio of the dispersing agent to the alumina in the mixed suspension alcohol liquid is 0.05-0.1: 1.
The ultrasonic reaction parameters in step 1.2 are as follows: the time is 10-30min, the frequency is 10-20kHz, and the temperature is not more than 65 ℃.
The reduced pressure distillation reaction in the step 2 is a gradient reduced pressure distillation reaction, the total reaction time is 0.5-1.5h, and the specific parameters are as follows:
a first gradient with pressure of 40-50% of standard atmospheric pressure, temperature of 50 deg.C, and time of 10-20 min; the second gradient, the pressure is 50-60% of the standard atmospheric pressure, the temperature is 60 ℃, the time is 10-30 min; the third gradient is that the pressure is 60-70% of the standard atmospheric pressure, the temperature is 70 ℃, and the time is the residual time.
The mass ratio of the silicon resin, the polyurethane resin, the curing agent and the alumina in the step 1.1 is 0.02-0.08:0.2-0.4:0.01-0.03:1 in the step 3, wherein the curing agent is specifically diethylaminopropylamine;
the ultrasonic reaction parameters are as follows: the time is 10-20min, the frequency is 5-10kHz, and the temperature is 80-100 ℃.
The heating curing temperature in the step 4 is 100-.
In the step 4, the total time of gradient microwave reaction is 4-10h, and the specific parameters are as follows: the first gradient, power is 200-; the second gradient, the power is 300-; the third gradient, power is 350-; the fourth gradient, power 450W, temperature 1350-.
In the step 5, the mass fraction of the ethanol in the ethanol water solution is 50-60%, and the drying temperature is 100-120 ℃;
micro-boiling reaction parameters: the time is 30-50min, and the temperature is 80-90 ℃.
The invention has the beneficial effects that: the preparation method of the porous aluminum titanate carrier comprises the steps of putting prefabricated slurry into a mold, heating and curing, and then carrying out micro-boiling reaction to obtain the porous aluminum titanate carrier; the preparation method has the advantages that the steps are simple, the process is easy to realize, gradient microwave sintering is carried out after heating and curing, the sintering temperature is reduced, and the obtained porous aluminum titanate carrier is high in strength and porosity and has good practical value.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments.
The invention relates to a preparation method of a porous aluminum titanate carrier, which comprises the following steps:
step 1, preparing a dispersion-based suspension alcohol solution
Step 1.1, adding alumina and titanium dioxide into a ball mill, uniformly mixing, then adding absolute ethyl alcohol, and carrying out water bath ball milling reaction to obtain a mixed suspended alcohol solution; wherein the mass ratio of the alumina to the titanium dioxide is 1:1.2-1.6, and the mass concentration of the alumina in the mixed suspension alcohol solution is 13-25 g/L;
the parameters of the water bath ball milling reaction are as follows: the reaction time is 2-4h, and the reaction temperature is not more than 60 ℃.
Step 1.2, adding a dispersant polyvinylpyrrolidone or sodium dodecyl sulfate into the mixed suspension alcohol solution obtained in the step 1.1 to carry out ultrasonic reaction to obtain a dispersion system suspension alcohol solution; wherein the mass ratio of the dispersant to the alumina in the mixed suspension alcohol liquid is 0.05-0.1: 1;
the ultrasonic reaction parameters are as follows: the time is 10-30min, the frequency is 10-20kHz, and the temperature is not more than 65 ℃.
Step 2, preparing viscous slurry
Putting the dispersion system suspended alcohol solution obtained in the step 1.2 into a reduced pressure distillation reaction kettle, and carrying out reduced pressure distillation reaction to obtain viscous slurry;
the reduced pressure distillation reaction is a gradient reduced pressure distillation reaction, the total reaction time is 0.5-1.5h, and the specific parameters are as follows:
a first gradient with pressure of 40-50% of standard atmospheric pressure, temperature of 50 deg.C, and time of 10-20 min; the second gradient, the pressure is 50-60% of the standard atmospheric pressure, the temperature is 60 ℃, the time is 10-30 min; the third gradient is that the pressure is 60-70% of the standard atmospheric pressure, the temperature is 70 ℃, and the time is the residual time.
Step 3, preparing the prefabricated slurry
Sequentially adding silicon resin, polyurethane resin and a curing agent diethylaminopropylamine into the viscous slurry obtained in the step 2, and carrying out ultrasonic reaction to obtain prefabricated slurry; in the step 3, the mass ratio of the silicon resin, the polyurethane resin, the curing agent to the aluminum oxide in the step 1.1 is 0.02-0.08:0.2-0.4:0.01-0.03: 1;
the ultrasonic reaction parameters are as follows: the time is 10-20min, the frequency is 5-10kHz, and the temperature is 80-100 ℃.
Step 4, preparing a porous model
Placing the prefabricated slurry obtained in the step (3) into a mold, heating and curing at the temperature of 100-150 ℃ for 2-3h, and then carrying out gradient microwave reaction to obtain a porous model;
the total time of the gradient microwave reaction is 4-10h, and the specific parameters are as follows: the first gradient, power is 200-; the second gradient, the power is 300-; the third gradient, power is 350-; the fourth gradient, power 450W, temperature 1350-.
Step 5, adding the porous model obtained in the step 4 into an ethanol water solution for micro-boiling reaction, removing the model, and drying to obtain a porous aluminum titanate carrier;
wherein the mass fraction of ethanol in the ethanol aqueous solution is 50-60%, and the drying temperature is 100-120 ℃;
micro-boiling reaction parameters: the time is 30-50min, and the temperature is 80-90 ℃.
Example 1
(1) Preparation of Dispersion-suspended alcohol solution
Adding alumina and titanium dioxide into a ball mill, uniformly mixing, and then adding absolute ethyl alcohol to perform water bath ball milling reaction to obtain mixed suspended alcohol liquid; and adding a dispersant polyvinylpyrrolidone into the mixed suspension alcohol solution for ultrasonic reaction to obtain the dispersion suspension alcohol solution.
Wherein the mass ratio of the alumina to the titanium dioxide is 1:1.2, and the mass concentration of the alumina in the mixed suspended alcohol solution is 13 g/L; the parameters of the water bath ball milling reaction are as follows: the reaction time is 2h, and the reaction temperature is 60 ℃.
The mass ratio of the dispersing agent to the alumina in the mixed suspension alcohol liquid is 0.05: 1; the ultrasonic reaction parameters are as follows: the time was 10min, the frequency 10kHz, the temperature 65 ℃.
(2) Preparation of viscous paste
And (3) putting the dispersed suspension alcohol solution into a reduced pressure distillation reaction kettle, and carrying out reduced pressure distillation reaction to obtain viscous slurry.
The reduced pressure distillation reaction is a gradient reduced pressure distillation reaction, the total reaction time is 1.5h, and the specific parameters are as follows: a first gradient with pressure of 40% of standard atmospheric pressure, temperature of 50 deg.C, and time of 20 min; a second gradient with pressure of 50% of standard atmospheric pressure, temperature of 60 deg.C, and time of 30 min; the third gradient, pressure 60% of standard atmospheric pressure, temperature 70 ℃, time is the remaining time.
(3) Preparation of a Pre-slurry
And sequentially adding the silicon resin, the polyurethane resin and the curing agent diethylaminopropylamine into the viscous slurry, and carrying out ultrasonic reaction to obtain the prefabricated slurry.
Wherein the mass ratio of the silicon resin to the polyurethane resin to the curing agent to the alumina is 0.02:0.2:0.01: 1; the ultrasonic reaction parameters are as follows: the time is 10min, the frequency is 5kHz, and the temperature is 80 ℃.
(4) Preparation of porous models
And (3) putting the prefabricated slurry into a mold, heating and curing for 2 hours at the temperature of 100 ℃, and then carrying out gradient microwave reaction to obtain the porous model.
The total time of the gradient microwave reaction is 4h, and the specific parameters are as follows:
the first gradient, the power is 200W, the temperature is 300 ℃, and the time is 20 min;
the second gradient, power is 300W, temperature is 800 ℃, time is 30 min;
the third gradient, power is 350W, temperature is 1100 deg.C, time is 50 min;
the fourth gradient, power 450W, temperature 1350 deg.C, time remaining.
(5) And adding the porous model into an ethanol water solution for micro-boiling reaction, removing the model, and drying to obtain the porous aluminum titanate carrier.
Wherein the mass fraction of ethanol in the ethanol water solution is 50 percent, and the drying temperature is 100 ℃;
micro-boiling reaction parameters: the time is 30min and the temperature is 80 ℃.
Example 2
(1) Preparation of Dispersion-suspended alcohol solution
Adding alumina and titanium dioxide into a ball mill, uniformly mixing, and then adding absolute ethyl alcohol to perform water bath ball milling reaction to obtain mixed suspended alcohol liquid; and adding the dispersing agent sodium dodecyl sulfate into the mixed suspension alcohol solution for ultrasonic reaction to obtain the dispersion suspension alcohol solution.
Wherein the mass ratio of the alumina to the titanium dioxide is 1:1.3, and the mass concentration of the alumina in the mixed suspension alcohol solution is 15 g/L; the parameters of the water bath ball milling reaction are as follows: the reaction time was 2.5h and the reaction temperature was 40 ℃.
The mass ratio of the dispersing agent to the alumina in the mixed suspension alcohol liquid is 0.06: 1; the ultrasonic reaction parameters are as follows: the time was 15min, the frequency 12kHz, the temperature 45 ℃.
(2) Preparation of viscous paste
And (3) putting the dispersed suspension alcohol solution into a reduced pressure distillation reaction kettle, and carrying out reduced pressure distillation reaction to obtain viscous slurry.
The reduced pressure distillation reaction is a gradient reduced pressure distillation reaction, the total reaction time is 80min, and the specific parameters are as follows: a first gradient with pressure of 43% of standard atmospheric pressure, temperature of 50 deg.C, and time of 18 min; a second gradient with pressure of 52% of standard atmospheric pressure, temperature of 60 deg.C, and time of 25 min; the third gradient, 64% pressure at standard atmospheric pressure, 70 ℃ temperature, time remaining.
(3) Preparation of a Pre-slurry
And sequentially adding the silicon resin, the polyurethane resin and the curing agent diethylaminopropylamine into the viscous slurry, and carrying out ultrasonic reaction to obtain the prefabricated slurry.
Wherein the mass ratio of the silicon resin, the polyurethane resin, the curing agent and the alumina is 0.04:0.25:0.01: 1; the ultrasonic reaction parameters are as follows: the time is 13min, the frequency is 7kHz, and the temperature is 85 ℃.
(4) Preparation of porous models
And (3) putting the prefabricated slurry into a mold, heating and curing at the temperature of 120 ℃ for 2.2h, and then carrying out gradient microwave reaction to obtain the porous model.
The total time of the gradient microwave reaction is 6h, and the specific parameters are as follows:
the first gradient, the power is 220W, the temperature is 320 ℃, and the time is 23 min;
the second gradient, power is 330W, temperature is 860 ℃, and time is 40 min;
the third gradient, power 360W, temperature 1130 deg.C, time 55 min;
the fourth gradient, power 450W, temperature 1380 deg.C, time is the remaining time.
(5) And adding the porous model into an ethanol water solution for micro-boiling reaction, removing the model, and drying to obtain the porous aluminum titanate carrier.
Wherein the mass fraction of ethanol in the ethanol water solution is 53 percent, and the drying temperature is 105 ℃;
micro-boiling reaction parameters: the time was 35min and the temperature was 82 ℃.
Example 3
(1) Preparation of Dispersion-suspended alcohol solution
Adding alumina and titanium dioxide into a ball mill, uniformly mixing, and then adding absolute ethyl alcohol to perform water bath ball milling reaction to obtain mixed suspended alcohol liquid; and adding a dispersant polyvinylpyrrolidone into the mixed suspension alcohol solution for ultrasonic reaction to obtain the dispersion suspension alcohol solution.
Wherein the mass ratio of the alumina to the titanium dioxide is 1:1.4, and the mass concentration of the alumina in the mixed suspension alcohol solution is 20 g/L; the parameters of the water bath ball milling reaction are as follows: the reaction time is 3h, and the reaction temperature is 50 ℃.
The mass ratio of the dispersing agent to the alumina in the mixed suspension alcohol liquid is 0.07: 1; the ultrasonic reaction parameters are as follows: the time was 20min, the frequency 15kHz, the temperature 50 ℃.
(2) Preparation of viscous paste
And (3) putting the dispersed suspension alcohol solution into a reduced pressure distillation reaction kettle, and carrying out reduced pressure distillation reaction to obtain viscous slurry.
The reduced pressure distillation reaction is a gradient reduced pressure distillation reaction, the total reaction time is 1h, and the specific parameters are as follows: a first gradient with pressure of 45% of standard atmospheric pressure, temperature of 50 deg.C, and time of 15 min; a second gradient with pressure of 55% of standard atmospheric pressure, temperature of 60 deg.C, and time of 20 min; the third gradient, 65% of pressure at standard atmospheric pressure, 70 ℃ of temperature and time remaining.
(3) Preparation of a Pre-slurry
And sequentially adding the silicon resin, the polyurethane resin and the curing agent diethylaminopropylamine into the viscous slurry, and carrying out ultrasonic reaction to obtain the prefabricated slurry.
Wherein the mass ratio of the silicon resin to the polyurethane resin to the curing agent to the alumina is 0.07:0.3:0.02: 1; the ultrasonic reaction parameters are as follows: the time is 15min, the frequency is 8kHz, and the temperature is 90 ℃.
(4) Preparation of porous models
And (3) placing the prefabricated slurry into a mold, heating and curing at the temperature of 100-150 ℃ for 2-3h, and then carrying out gradient microwave reaction to obtain the porous model.
The total time of the gradient microwave reaction is 7h, and the specific parameters are as follows:
the first gradient, the power is 260W, the temperature is 330 ℃, and the time is 25 min;
the second gradient, power is 360W, temperature is 850 deg.C, time is 50 min;
the third gradient, power 375W, temperature 1130 deg.C, time 60 min;
the fourth gradient, power 450W, temperature 1400 deg.C, time is the remaining time.
(5) And adding the porous model into an ethanol water solution for micro-boiling reaction, removing the model, and drying to obtain the porous aluminum titanate carrier.
Wherein the mass fraction of ethanol in the ethanol water solution is 55 percent, and the drying temperature is 110 ℃;
micro-boiling reaction parameters: the time was 40min and the temperature was 85 ℃.
Example 4
(1) Preparation of Dispersion-suspended alcohol solution
Adding alumina and titanium dioxide into a ball mill, uniformly mixing, and then adding absolute ethyl alcohol to perform water bath ball milling reaction to obtain mixed suspended alcohol liquid; and adding a dispersant polyvinylpyrrolidone into the mixed suspension alcohol solution for ultrasonic reaction to obtain the dispersion suspension alcohol solution.
Wherein the mass ratio of the alumina to the titanium dioxide is 1:1.5, and the mass concentration of the alumina in the mixed suspension alcohol solution is 22 g/L; the parameters of the water bath ball milling reaction are as follows: the reaction time was 3.5h and the reaction temperature was 55 ℃.
The mass ratio of the dispersing agent to the alumina in the mixed suspension alcohol liquid is 0.08: 1; the ultrasonic reaction parameters are as follows: the time was 25min, the frequency 18kHz, the temperature 55 ℃.
(2) Preparation of viscous paste
And (3) putting the dispersed suspension alcohol solution into a reduced pressure distillation reaction kettle, and carrying out reduced pressure distillation reaction to obtain viscous slurry.
The reduced pressure distillation reaction is a gradient reduced pressure distillation reaction, the total reaction time is 40min, and the specific parameters are as follows: a first gradient with pressure of 48% of standard atmospheric pressure, temperature of 50 deg.C, and time of 13 min; a second gradient with pressure of 56% of standard atmospheric pressure, temperature of 60 deg.C, and time of 17 min; the third gradient, 67% of pressure at standard atmospheric pressure, 70 ℃ of temperature, time remaining.
(3) Preparation of a Pre-slurry
And sequentially adding the silicon resin, the polyurethane resin and the curing agent diethylaminopropylamine into the viscous slurry, and carrying out ultrasonic reaction to obtain the prefabricated slurry.
Wherein the mass ratio of the silicon resin to the polyurethane resin to the curing agent to the alumina is 0.07:0.35:0.03: 1; the ultrasonic reaction parameters are as follows: the time is 18min, the frequency is 9kHz, and the temperature is 95 ℃.
(4) Preparation of porous models
And (3) putting the prefabricated slurry into a mold, heating and curing at the temperature of 140 ℃ for 2.8h, and then carrying out gradient microwave reaction to obtain the porous model.
The total time of the gradient microwave reaction is 9h, and the specific parameters are as follows:
the first gradient, power is 280W, temperature is 340 ℃, and time is 28 min;
the second gradient, the power is 370W, the temperature is 880 ℃, and the time is 55 min;
the third gradient, power is 390W, temperature is 1140 deg.C, time is 65 min;
the fourth gradient, power 450W, temperature 1420 deg.C, time remaining.
(5) And adding the porous model into an ethanol water solution for micro-boiling reaction, removing the model, and drying to obtain the porous aluminum titanate carrier.
Wherein the mass fraction of ethanol in the ethanol water solution is 57%, and the drying temperature is 115 ℃;
micro-boiling reaction parameters: the time was 45min and the temperature was 87 ℃.
Example 5
(1) Preparation of Dispersion-suspended alcohol solution
Adding alumina and titanium dioxide into a ball mill, uniformly mixing, and then adding absolute ethyl alcohol to perform water bath ball milling reaction to obtain mixed suspended alcohol liquid; and adding the dispersing agent sodium dodecyl sulfate into the mixed suspension alcohol solution for ultrasonic reaction to obtain the dispersion suspension alcohol solution.
Wherein the mass ratio of the alumina to the titanium dioxide is 1:1.6, and the mass concentration of the alumina in the mixed suspended alcohol solution is 25 g/L; the parameters of the water bath ball milling reaction are as follows: the reaction time is 4h, and the reaction temperature is 30 ℃.
The mass ratio of the dispersing agent to the alumina in the mixed suspension alcohol liquid is 0.1: 1; the ultrasonic reaction parameters are as follows: the time was 30min, the frequency was 20kHz, and the temperature was 35 ℃.
(2) Preparation of viscous paste
And (3) putting the dispersed suspension alcohol solution into a reduced pressure distillation reaction kettle, and carrying out reduced pressure distillation reaction to obtain viscous slurry.
The reduced pressure distillation reaction is a gradient reduced pressure distillation reaction, the total reaction time is 0.5h, and the specific parameters are as follows: a first gradient with pressure of 50% of standard atmospheric pressure, temperature of 50 deg.C, and time of 10 min; a second gradient with a pressure of 60% of the standard atmospheric pressure, a temperature of 60 ℃ and a time of 10 min; and the third gradient, the pressure is 70% of the standard atmospheric pressure, the temperature is 70 ℃, and the time is the rest time.
(3) Preparation of a Pre-slurry
And sequentially adding the silicon resin, the polyurethane resin and the curing agent diethylaminopropylamine into the viscous slurry, and carrying out ultrasonic reaction to obtain the prefabricated slurry.
Wherein the mass ratio of the silicon resin to the polyurethane resin to the curing agent to the alumina is 0.08:0.4:0.03: 1; the ultrasonic reaction parameters are as follows: the time is 20min, the frequency is 10kHz, and the temperature is 100 ℃.
(4) Preparation of porous models
And (3) putting the prefabricated slurry into a mold, heating and curing for 3 hours at the temperature of 150 ℃, and then carrying out gradient microwave reaction to obtain the porous model.
The total time of the gradient microwave reaction is 10h, and the specific parameters are as follows:
the first gradient is carried out, the power is 300W, the temperature is 350 ℃, and the time is 30 min;
the second gradient, the power is 350W, the temperature is 900 ℃, and the time is 60 min;
the third gradient, power 400W, temperature 1150 deg.C, time 70 min;
the fourth gradient, power 450W, temperature 1450 deg.C, time remaining.
(5) And adding the porous model into an ethanol water solution for micro-boiling reaction, removing the model, and drying to obtain the porous aluminum titanate carrier.
Wherein the mass fraction of ethanol in the ethanol water solution is 60 percent, and the drying temperature is 120 ℃;
micro-boiling reaction parameters: the time is 50min and the temperature is 90 ℃.
The porous aluminum carbonate carriers obtained in examples 1 to 5 have not only improved strength compared with the prior art, but also uniform pores, high porosity, simple process and good practical value.
Claims (7)
1. The preparation method of the porous aluminum titanate carrier is characterized by comprising the following steps of:
step 1, preparing a dispersion-based suspension alcohol solution
Step 1.1, adding alumina and titanium dioxide into a ball mill, uniformly mixing, then adding absolute ethyl alcohol, and carrying out water bath ball milling reaction to obtain a mixed suspended alcohol solution;
step 1.2, adding a dispersing agent into the mixed suspension alcohol solution obtained in the step 1.1 to carry out ultrasonic reaction to obtain a dispersion system suspension alcohol solution;
step 2, preparing viscous slurry
Putting the dispersion system suspended alcohol solution obtained in the step 1.2 into a reduced pressure distillation reaction kettle, and carrying out reduced pressure distillation reaction to obtain viscous slurry;
step 3, preparing the prefabricated slurry
Sequentially adding silicon resin, polyurethane resin and a curing agent into the viscous slurry obtained in the step (2), and carrying out ultrasonic reaction to obtain prefabricated slurry;
step 4, preparing a porous model
Placing the prefabricated slurry obtained in the step (3) into a mold for heating and curing, and then carrying out gradient microwave reaction to obtain a porous model;
the total time of the gradient microwave reaction is 4-10h, and the specific parameters are as follows: the first gradient, power is 200-; the second gradient, the power is 300-; the third gradient, power is 350-; the fourth gradient, the power is 450W, the temperature is 1350-;
step 5, adding the porous model obtained in the step 4 into an ethanol water solution for micro-boiling reaction, removing the model, and drying to obtain a porous aluminum titanate carrier;
the mass fraction of ethanol in the ethanol aqueous solution is 50-60%, and the drying temperature is 100-120 ℃;
the micro-boiling reaction parameters are as follows: the time is 30-50min, and the temperature is 80-90 ℃.
2. The method for preparing a porous aluminum titanate support according to claim 1, wherein the mass ratio of alumina to titania in step 1.1 is 1:1.2-1.6, and the mass concentration of alumina in the mixed suspension alcohol solution is 13-25 g/L;
the parameters of the water bath ball milling reaction are as follows: the reaction time is 2-4h, and the reaction temperature is not more than 60 ℃.
3. The method for preparing a porous aluminum titanate carrier according to claim 1, wherein the dispersant in step 1.2 is any one of polyvinylpyrrolidone and sodium dodecyl sulfate, and the mass ratio of the dispersant to the alumina in the mixed suspension alcohol solution is 0.05-0.1: 1.
4. The method for preparing a porous aluminum titanate support according to claim 1 or 3, wherein the ultrasonic reaction parameters in step 1.2 are as follows: the time is 10-30min, the frequency is 10-20kHz, and the temperature is not more than 65 ℃.
5. The method for preparing a porous aluminum titanate carrier according to claim 1, wherein the vacuum distillation reaction in the step 2 is a gradient vacuum distillation reaction, the total reaction time is 0.5-1.5h, and the specific parameters are as follows:
a first gradient with pressure of 40-50% of standard atmospheric pressure, temperature of 50 deg.C, and time of 10-20 min;
the second gradient, the pressure is 50-60% of the standard atmospheric pressure, the temperature is 60 ℃, the time is 10-30 min; the third gradient is that the pressure is 60-70% of the standard atmospheric pressure, the temperature is 70 ℃, and the time is the residual time.
6. The method for preparing the porous aluminum titanate carrier according to claim 1, wherein the mass ratio of the silicone resin, the polyurethane resin, the curing agent and the alumina in the step 3.1 is 0.02-0.08:0.2-0.4:0.01-0.03:1, wherein the curing agent is diethylaminopropylamine;
the ultrasonic reaction parameters are as follows: the time is 10-20min, the frequency is 5-10kHz, and the temperature is 80-100 ℃.
7. The method as claimed in claim 1, wherein the heating curing temperature in step 4 is 100 ℃ and 150 ℃ for 2-3 h.
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