CN108840357A - A kind of preparation method of the big mesoporous boehmite of high-specific surface area - Google Patents
A kind of preparation method of the big mesoporous boehmite of high-specific surface area Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/34—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination
- C01F7/442—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination in presence of a calcination additive
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a kind of preparation methods of the big mesoporous boehmite of high-specific surface area, belong to catalyst carrier technical field.Aluminum nitrate solution and gelatin solution are first 1 by the present invention in mass ratio：1~1：After 3 mixing, the borax of aluminum nitrate solution quality 3~5% is added, then adjusts pH to gelatin isoelectric point, ultrasonic disperse obtains dispersion liquid；Urea is added into dispersion liquid again, adjusts pH, adds urase and dehydrated alcohol, after constant temperature is stirred to react 4~6h, is concentrated under reduced pressure, it is cooling, obtain wet gel；It is 8~10% by wet gel vacuum freeze drying to moisture content, obtains desiccant gel；It after desiccant gel ethyl orthosilicate dilution ultrasonic immersing, takes out, vacuum freeze drying obtains modified xerogels；By modified xerogels under inert gas shielding state, heating roasting is cooling to get the big mesoporous boehmite of high-specific surface area.The big mesoporous agent of high-specific surface area of technical solution of the present invention preparation has the characteristics that the big mesoporous of high-specific surface area.
Description
Technical field
The invention discloses a kind of preparation methods of the big mesoporous boehmite of high-specific surface area, belong to catalyst carrier skill
Art field.
Background technique
Boehmite is also referred to as gel boehmite, false quasi- quasi- boehmite, boehmite colloid or the vigorous nurse of class
Stone, be a kind of composition do not know, crystallize it is incomplete by disorder to order, the Evolution Series of weak crystalline state to crystalline state, typical structure
For very thin fold lamella.Nontoxic, tasteless, odorless, white colloidal shape（Wet product）Or powder（Dry product）, crystal phase purity is high, peptization
Performance is good, and caking property is strong, has the characteristics that specific surface is high, Kong Rong great, dispersibility and peptization is good and thixotropic gel etc. is excellent
Characteristic is mainly used as preparation γ-Al2O3、α-Al2O3Raw material and be difficult to the binder of preformed catalyst or catalyst carrier.It can
Make the binder of semi-synthetic rare earth Y type molecular sieve Cracking catalyst, the binder of aluminosilicate refractory fiber, dehydration of alcohol ethylene
Catalyst and oxidative ethane catalyst etc. is gone back, can also make the raw material of production catalyst carrier, activated alumina and other aluminium salts.
Its product γ-Al roasted between 400~700 DEG C2O3It is widely used as catalyst carrier, catalyst and adsorbent
Deng；Calcining can obtain nanometer alpha-Al between 1100~1200 DEG C2O3, it is widely used as coating additive, high-grade ceramic, petrochemical industry
Effective catalyst, submicron/nanometer grade grinding-material and polishing material, cosmetics filler and inorganic material film etc., be a kind of
New material with broad based growth future.
It is additionally the preferred silicon source of synthesizing P-Al molecular sieve and heteroatom phosphate aluminium molecular sieve.For synthesizing P-Al molecular sieve
And for heteroatom phosphate aluminium Series Molecules sieve, preferably along with the addition of oxygen source while phosphorus source and silicon source is added.And it is general
Be not connected with oxygen atom in the aluminium atom of aluminium salt, if doing silicon source with it, be difficult or enough to oxygen source, so ordinary circumstance
Aluminium salt is not had to down.In view of the evenly dispersed requirement of reaction mixture, the silicon source of addition is preferably soluble in weak acid or moderate strength
Acid solution in, and aluminum oxide or aluminium hydroxide are dissolved only in strong acid or strong base solution, are unfavorable for point of reaction mixture
It dissipates, less properly does silicon source.And boehmite can satisfy oxygen source and reaction is uniformly mixed the requirement of dispersion, be that experiment is preferred
Silicon source.
And traditional boehmite is during the preparation process, presoma and product are easy to happen reunion, and pore structure holds
It easily collapses, the defect for causing product specific surface area not high can not further increase, and bring certain be stranded to practical application
Difficulty, therefore this is also the urgent problem in terms of boehmite at present.
Summary of the invention
The present invention solves the technical problem of：During the preparation process for traditional boehmite, presoma and production
Product are easy to happen reunion, and pore structure is easy to happen and collapses, and the defect for causing product specific surface area not high can not be mentioned further
High disadvantage provides a kind of preparation method of big mesoporous boehmite of high-specific surface area.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that：
A kind of preparation method of the big mesoporous boehmite of high-specific surface area, specific preparation step are：
（1）It is in mass ratio 1 by aluminum nitrate solution and gelatin solution：1~1：After 3 mixing, aluminum nitrate solution quality 3~5% is added
Borax, then adjust pH to gelatin isoelectric point, ultrasonic disperse obtains dispersion liquid；
（2）Be added urea into dispersion liquid, adjust pH to 8.6~9.0, add dispersion liquid quality 0.3~0.5% urase and
The dehydrated alcohol of dispersion liquid quality 8~10% after constant temperature is stirred to react 4~6h, is concentrated under reduced pressure, cooling, obtains wet gel；
（3）It is 8~10% by wet gel vacuum freeze drying to moisture content, obtains desiccant gel；
（4）It after desiccant gel ethyl orthosilicate dilution ultrasonic immersing, takes out, vacuum freeze drying obtains modified xerogels；
（5）By modified xerogels under inert gas shielding state, heating roasting is cooling quasi- to get the big mesoporous of high-specific surface area
Boehmite.
Step（1）The gelatin is the gelatin that isoelectric point is 5.5~6.0.
Step（1）The aluminum nitrate solution is the aluminum nitrate solution that mass fraction is 8~20%.
Step（1）Institute's gelatine solution is the gelatin solution that mass fraction is 3~5%.
Step（4）It is 1 that the ethyl orthosilicate dilution is by ethyl orthosilicate and dehydrated alcohol by volume：8~1：
10 are formulated.
Step（5）The inert gas is any one in nitrogen or argon gas.
Step（5）The heating is roasted under the conditions of temperature is 900~980 DEG C, 3~5h of heating roasting.
The beneficial effects of the invention are as follows：
（1）Technical solution of the present invention is mixed with aluminum nitrate solution and gelatin solution, and first adjusting pH is bright at this time to gelatin isoelectric point
Xanthan molecule structure is in contraction state, and with the addition of precipitating reagent urea, urea, which occurs slowly to hydrolyze in aqueous solution, generates hydrogen
Oxygen radical ion rises the pH of system slowly, thus the Precipitation rate of Effective Regulation sediment aluminium hydroxide, and once have
Aluminum hydroxide crystal nucleus formation can be adsorbed by gelatin molecule structure, and the further growth of aluminum hydroxide crystals is effectively avoided to reunite,
Secondly, with the rising of system pH, the carboxyl in gelatin molecule structure is gradually ionized, so as to cause gelatin molecule knot
Structure because with like charges it is mutually exclusive due to expand, in expansion process, make absorption generation presoma aluminum hydroxide precipitation hole
Gap increases, and in subsequent concentration and cooling procedure, makes the presoma of the big mesoporous generated in system and other by-products quilt jointly
It is fixed in the gel rubber system of gelatin formation；During vacuum freeze drying, most of moisture volatilization, moisture evaporation, which is formed, to be expanded
Dissipate channel, and residual moisture contact with the subsequent ethyl orthosilicate diffused into make its hydrolysis generate silica, and hydrolysis production
Raw alcohols and dehydrated alcohol and residual moisture volatilizees in subsequent drying process, further functions as pore effect, enriches body
The pore structure of system, increasing specific surface area, and the filling of silica, be conducive in subsequent roasting process and borax rises jointly
To sintering aids role, and it can effectively play and consolidate pore structure, avoid the effect of collapse of pore structure；Furthermore in inert gas shielding
Lower roasting, may make organic matter gelatin to carbonize, and form porous charing skeleton, carbonize skeleton presence can play it is good
Barrier action avoids product generation during the sintering process from reuniting again, also can further improve the porosity of product and play
Consolidate pore structure, the effect for avoiding hole from collapsing；
（2）The present invention further functions as by addition urase auxiliary and plays regulating and controlling effect in presoma precipitation process, after being conducive to
The big formation of central hole structure and the homogenization of pore structure in continuous treatment process；Furthermore the application is limited to be made using aluminum nitrate
It can produce by-product ammonium nitrate during subsequent reactions for silicon source, ammonium nitrate is that violent heat release is anti-in roasting process
It answers, and reaction can produce bulk gas, the heat of releasing can be conducive to the abundant sintering of system, and the generation of gas can then be played
Pore effect, further enriches product pore structure, improves product specific surface area.
Specific embodiment
By mass fraction be 8~20% aluminum nitrate solution and mass fraction be 3~5% gelatin solution be in mass ratio 1：
1~1：3 mixing are poured into three-necked flask, and the borax of aluminum nitrate solution quality 3~5% is added, and are 40~45 DEG C in temperature, are turned
Under the conditions of speed is 300~500r/min, after constant temperature is stirred 30~60min, material pH is adjusted in three-necked flask to gelatin etc.
It is electric, it is then 45~50kHz in supersonic frequency, under the conditions of temperature is 40~45 DEG C, 20~30min of ultrasonic disperse must disperse
Liquid；Dispersion liquid is transferred in reaction kettle again, and urea is added, adjusts dispersion liquid pH to 8.6~9.0, to the end of pH is adjusted, then plus
Enter the urase of dispersion liquid quality 0.3~0.5% and the dehydrated alcohol of dispersion liquid quality 8~10%, in temperature be 38~40 DEG C, revolving speed
Under the conditions of 500~600r/min, after constant temperature is stirred to react 4~6h, material in reaction kettle is transferred in Rotary Evaporators, Yu Wen
Degree is 75~85 DEG C, under the conditions of pressure is 550~600kPa, is concentrated under reduced pressure into 1/3 of material original volume in reaction kettle, must be concentrated
Liquid, then concentrate is poured into beaker, cooled to room temperature is stood, wet gel is obtained；Again extremely by wet gel vacuum freeze drying
Moisture content is 8~10%, obtains desiccant gel；Gained desiccant gel is immersed in ethyl orthosilicate dilution again, in supersonic frequency
For 55~60kHz, under the conditions of temperature is 40~50 DEG C, 45~60min of ultrasonic immersing, then the gel after dipping is taken out, vacuum
Freeze-drying obtains modified xerogels to constant weight；Gained modified xerogels are moved into roaster again, with 800~1200mL/min
Rate is passed through inert gas into roaster, under inert gas shielding state, is warming up to 900 with 3~5 DEG C/min rate program
It~980 DEG C, after heat preservation roasts 3~5h, cools to room temperature with the furnace, discharges to get the big mesoporous boehmite of high-specific surface area.Institute
Stating glue clearly is the gelatin that isoelectric point is 5.5~6.0.The ethyl orthosilicate dilution be by ethyl orthosilicate and dehydrated alcohol by
Volume ratio is 1：8~1：10 are formulated.The inert gas is any one in nitrogen or argon gas.
Example 1
By mass fraction be 20% aluminum nitrate solution and mass fraction be 5% gelatin solution be in mass ratio 1：3 mixing are poured into
In three-necked flask, add the borax of aluminum nitrate solution quality 5%, in temperature be 45 DEG C, it is permanent under the conditions of revolving speed is 500r/min
After temperature is stirred 60min, adjust in three-necked flask material pH to gelatin isoelectric point, then in supersonic frequency be 50kHz, temperature
Under the conditions of 45 DEG C, ultrasonic disperse 30min obtains dispersion liquid；Dispersion liquid is transferred in reaction kettle again, and urea is added, adjusts and divides
Dispersion liquid pH to 9.0 adds the urase of dispersion liquid quality 0.5% and the dehydrated alcohol of dispersion liquid quality 10% to the end of pH is adjusted,
It is 40 DEG C in temperature, under the conditions of revolving speed is 600r/min, after constant temperature is stirred to react 6h, material in reaction kettle is transferred to rotary evaporation
In instrument, it is 85 DEG C in temperature, under the conditions of pressure is 600kPa, is concentrated under reduced pressure into 1/3 of material original volume in reaction kettle, must be concentrated
Liquid, then concentrate is poured into beaker, cooled to room temperature is stood, wet gel is obtained；Again extremely by wet gel vacuum freeze drying
Moisture content is 10%, obtains desiccant gel；Gained desiccant gel is immersed in ethyl orthosilicate dilution again, is in supersonic frequency
60kHz, under the conditions of temperature is 50 DEG C, ultrasonic immersing 60min, then the gel after dipping is taken out, vacuum freeze drying to constant weight,
Obtain modified xerogels；Gained modified xerogels are moved into roaster again, are passed through with 1200mL/min rate into roaster lazy
Property gas be warming up to 980 DEG C under inert gas shielding state with 5 DEG C/min rate program, it is cold with furnace after heat preservation roasting 5h
But it to room temperature, discharges to get the big mesoporous boehmite of high-specific surface area.The gelatin is the gelatin that isoelectric point is 6.0.It is described
It is 1 that ethyl orthosilicate dilution is by ethyl orthosilicate and dehydrated alcohol by volume：10 are formulated.The inert gas is
Nitrogen.
Example 2
By mass fraction be 20% liquor alumini chloridi and mass fraction be 5% gelatin solution be in mass ratio 1：3 mixing are poured into
In three-necked flask, add the borax of liquor alumini chloridi quality 5%, in temperature be 45 DEG C, it is permanent under the conditions of revolving speed is 500r/min
After temperature is stirred 60min, adjust in three-necked flask material pH to gelatin isoelectric point, then in supersonic frequency be 50kHz, temperature
Under the conditions of 45 DEG C, ultrasonic disperse 30min obtains dispersion liquid；Dispersion liquid is transferred in reaction kettle again, and urea is added, adjusts and divides
Dispersion liquid pH to 9.0 adds the urase of dispersion liquid quality 0.5% and the dehydrated alcohol of dispersion liquid quality 10% to the end of pH is adjusted,
It is 40 DEG C in temperature, under the conditions of revolving speed is 600r/min, after constant temperature is stirred to react 6h, material in reaction kettle is transferred to rotary evaporation
In instrument, it is 85 DEG C in temperature, under the conditions of pressure is 600kPa, is concentrated under reduced pressure into 1/3 of material original volume in reaction kettle, must be concentrated
Liquid, then concentrate is poured into beaker, cooled to room temperature is stood, wet gel is obtained；Again extremely by wet gel vacuum freeze drying
Moisture content is 10%, obtains desiccant gel；Gained desiccant gel is immersed in ethyl orthosilicate dilution again, is in supersonic frequency
60kHz, under the conditions of temperature is 50 DEG C, ultrasonic immersing 60min, then the gel after dipping is taken out, vacuum freeze drying to constant weight,
Obtain modified xerogels；Gained modified xerogels are moved into roaster again, are passed through with 1200mL/min rate into roaster lazy
Property gas be warming up to 980 DEG C under inert gas shielding state with 5 DEG C/min rate program, it is cold with furnace after heat preservation roasting 5h
But it to room temperature, discharges to get the big mesoporous boehmite of high-specific surface area.The gelatin is the gelatin that isoelectric point is 6.0.It is described
It is 1 that ethyl orthosilicate dilution is by ethyl orthosilicate and dehydrated alcohol by volume：10 are formulated.The inert gas is
Nitrogen.
Example 3
By mass fraction be 20% aluminum nitrate solution and mass fraction be 5% gelatin solution be in mass ratio 1：3 mixing are poured into
In three-necked flask, add the borax of aluminum nitrate solution quality 5%, in temperature be 45 DEG C, it is permanent under the conditions of revolving speed is 500r/min
After temperature is stirred 60min, adjust in three-necked flask material pH to gelatin isoelectric point, then in supersonic frequency be 50kHz, temperature
Under the conditions of 45 DEG C, ultrasonic disperse 30min obtains dispersion liquid；Dispersion liquid is transferred in reaction kettle again, and urea is added, adjusts and divides
Dispersion liquid pH to 9.0 adds the dehydrated alcohol of dispersion liquid quality 10% to the end of pH is adjusted, and is 40 DEG C in temperature, revolving speed is
Under the conditions of 600r/min, after constant temperature is stirred to react 6h, material in reaction kettle is transferred in Rotary Evaporators, in temperature be 85 DEG C,
Under the conditions of pressure is 600kPa, it is concentrated under reduced pressure into 1/3 of material original volume in reaction kettle, obtains concentrate, then concentrate is poured into
In beaker, cooled to room temperature is stood, wet gel is obtained；It is again 10% by wet gel vacuum freeze drying to moisture content, obtains drying
Gel；Gained desiccant gel is immersed in ethyl orthosilicate dilution again, is 60kHz in supersonic frequency, temperature is 50 DEG C of items
Under part, ultrasonic immersing 60min, then the gel after dipping is taken out, vacuum freeze drying to constant weight obtains modified xerogels；Again will
Gained modified xerogels move into roaster, inert gas are passed through into roaster with 1200mL/min rate, in inert gas
Under guard mode, be warming up to 980 DEG C with 5 DEG C/min rate program, after heat preservation roasting 5h, cool to room temperature with the furnace, discharging to get
The big mesoporous boehmite of high-specific surface area.The gelatin is the gelatin that isoelectric point is 6.0.The ethyl orthosilicate dilution is
It is by volume 1 by ethyl orthosilicate and dehydrated alcohol：10 are formulated.The inert gas is nitrogen.
Example 4
By mass fraction be 20% aluminum nitrate solution and mass fraction be 5% gelatin solution be in mass ratio 1：3 mixing are poured into
In three-necked flask, add the borax of aluminum nitrate solution quality 5%, in temperature be 45 DEG C, it is permanent under the conditions of revolving speed is 500r/min
After temperature is stirred 60min, adjust in three-necked flask material pH to gelatin isoelectric point, then in supersonic frequency be 50kHz, temperature
Under the conditions of 45 DEG C, ultrasonic disperse 30min obtains dispersion liquid；Dispersion liquid is transferred in reaction kettle again, and ammonium hydroxide is added, adjusts and divides
Dispersion liquid pH to 9.0 adds the urase of dispersion liquid quality 0.5% and the dehydrated alcohol of dispersion liquid quality 10% to the end of pH is adjusted,
It is 40 DEG C in temperature, under the conditions of revolving speed is 600r/min, after constant temperature is stirred to react 6h, material in reaction kettle is transferred to rotary evaporation
In instrument, it is 85 DEG C in temperature, under the conditions of pressure is 600kPa, is concentrated under reduced pressure into 1/3 of material original volume in reaction kettle, must be concentrated
Liquid, then concentrate is poured into beaker, cooled to room temperature is stood, wet gel is obtained；Again extremely by wet gel vacuum freeze drying
Moisture content is 10%, obtains desiccant gel；Gained desiccant gel is immersed in ethyl orthosilicate dilution again, is in supersonic frequency
60kHz, under the conditions of temperature is 50 DEG C, ultrasonic immersing 60min, then the gel after dipping is taken out, vacuum freeze drying to constant weight,
Obtain modified xerogels；Gained modified xerogels are moved into roaster again, are passed through with 1200mL/min rate into roaster lazy
Property gas be warming up to 980 DEG C under inert gas shielding state with 5 DEG C/min rate program, it is cold with furnace after heat preservation roasting 5h
But it to room temperature, discharges to get the big mesoporous boehmite of high-specific surface area.The gelatin is the gelatin that isoelectric point is 6.0.It is described
It is 1 that ethyl orthosilicate dilution is by ethyl orthosilicate and dehydrated alcohol by volume：10 are formulated.The inert gas is
Nitrogen.
Example 5
By mass fraction be 20% aluminum nitrate solution and mass fraction be 5% poly-vinyl alcohol solution be in mass ratio 1：3 mixing
It pours into three-necked flask, adds the borax of aluminum nitrate solution quality 5%, be 45 DEG C in temperature, revolving speed is 500r/min condition
Under, material pH is changed to gelatin isoelectric point after constant temperature is stirred 60min, in adjusting three-necked flask adjusts pH to 6.0, then
It is 50kHz in supersonic frequency, under the conditions of temperature is 45 DEG C, ultrasonic disperse 30min obtains dispersion liquid；Dispersion liquid is transferred to reaction again
In kettle, and urea is added, adjusts dispersion liquid pH to 9.0, to the end of pH is adjusted, adds the urase of dispersion liquid quality 0.5% and divide
The dehydrated alcohol of dispersion liquid quality 10%, in temperature be 40 DEG C, revolving speed be 600r/min under the conditions of, will be anti-after constant temperature is stirred to react 6h
It answers material in kettle to be transferred in Rotary Evaporators, is 85 DEG C in temperature, under the conditions of pressure is 600kPa, is concentrated under reduced pressure into reaction kettle
The 1/3 of material original volume obtains concentrate, then concentrate is poured into beaker, stands cooled to room temperature, obtains wet gel；Again
It is 10% by wet gel vacuum freeze drying to moisture content, obtains desiccant gel；Gained desiccant gel is immersed in ethyl orthosilicate again
In dilution, in supersonic frequency be 60kHz, under the conditions of temperature is 50 DEG C, ultrasonic immersing 60min, then the gel after dipping is taken
Out, vacuum freeze drying obtains modified xerogels to constant weight；Gained modified xerogels are moved into roaster again, with 1200mL/
Min rate is passed through inert gas into roaster, under inert gas shielding state, is warming up to 980 with 5 DEG C/min rate program
DEG C, after heat preservation roasting 5h, cools to room temperature with the furnace, discharge to get the big mesoporous boehmite of high-specific surface area.The positive silicic acid
It is 1 that ethyl ester dilution is by ethyl orthosilicate and dehydrated alcohol by volume：10 are formulated.The inert gas is nitrogen.
Example 6
By mass fraction be 20% aluminum nitrate solution and mass fraction be 5% gelatin solution be in mass ratio 1：3 mixing are poured into
In three-necked flask, add the borax of aluminum nitrate solution quality 5%, in temperature be 45 DEG C, it is permanent under the conditions of revolving speed is 500r/min
After temperature is stirred 60min, adjust in three-necked flask material pH to gelatin isoelectric point, then in supersonic frequency be 50kHz, temperature
Under the conditions of 45 DEG C, ultrasonic disperse 30min obtains dispersion liquid；Dispersion liquid is transferred in reaction kettle again, and urea is added, adjusts and divides
Dispersion liquid pH to 9.0 adds the urase of dispersion liquid quality 0.5% and the dehydrated alcohol of dispersion liquid quality 10% to the end of pH is adjusted,
It is 40 DEG C in temperature, under the conditions of revolving speed is 600r/min, after constant temperature is stirred to react 6h, material in reaction kettle is transferred to rotary evaporation
In instrument, it is 85 DEG C in temperature, under the conditions of pressure is 600kPa, is concentrated under reduced pressure into 1/3 of material original volume in reaction kettle, must be concentrated
Liquid, then concentrate is poured into beaker, cooled to room temperature is stood, wet gel is obtained；Again extremely by wet gel vacuum freeze drying
Moisture content is 10%, obtains desiccant gel；Gained xerogel is moved into roaster again, with 1200mL/min rate into roaster
It is passed through inert gas, under inert gas shielding state, is warming up to 980 DEG C, after heat preservation roasts 5h with 5 DEG C/min rate program,
It cools to room temperature with the furnace, discharges to get the big mesoporous boehmite of high-specific surface area.The gelatin be isoelectric point be 6.0 it is bright
Glue.The inert gas is nitrogen.
Example 7
By mass fraction be 20% aluminum nitrate solution and mass fraction be 5% gelatin solution be in mass ratio 1：3 mixing are poured into
In three-necked flask, add the borax of aluminum nitrate solution quality 5%, in temperature be 45 DEG C, it is permanent under the conditions of revolving speed is 500r/min
After temperature is stirred 60min, adjust in three-necked flask material pH to gelatin isoelectric point, then in supersonic frequency be 50kHz, temperature
Under the conditions of 45 DEG C, ultrasonic disperse 30min obtains dispersion liquid；Dispersion liquid is transferred in reaction kettle again, and urea is added, adjusts and divides
Dispersion liquid pH to 9.0 adds the urase of dispersion liquid quality 0.5% and the dehydrated alcohol of dispersion liquid quality 10% to the end of pH is adjusted,
It is 40 DEG C in temperature, under the conditions of revolving speed is 600r/min, after constant temperature is stirred to react 6h, material in reaction kettle is transferred to rotary evaporation
In instrument, it is 85 DEG C in temperature, under the conditions of pressure is 600kPa, is concentrated under reduced pressure into 1/3 of material original volume in reaction kettle, must be concentrated
Liquid, then concentrate is poured into beaker, cooled to room temperature is stood, wet gel is obtained；Again extremely by wet gel vacuum freeze drying
Moisture content is 10%, obtains desiccant gel；Gained desiccant gel is immersed in ethyl orthosilicate dilution again, is in supersonic frequency
60kHz, under the conditions of temperature is 50 DEG C, ultrasonic immersing 60min, then the gel after dipping is taken out, vacuum freeze drying to constant weight,
Obtain modified xerogels；Gained modified xerogels are moved into roaster again, are warming up to 980 DEG C with 5 DEG C/min rate program, heat preservation
After roasting 5h, room temperature is cooled to the furnace, discharge to get the big mesoporous boehmite of high-specific surface area.The gelatin is isoelectric point
For 6.0 gelatin.It is 1 that the ethyl orthosilicate dilution is by ethyl orthosilicate and dehydrated alcohol by volume：10 prepare and
At.
Comparative example：The boehmite of Nanjing development in science and technology Co., Ltd production.
Example 1 to the big mesoporous boehmite of the resulting high-specific surface area of example 7 and comparative example product are subjected to performance inspection
It surveys, the specific detection method is as follows：
Aluminium isopropoxide binary alcohol heating method 2h detects the Kong Rong and specific surface area of test specimen at 300 DEG C.
Specific testing result is as shown in table 1：
The specific testing result of the big mesoporous of 1 high-specific surface area of table
By 1 testing result of table it is found that the big mesoporous agent of high-specific surface area of technical solution of the present invention preparation has high-specific surface area big
The characteristics of mesoporous, has broad prospects in the development of catalyst carrier technology industry.
Claims (7)
1. a kind of preparation method of the big mesoporous boehmite of high-specific surface area, it is characterised in that specifically preparation step is：
（1）It is in mass ratio 1 by aluminum nitrate solution and gelatin solution：1~1：After 3 mixing, aluminum nitrate solution quality 3~5% is added
Borax, then adjust pH to gelatin isoelectric point, ultrasonic disperse obtains dispersion liquid；
（2）Be added urea into dispersion liquid, adjust pH to 8.6~9.0, add dispersion liquid quality 0.3~0.5% urase and
The dehydrated alcohol of dispersion liquid quality 8~10% after constant temperature is stirred to react 4~6h, is concentrated under reduced pressure, cooling, obtains wet gel；
（3）It is 8~10% by wet gel vacuum freeze drying to moisture content, obtains desiccant gel；
（4）It after desiccant gel ethyl orthosilicate dilution ultrasonic immersing, takes out, vacuum freeze drying obtains modified xerogels；
（5）By modified xerogels under inert gas shielding state, heating roasting is cooling quasi- to get the big mesoporous of high-specific surface area
Boehmite.
2. a kind of preparation method of the big mesoporous boehmite of high-specific surface area according to claim 1, which is characterized in that
Step（1）The gelatin is the gelatin that isoelectric point is 5.5~6.0.
3. a kind of preparation method of the big mesoporous boehmite of high-specific surface area according to claim 1, which is characterized in that
Step（1）The aluminum nitrate solution is the aluminum nitrate solution that mass fraction is 8~20%.
4. a kind of preparation method of the big mesoporous boehmite of high-specific surface area according to claim 1, which is characterized in that
Step（1）Institute's gelatine solution is the gelatin solution that mass fraction is 3~5%.
5. a kind of preparation method of the big mesoporous boehmite of high-specific surface area according to claim 1, which is characterized in that
Step（4）It is 1 that the ethyl orthosilicate dilution is by ethyl orthosilicate and dehydrated alcohol by volume：8~1：10 prepare and
At.
6. a kind of preparation method of the big mesoporous boehmite of high-specific surface area according to claim 1, which is characterized in that
Step（5）The inert gas is any one in nitrogen or argon gas.
7. a kind of preparation method of the big mesoporous boehmite of high-specific surface area according to claim 1, which is characterized in that
Step（5）The heating is roasted under the conditions of temperature is 900~980 DEG C, 3~5h of heating roasting.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111530273A (en) * | 2020-05-07 | 2020-08-14 | 周尚生 | Hydrolysis catalytic adsorption ball for high-temperature waste gas treatment |
| CN115180642A (en) * | 2022-08-26 | 2022-10-14 | 杭州智华杰科技有限公司 | Method for increasing pore volume and pore diameter of pseudo-boehmite |
-
2018
- 2018-06-29 CN CN201810692836.0A patent/CN108840357A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111530273A (en) * | 2020-05-07 | 2020-08-14 | 周尚生 | Hydrolysis catalytic adsorption ball for high-temperature waste gas treatment |
| CN111530273B (en) * | 2020-05-07 | 2022-05-31 | 广东绿羽环保科技有限公司 | Hydrolysis catalytic adsorption ball for high-temperature waste gas treatment |
| CN115180642A (en) * | 2022-08-26 | 2022-10-14 | 杭州智华杰科技有限公司 | Method for increasing pore volume and pore diameter of pseudo-boehmite |
| CN115180642B (en) * | 2022-08-26 | 2024-01-26 | 杭州智华杰科技有限公司 | Method for improving pore volume and pore diameter of pseudo-boehmite |
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