CN106966417B - A method of preparing soilless sticking high specific area boehmite - Google Patents

A method of preparing soilless sticking high specific area boehmite Download PDF

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CN106966417B
CN106966417B CN201710212129.2A CN201710212129A CN106966417B CN 106966417 B CN106966417 B CN 106966417B CN 201710212129 A CN201710212129 A CN 201710212129A CN 106966417 B CN106966417 B CN 106966417B
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solution
sodium hydroxide
rate
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hydroxide solution
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CN106966417A (en
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廖志龙
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/14—Pore volume

Abstract

The invention discloses a kind of methods preparing soilless sticking high specific area boehmite, including：Step 1: preparing sodium hydroxide solution, metabisulfite solution and soluble aluminum salting liquid respectively；Step 2: sodium hydroxide solution and metabisulfite solution are added drop-wise in soluble aluminum salting liquid according to different rate of addition to certain pH value, white suspension is obtained；Step 3: nonionic surface active agent is added drop-wise in the white suspension, mixture is obtained after stirring 15~20min；Crystallization is carried out Step 4: the mixture is transferred in autoclave, the substance obtained after crystallization is filtered and is dried successively, soilless sticking high specific area boehmite is obtained.The boehmite that the preparation method of boehmite disclosed by the invention is prepared is Nano grade, and soilless sticking, specific surface area is 510~550m2/ g, pore volume are 1.1~1.5cm3/ g, uniform particle sizes, suitable for industrialized production.

Description

A method of preparing soilless sticking high specific area boehmite
Technical field
The present invention relates to technical field of nanometer material preparation, it is more particularly related to which a kind of Nano grade is without group The preparation method of poly- high specific area boehmite.
Background technology
γ-Al2O3It is widely used in catalyst carrier, adsorbent etc., γ-Al2O3It is boehmite in certain temperature What lower roasting obtained, and the morphological feature of boehmite can be retained, therefore the specific surface area of boehmite and pore volume etc. Morphological feature affects γ-Al2O3Application range.
There are many ways to preparing boehmite, hydrothermal synthesis method is as a kind of environmentally protective and easy to operate preparation side Method has been widely used, but in the existing report for preparing boehmite using hydro-thermal method, can't be ensured in soilless sticking On the basis of obtain specific surface area height and the big boehmite of pore volume.
Invention content
It is an object of the invention to solve at least the above, and provide the advantages of at least will be described later.
It is a still further object of the present invention to provide a kind of methods preparing soilless sticking high specific area boehmite, pass through The uniform boehmite of soilless sticking, high-specific surface area, macropore volume, particle diameter distribution has been prepared in hydro-thermal method.
To achieve the goals above, the present invention provides a kind of method preparing soilless sticking high specific area boehmite, packets Include following steps：
Step 1: the sodium hydroxide powder after weighing is dissolved in deionized water, and it is configured to a concentration of 5.5~ The sodium hydroxide solution of 6.0mol/L；A certain amount of sodium sulfate powder is weighed, a concentration of 6.2 are configured to using deionized water~ The metabisulfite solution of 8.5mol/L；And a certain amount of aluminum soluble salt is weighed, it is dissolved in being configured in deionized water a concentration of The soluble aluminum salting liquid of 0.58~0.62mol/L；
Step 2: at ambient temperature, the above-mentioned soluble aluminum salting liquid of certain volume is measured, in 600~700r/min Mixing speed under, the sodium hydroxide solution and the metabisulfite solution are added drop-wise to the solubility of the certain volume simultaneously In aluminum salt solution, the rate of addition of the sodium hydroxide solution is 1.2~2.0 times of the rate of addition of the metabisulfite solution； When the pH value of solution is to 5~6 after being added dropwise, mixing speed is adjusted to 800~1000r/min, reduces the sodium hydroxide solution Rate of addition, and adjust according to the rate of addition of the sodium hydroxide solution rate of addition of the metabisulfite solution so that The rate of addition of the sodium hydroxide solution is 1.5~2.5 times of the rate of addition of the metabisulfite solution；The solution after being added dropwise PH value to 6.5~7.0 when, stop that the metabisulfite solution is added dropwise, and keep the rate of addition of the sodium hydroxide solution；It waits for When the pH value of solution is 7.9~8.3 after dropwise addition, stop that the sodium hydroxide solution is added dropwise, adjusts mixing speed to 1100r/ Min obtains white suspension after stirring 10min；
Step 3: under the mixing speed of room temperature condition and 400r/min, by certain mass and it is certain density it is non-from Subtype surfactant is added drop-wise in the white suspension, and mixture is obtained after stirring 15~20min；
Crystallization is carried out Step 4: the mixture is transferred in autoclave, successively to the substance that is obtained after crystallization It is filtered and dries, obtain soilless sticking high specific area boehmite.
Preferably, wherein in the step 4, to the mixture carry out crystallization the specific steps are：
First, the autoclave for being loaded with mixture is placed in 30 DEG C of baking oven, adjust heating rate be 0.2~ 0.6 DEG C/min, when the temperature of the baking oven reaches 40 DEG C, the temperature is maintained, the autoclave for being loaded with mixture is made to exist 10min is kept the temperature at this temperature；
Then, under the heating rate of 0.2~0.6 DEG C/min, the temperature of baking oven is increased to 50 DEG C, and make to be loaded with mixed The autoclave for closing object keeps the temperature 20min at such a temperature；
Finally, under the heating rate of 10 DEG C/min, the temperature of baking oven is increased to 90 DEG C, and make to be loaded with mixture Autoclave keeps the temperature 8~9h at such a temperature.
Preferably, wherein in the step 3, the quality of the nonionic surface active agent and the white suspension The mass ratio of liquid is 1:50~150.
Preferably, wherein in the step 4, the deionized water that temperature in use is 45 DEG C carries out the substance after crystallization Not sulphate-containing ion is filtered for multiple times into filtrate, and the pH value of filtrate is 7.0 ± 0.5.
Preferably, wherein a concentration of 0.1mol/kg of the nonionic surface active agent.
Preferably, wherein the aluminum soluble salt is aluminum nitrate, aluminium chloride and aluminum sulfate.
Preferably, wherein in the step 4, drying temperature is 60 DEG C.
Preferably, wherein the step 2 is specially：
At ambient temperature, the above-mentioned soluble aluminum salting liquid for measuring certain volume, in the stirring speed of 600~700r/min Under degree, the sodium hydroxide solution and the metabisulfite solution are added drop-wise to the soluble aluminum salting liquid of the certain volume simultaneously In, the rate of addition of the sodium hydroxide solution is 2.0~2.5mL/min, and the rate of addition of the sodium hydroxide solution is institute State the rate of addition of metabisulfite solution 1.5 times；
When the pH value of solution is to 5.5 after being added dropwise, mixing speed is adjusted to 800~1000r/min, adjusts the hydroxide The rate of addition of sodium solution is 1.5~1.9mL/min, and adjusts the sulfuric acid according to the rate of addition of the sodium hydroxide solution The rate of addition of sodium solution so that the rate of addition of the sodium hydroxide solution is the rate of addition of the metabisulfite solution 2.0 again；
When the pH value of solution is to 6.8 after being added dropwise, stop that the metabisulfite solution is added dropwise, and keep the sodium hydroxide molten The rate of addition of liquid is 1.5~1.9mL/min；When the pH value of solution is 8.2 after being added dropwise, it is molten to stop the dropwise addition sodium hydroxide Liquid adjusts mixing speed to 1100r/min, white suspension is obtained after stirring 10min.
Preferably, wherein the nonionic surface active agent is fatty alcohol polyoxyethylene ether.
The present invention includes at least following advantageous effect：
1, the method for the present invention for preparing soilless sticking high specific area boehmite is prepared using hydrothermal method Specific surface area is 510~550m2/ g, pore volume are 1.1~1.5cm3/ g, uniform particle diameter, and 95% or more particle diameter distribution exists 2.5~3.5nm.
2, by the selection of raw material, raw material in the method for the present invention for preparing soilless sticking high specific area boehmite The adjustment of the dropwise addition mode and change of rate of addition, the introducing of the surfactant and adjustment of crystal pattern, mode of washing Selection so that the boehmite soilless sticking phenomenon prepared.
3, the method short preparation period of the present invention for preparing soilless sticking high specific area boehmite, substantially increase it is thin The industrialized speed of production of diaspore, thus greatly reduces the production cost of boehmite.
Part is illustrated to embody by further advantage, target and the feature of the present invention by following, and part will also be by this The research and practice of invention and be understood by the person skilled in the art.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail, to enable those skilled in the art with reference to specification Word can be implemented according to this.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein are not precluded one or more The presence or addition of a other elements or combinations thereof.
<Embodiment 1>
A kind of preparation method of the boehmite of soilless sticking high-specific surface area is present embodiments provided, following step is specifically included Suddenly：
Step 1: compound concentration is the metabisulfite solution of the sodium hydroxide solution of 6mol/L, a concentration of 8.5mol/L respectively And the liquor alumini chloridi of a concentration of 0.62mol/L；
Step 2: at ambient temperature, the above-mentioned liquor alumini chloridi of certain volume is measured, in stirring for 600~700r/min It mixes under speed, the metabisulfite solution of the sodium hydroxide solution of 6mol/L and 8.5mol/L is added drop-wise to certain volume simultaneously In the liquor alumini chloridi of 0.62mol/L, the rate of addition of sodium hydroxide solution is 2.5mL/min, and the drop of sodium hydroxide solution Acceleration is 2.0 times of the rate of addition of metabisulfite solution；When the pH value of solution is to 5 after being added dropwise, mixing speed is adjusted to 800 ~1000r/min, the rate of addition for adjusting sodium hydroxide solution are 1.9mL/min, and according to the dropwise addition of sodium hydroxide solution speed Degree adjusts the rate of addition of metabisulfite solution, and it is the rate of addition of metabisulfite solution to make the rate of addition of sodium hydroxide solution 2.5 again；When the pH value of solution is to 6.5 after being added dropwise, stop that the metabisulfite solution is added dropwise, and keep the drop of sodium hydroxide solution Acceleration；When the pH value of solution is 8.3 after being added dropwise, stop that sodium hydroxide solution is added dropwise, adjusts mixing speed to 1100r/ Min obtains white suspension after stirring 10min；
Step 3: under the mixing speed of room temperature condition and 400r/min, ethoxylated dodecyl alcohol is added drop-wise to It states in white suspension, mixture is obtained after stirring 15~20min, the quality of ethoxylated dodecyl alcohol and white suspension Mass ratio is 1:50, a concentration of 0.1mol/kg of ethoxylated dodecyl alcohol；
Crystallization is carried out Step 4: mixture is transferred in autoclave, the deionized water pair that temperature in use is 45 DEG C Not sulphate-containing ion is filtered for multiple times into filtrate in substance after crystallization, and the pH value of filtrate is 7.0 ± 0.5, to filtering Substance afterwards is dried at 60 DEG C, obtains soilless sticking high specific area boehmite；
To mixture carry out crystallization the specific steps are：
First, the autoclave for being loaded with mixture is placed in 30 DEG C of baking oven, adjust heating rate be 0.2 DEG C/ Min maintains the temperature when temperature of the baking oven reaches 40 DEG C, makes the autoclave for being loaded with mixture in the temperature Lower heat preservation 10min；
Then, under the heating rate of 0.5 DEG C/min, the temperature of baking oven is increased to 50 DEG C, and make to be loaded with mixture Autoclave keep the temperature 20min at such a temperature；
Finally, under the heating rate of 10 DEG C/min, the temperature of baking oven is increased to 90 DEG C, and make to be loaded with mixture Autoclave keeps the temperature 8~9h at such a temperature.
The boehmite prepared to the embodiment has carried out morphologic detection, it was demonstrated that the purity of the boehmite is high, without miscellaneous Matter, uniform particle diameter, 95% or more particle size range are distributed in 2.5~3.5nm, specific surface area 516m2/ g, pore volume are 1.28cm3/g。
<Embodiment 2>
A kind of preparation method of the boehmite of soilless sticking high-specific surface area is present embodiments provided, following step is specifically included Suddenly：
Step 1: compound concentration is that sodium hydroxide solution, the sodium sulphate of a concentration of 7.5mol/L of 5.5mol/L are molten respectively The aluminum nitrate solution of liquid and a concentration of 0.6mol/L；
Step 2: at ambient temperature, the above-mentioned liquor alumini chloridi of certain volume is measured, in stirring for 600~700r/min It mixes under speed, the metabisulfite solution of the sodium hydroxide solution of 5.5mol/L and 7.5mol/L is added drop-wise to certain volume simultaneously In the liquor alumini chloridi of 0.6mol/L, the rate of addition of sodium hydroxide solution is 2.2mL/min, and the dropwise addition of sodium hydroxide solution Speed is 1.2 times of the rate of addition of metabisulfite solution；When the pH value of solution is to 6 after being added dropwise, adjusting mixing speed to 800~ 1000r/min, the rate of addition for adjusting sodium hydroxide solution is 1.8mL/min, and according to the rate of addition of sodium hydroxide solution The rate of addition for adjusting metabisulfite solution, it is the 1.5 of the rate of addition of metabisulfite solution to make the rate of addition of sodium hydroxide solution Times；When the pH value of solution is to 7 after being added dropwise, stop that the metabisulfite solution is added dropwise, and keeps the dropwise addition speed of sodium hydroxide solution Degree is 1.8mL/min；After being added dropwise the pH value of solution be 8 when, stop be added dropwise sodium hydroxide solution, adjust mixing speed to 1100r/min obtains white suspension after stirring 10min；
Step 3: under the mixing speed of room temperature condition and 400r/min, ethoxylated dodecyl alcohol is added drop-wise to It states in white suspension, mixture is obtained after stirring 15~20min, the quality of ethoxylated dodecyl alcohol and white suspension Mass ratio is 1:150, a concentration of 0.1mol/kg of ethoxylated dodecyl alcohol；
Crystallization is carried out Step 4: mixture is transferred in autoclave, the deionized water pair that temperature in use is 45 DEG C Not sulphate-containing ion is filtered for multiple times into filtrate in substance after crystallization, and the pH value of filtrate is 7.0 ± 0.5, to filtering Substance afterwards is dried at 60 DEG C, obtains soilless sticking high specific area boehmite；
To mixture carry out crystallization the specific steps are：
First, the autoclave for being loaded with mixture is placed in 30 DEG C of baking oven, adjust heating rate be 0.4 DEG C/ Min maintains the temperature when temperature of the baking oven reaches 40 DEG C, makes the autoclave for being loaded with mixture in the temperature Lower heat preservation 10min；
Then, under the heating rate of 0.6 DEG C/min, the temperature of baking oven is increased to 50 DEG C, and make to be loaded with mixture Autoclave keep the temperature 20min at such a temperature；
Finally, under the heating rate of 10 DEG C/min, the temperature of baking oven is increased to 90 DEG C, and make to be loaded with mixture Autoclave keeps the temperature 8~9h at such a temperature.
The boehmite prepared to the embodiment has carried out morphologic detection, it was demonstrated that the purity of the boehmite is high, without miscellaneous Matter, uniform particle diameter, 95% or more particle size range are distributed in 2.5~3.5nm, specific surface area 539m2/ g, pore volume are 1.46cm3/g。
<Embodiment 3>
A kind of preparation method of the boehmite of soilless sticking high-specific surface area is present embodiments provided, following step is specifically included Suddenly：
Step 1: compound concentration is that sodium hydroxide solution, the sodium sulphate of a concentration of 6.2mol/L of 5.8mol/L are molten respectively The aluminum sulfate solution of liquid and a concentration of 0.58mol/L；
Step 2: at ambient temperature, the above-mentioned soluble aluminum salting liquid of certain volume is measured, in 600~700r/min Mixing speed under, the sodium hydroxide solution and the metabisulfite solution are added drop-wise to the solubility of the certain volume simultaneously In aluminum salt solution, the rate of addition of the sodium hydroxide solution is 2mL/min, and the rate of addition of the sodium hydroxide solution is institute State the rate of addition of metabisulfite solution 1.5 times；When the pH value of solution is to 5.5 after being added dropwise, adjusting mixing speed to 800~ 1000r/min, the rate of addition for adjusting the sodium hydroxide solution is 1.5mL/min, and according to the sodium hydroxide solution Rate of addition adjusts the rate of addition of the metabisulfite solution so that the rate of addition of the sodium hydroxide solution is the sulfuric acid 2.0 times of the rate of addition of sodium solution；When the pH value of solution is to 6.8 after being added dropwise, stop that the metabisulfite solution is added dropwise, and protect The rate of addition for holding the sodium hydroxide solution is 1.5mL/min；When the pH value of solution is 8.2 after being added dropwise, stop that institute is added dropwise Sodium hydroxide solution is stated, mixing speed is adjusted to 1100r/min, white suspension is obtained after stirring 10min；
Step 3: under the mixing speed of room temperature condition and 400r/min, ethoxylated dodecyl alcohol is added drop-wise to It states in white suspension, mixture is obtained after stirring 15~20min, the quality of ethoxylated dodecyl alcohol and white suspension Mass ratio is 1:150, a concentration of 0.1mol/kg of ethoxylated dodecyl alcohol；
Crystallization is carried out Step 4: mixture is transferred in autoclave, the deionized water pair that temperature in use is 45 DEG C Not sulphate-containing ion is filtered for multiple times into filtrate in substance after crystallization, and the pH value of filtrate is 7.0 ± 0.5, to filtering Substance afterwards is dried at 60 DEG C, obtains soilless sticking high specific area boehmite；
To mixture carry out crystallization the specific steps are：
First, the autoclave for being loaded with mixture is placed in 30 DEG C of baking oven, adjust heating rate be 0.5 DEG C/ Min maintains the temperature when temperature of the baking oven reaches 40 DEG C, makes the autoclave for being loaded with mixture in the temperature Lower heat preservation 10min；
Then, under the heating rate of 0.5 DEG C/min, the temperature of baking oven is increased to 50 DEG C, and make to be loaded with mixture Autoclave keep the temperature 20min at such a temperature；
Finally, under the heating rate of 10 DEG C/min, the temperature of baking oven is increased to 90 DEG C, and make to be loaded with mixture Autoclave keeps the temperature 8~9h at such a temperature.
The boehmite prepared to the embodiment has carried out morphologic detection, it was demonstrated that the purity of the boehmite is high, without miscellaneous Matter, uniform particle diameter, 95% or more particle size range are distributed in 2.5~3.5nm, specific surface area 550.2m2/ g, pore volume are 1.49cm3/g。
The present invention by aluminum soluble salt and sodium hydroxide reaction process increase sulfate in sulfate radical amount, and Rate of addition between each reactant and dropwise addition sequence, conducive to the boehmite of macropore volume is prepared, and pass through nonionic The cooperation of the crystallization steps that time and later stage is added of surfactant, can increase thin water aluminium on the basis of ensureing soilless sticking The specific surface area of stone, and reduce the preparation time of boehmite, production efficiency is improved, production cost is reduced, is convenient for Industrialized production, and be the γ-Al in later stage2O3Preparation lay a solid foundation.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited In specific details and embodiment shown and described herein.

Claims (8)

1. a kind of method preparing soilless sticking high specific area boehmite, which is characterized in that include the following steps：
Step 1: the sodium hydroxide powder after weighing is dissolved in deionized water, and it is configured to a concentration of 5.5~6.0mol/L's Sodium hydroxide solution；A certain amount of sodium sulfate powder is weighed, the sulphur of a concentration of 6.2~8.5mol/L is configured to using deionized water Acid sodium solution；And a certain amount of aluminum soluble salt is weighed, it is dissolved in being configured to a concentration of 0.58 in deionized water~ The soluble aluminum salting liquid of 0.62mol/L；
Step 2: at ambient temperature, the above-mentioned soluble aluminum salting liquid of certain volume is measured, in stirring for 600~700r/min It mixes under speed, the sodium hydroxide solution and the metabisulfite solution is added drop-wise to the aluminum soluble salt of the certain volume simultaneously In solution, the rate of addition of the sodium hydroxide solution is 1.2~2.0 times of the rate of addition of the metabisulfite solution；It waits dripping When adding the pH value of rear solution to 5~6, mixing speed is adjusted to 800~1000r/min, reduces the drop of the sodium hydroxide solution Acceleration, and adjust according to the rate of addition of the sodium hydroxide solution rate of addition of the metabisulfite solution so that it is described The rate of addition of sodium hydroxide solution is 1.5~2.5 times of the rate of addition of the metabisulfite solution；The pH of solution after being added dropwise When value is to 6.5~7.0, stop that the metabisulfite solution is added dropwise, and keep the rate of addition of the sodium hydroxide solution；It waits being added dropwise When the pH value of solution is 7.9~8.3 afterwards, stop that the sodium hydroxide solution is added dropwise, adjusts mixing speed to 1100r/min, stir White suspension is obtained after mixing 10min；
Step 3: under the mixing speed of room temperature condition and 400r/min, by certain mass and certain density nonionic Surfactant is added drop-wise in the white suspension, and mixture is obtained after stirring 15~20min；
Crystallization is carried out Step 4: the mixture is transferred in autoclave, the substance obtained after crystallization is carried out successively Filtering and drying, obtain soilless sticking high specific area boehmite；
Wherein, in the step 4, to the mixture carry out crystallization the specific steps are：
First, the autoclave for being loaded with mixture is placed in 30 DEG C of baking oven, adjust heating rate be 0.2~0.6 DEG C/ Min maintains the temperature when temperature of the baking oven reaches 40 DEG C, makes the autoclave for being loaded with mixture in the temperature Lower heat preservation 10min；
Then, under the heating rate of 0.2~0.6 DEG C/min, the temperature of baking oven is increased to 50 DEG C, and make to be loaded with mixture Autoclave keep the temperature 20min at such a temperature；
Finally, under the heating rate of 10 DEG C/min, the temperature of baking oven is increased to 90 DEG C, and make the high pressure for being loaded with mixture Reaction kettle keeps the temperature 8~9h at such a temperature.
2. a kind of method preparing soilless sticking high specific area boehmite according to claim 1, which is characterized in that described In step 3, the mass ratio of the quality of the nonionic surface active agent and the white suspension is 1:50~150.
3. a kind of method preparing soilless sticking high specific area boehmite according to claim 1, which is characterized in that described In step 4, temperature in use is that not containing sulfate radicals are filtered for multiple times into filtrate to the substance after crystallization in 45 DEG C of deionized water Ion, and the pH value of filtrate is 7.0 ± 0.5.
4. a kind of method preparing soilless sticking high specific area boehmite according to claim 1, which is characterized in that described A concentration of 0.1mol/kg of nonionic surface active agent.
5. a kind of method preparing soilless sticking high specific area boehmite according to claim 1, which is characterized in that described Aluminum soluble salt is aluminum nitrate, aluminium chloride and aluminum sulfate.
6. a kind of method preparing soilless sticking high specific area boehmite according to claim 1, which is characterized in that described In step 4, drying temperature is 60 DEG C.
7. a kind of method preparing soilless sticking high specific area boehmite according to claim 1, which is characterized in that described Step 2 is specially：
At ambient temperature, the above-mentioned soluble aluminum salting liquid for measuring certain volume, in the mixing speed of 600~700r/min Under, the sodium hydroxide solution and the metabisulfite solution are added drop-wise to the soluble aluminum salting liquid of the certain volume simultaneously In, the rate of addition of the sodium hydroxide solution is 2.0~2.5mL/min, and the rate of addition of the sodium hydroxide solution is institute State the rate of addition of metabisulfite solution 1.5 times；
When the pH value of solution is to 5.5 after being added dropwise, mixing speed is adjusted to 800~1000r/min, it is molten to adjust the sodium hydroxide The rate of addition of liquid is 1.5~1.9mL/min, and molten according to the rate of addition of the sodium hydroxide solution adjusting sodium sulphate The rate of addition of liquid so that the rate of addition of the sodium hydroxide solution is 2.0 times of the rate of addition of the metabisulfite solution；
When the pH value of solution is to 6.8 after being added dropwise, stop that the metabisulfite solution is added dropwise, and keep the sodium hydroxide solution Rate of addition is 1.5~1.9mL/min；When the pH value of solution is 8.2 after being added dropwise, stop that the sodium hydroxide solution is added dropwise, Mixing speed is adjusted to 1100r/min, white suspension is obtained after stirring 10min.
8. a kind of method preparing soilless sticking high specific area boehmite according to claim 1, which is characterized in that described Nonionic surface active agent is fatty alcohol polyoxyethylene ether.
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CN104692429B (en) * 2015-02-16 2017-03-01 北京化工大学 A kind of controllable method for preparing of bigger serface macropore volume boehmite
CN105036163B (en) * 2015-08-14 2017-01-04 黄志强 A kind of preparation method of nanometer fibrous boehmite
CN105883871B (en) * 2016-04-17 2017-12-29 北京化工大学 A kind of preparation method of boehmite

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