CN106966417A - A kind of method for preparing soilless sticking specific area boehmite - Google Patents

A kind of method for preparing soilless sticking specific area boehmite Download PDF

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CN106966417A
CN106966417A CN201710212129.2A CN201710212129A CN106966417A CN 106966417 A CN106966417 A CN 106966417A CN 201710212129 A CN201710212129 A CN 201710212129A CN 106966417 A CN106966417 A CN 106966417A
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solution
sodium hydroxide
rate
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hydroxide solution
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CN106966417B (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 method for preparing soilless sticking 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 to certain pH value according to different rate of addition, white suspension is obtained；Step 3: nonionic surface active agent is added drop-wise in the white suspension, mixture is obtained after 15~20min of stirring；Crystallization is carried out Step 4: the mixture is transferred in autoclave, the material obtained after crystallization is filtered and dried successively, soilless sticking specific area boehmite is obtained.The boehmite prepared by the preparation method of boehmite disclosed by the invention is Nano grade, and soilless sticking, its specific surface area is 510~550m2/ g, pore volume is 1.1~1.5cm3/ g, uniform particle sizes, suitable industrialized production.

Description

A kind of method for preparing soilless sticking 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- specific area boehmite.
Background technology
γ-Al2O3It is widely used in catalyst carrier, adsorbent etc., γ-Al2O3It is boehmite in certain temperature It is lower to be calcined what is obtained, and the morphological feature of boehmite, therefore specific surface area and pore volume of boehmite etc. can be retained Morphological feature have impact on γ-Al2O3Application.
Preparing the method for boehmite has a variety of, and hydrothermal synthesis method is used as a kind of environmental protection and preparation side simple to operate Method, has been widely used, but existing use hydro-thermal method is prepared in the report of boehmite, can't be ensured in soilless sticking On the basis of obtain that specific surface area is high and the big boehmite of pore volume.
The content of the invention
It is an object of the invention to solve at least the above, and provide the advantage that at least will be described later.
It is a still further object of the present invention to provide a kind of method for preparing soilless sticking specific area boehmite, it passes through Hydro-thermal method has prepared the uniform boehmite of soilless sticking, high-specific surface area, macropore volume, particle diameter distribution.
To achieve these goals, the invention provides a kind of method for preparing soilless sticking specific area boehmite, bag Include following steps：
Step 1: the sodium hydroxide powder after weighing is dissolved in deionized water, and be configured to concentration for 5.5~ 6.0mol/L sodium hydroxide solution；Weigh a certain amount of sodium sulfate powder, using deionized water be configured to concentration for 6.2~ 8.5mol/L metabisulfite solution；And weigh a certain amount of aluminum soluble salt, be dissolved in being configured to concentration in deionized water be 0.58~0.62mol/L soluble aluminum salting liquid；
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, regulation mixing speed 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；Treat When the pH value of solution is 7.9~8.3 after dropwise addition, stop that the sodium hydroxide solution, regulation mixing speed to 1100r/ is added dropwise White suspension is obtained after min, stirring 10min；
Step 3: under room temperature condition and 400r/min mixing speed, 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 15~20min of stirring；
Crystallization is carried out Step 4: the mixture is transferred in autoclave, to the material that is obtained after crystallization successively Filtered and dried, obtain soilless sticking specific area boehmite.
Preferably, wherein, in the step 4, to the mixture carry out crystallization concretely comprise the following steps：
First, the autoclave for being loaded with mixture is placed in 30 DEG C of baking oven, regulation 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 existed 10min is incubated at this temperature；
Then, under 0.2~0.6 DEG C/min heating rate, the temperature of baking oven is increased to 50 DEG C, and makes to be loaded with mixed The autoclave of compound is incubated 20min at such a temperature；
Finally, under 10 DEG C/min heating rate, the temperature of baking oven is increased to 90 DEG C, and makes to be loaded with mixture Autoclave is incubated 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, temperature in use for 45 DEG C deionized water to after crystallization material carry out Multiple times of filtration not sulphate-containing ion, and the pH value of filtrate is 7.0 ± 0.5 into filtrate.
Preferably, wherein, the concentration of the nonionic surface active agent is 0.1mol/kg.
Preferably, wherein, the aluminum soluble salt be aluminum nitrate, aluminium chloride and aluminum sulfate.
Preferably, wherein, in the step 4, drying temperature be 60 DEG C.
Preferably, wherein, the step 2 is specially：
At ambient temperature, the above-mentioned soluble aluminum salting liquid of certain volume is measured, in 600~700r/min stirring speed 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, regulation mixing speed 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, stop the dropwise addition sodium hydroxide molten White suspension is obtained after liquid, regulation mixing speed to 1100r/min, stirring 10min.
Preferably, wherein, the nonionic surface active agent be AEO.
The present invention at least includes following beneficial effect：
1st, the method for the present invention for preparing soilless sticking specific area boehmite is prepared using hydrothermal method Specific surface area is 510~550m2/ g, pore volume is 1.1~1.5cm3Particle diameter distribution more than/g, uniform particle diameter, and 95% exists 2.5~3.5nm.
2nd, by the selection of raw material, raw material in the method for the present invention for preparing soilless sticking specific area boehmite The adjustment of dropwise addition mode and the change of rate of addition, the introducing of surfactant and the adjustment of crystal pattern, mode of washing Selection so that the boehmite soilless sticking phenomenon prepared.
3rd, the method short preparation period of the present invention for preparing soilless sticking specific area boehmite, substantially increase it is thin The industrialized speed of production of diaspore, so as to greatly reduce the production cost of boehmite.
Further advantage, target and the feature of the present invention embodies part by following explanation, and part will also be by this The research and practice of invention and be understood by the person skilled in the art.
Embodiment
With reference to embodiment, the present invention is described in further detail, to make 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 from one or many The presence or addition of individual other elements or its combination.
<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: the metabisulfite solution that the sodium hydroxide solution that compound concentration is 6mol/L respectively, concentration are 8.5mol/L And the liquor alumini chloridi that concentration is 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 Mix under speed, 6mol/L sodium hydroxide solution and 8.5mol/L metabisulfite solution are added drop-wise to certain volume simultaneously In 0.62mol/L liquor alumini chloridi, 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, regulation mixing speed to 800 ~1000r/min, the rate of addition of regulation sodium hydroxide solution is 1.9mL/min, and according to the dropwise addition speed of sodium hydroxide solution The rate of addition of degree regulation metabisulfite solution, 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, regulation mixing speed to 1100r/ is added dropwise White suspension is obtained after min, stirring 10min；
Step 3: under room temperature condition and 400r/min mixing speed, ethoxylated dodecyl alcohol is added drop-wise to State in white suspension, mixture is obtained after 15~20min of stirring, the quality of ethoxylated dodecyl alcohol and white suspension Mass ratio is 1:50, the concentration of ethoxylated dodecyl alcohol is 0.1mol/kg；
Crystallization is carried out Step 4: mixture is transferred in autoclave, temperature in use is 45 DEG C of deionized water pair Material after crystallization carries out multiple times of filtration not sulphate-containing ion, and the pH value of filtrate is 7.0 ± 0.5 into filtrate, to filtering Material afterwards is dried at 60 DEG C, obtains soilless sticking specific area boehmite；
Crystallization is carried out to mixture to concretely comprise the following steps：
First, the autoclave for being loaded with mixture is placed in 30 DEG C of baking oven, regulation heating rate be 0.2 DEG C/ Min, when the temperature of the baking oven reaches 40 DEG C, maintains the temperature, makes the autoclave for being loaded with mixture in the temperature Lower insulation 10min；
Then, under 0.5 DEG C/min heating rate, the temperature of baking oven is increased to 50 DEG C, and makes to be loaded with mixture Autoclave be incubated 20min at such a temperature；
Finally, under 10 DEG C/min heating rate, the temperature of baking oven is increased to 90 DEG C, and makes to be loaded with mixture Autoclave is incubated 8~9h at such a temperature.
Morphologic detection is carried out to boehmite prepared by the embodiment, it was demonstrated that the purity of the boehmite is high, without miscellaneous Matter, uniform particle diameter, more than 95% particle size range is distributed in 2.5~3.5nm, and specific surface area is 516m2/ g, pore volume is 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: the sodium sulphate that the sodium hydroxide solution that compound concentration is 5.5mol/L respectively, concentration are 7.5mol/L is molten Liquid and the aluminum nitrate solution that concentration is 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 Mix under speed, 5.5mol/L sodium hydroxide solution and 7.5mol/L metabisulfite solution are added drop-wise to certain volume simultaneously In 0.6mol/L liquor alumini chloridi, 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, regulation mixing speed to 800~ 1000r/min, the rate of addition of regulation sodium hydroxide solution is 1.8mL/min, and according to the rate of addition of sodium hydroxide solution The rate of addition of metabisulfite solution is adjusted, 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 keep the dropwise addition speed of sodium hydroxide solution Spend for 1.8mL/min；After being added dropwise the pH value of solution be 8 when, stop be added dropwise sodium hydroxide solution, regulation mixing speed to White suspension is obtained after 1100r/min, stirring 10min；
Step 3: under room temperature condition and 400r/min mixing speed, ethoxylated dodecyl alcohol is added drop-wise to State in white suspension, mixture is obtained after 15~20min of stirring, the quality of ethoxylated dodecyl alcohol and white suspension Mass ratio is 1:150, the concentration of ethoxylated dodecyl alcohol is 0.1mol/kg；
Crystallization is carried out Step 4: mixture is transferred in autoclave, temperature in use is 45 DEG C of deionized water pair Material after crystallization carries out multiple times of filtration not sulphate-containing ion, and the pH value of filtrate is 7.0 ± 0.5 into filtrate, to filtering Material afterwards is dried at 60 DEG C, obtains soilless sticking specific area boehmite；
Crystallization is carried out to mixture to concretely comprise the following steps：
First, the autoclave for being loaded with mixture is placed in 30 DEG C of baking oven, regulation heating rate be 0.4 DEG C/ Min, when the temperature of the baking oven reaches 40 DEG C, maintains the temperature, makes the autoclave for being loaded with mixture in the temperature Lower insulation 10min；
Then, under 0.6 DEG C/min heating rate, the temperature of baking oven is increased to 50 DEG C, and makes to be loaded with mixture Autoclave be incubated 20min at such a temperature；
Finally, under 10 DEG C/min heating rate, the temperature of baking oven is increased to 90 DEG C, and makes to be loaded with mixture Autoclave is incubated 8~9h at such a temperature.
Morphologic detection is carried out to boehmite prepared by the embodiment, it was demonstrated that the purity of the boehmite is high, without miscellaneous Matter, uniform particle diameter, more than 95% particle size range is distributed in 2.5~3.5nm, and specific surface area is 539m2/ g, pore volume is 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: the sodium sulphate that the sodium hydroxide solution that compound concentration is 5.8mol/L respectively, concentration are 6.2mol/L is molten Liquid and the aluminum sulfate solution that concentration is 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, regulation 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 White suspension is obtained after stating sodium hydroxide solution, regulation mixing speed to 1100r/min, stirring 10min；
Step 3: under room temperature condition and 400r/min mixing speed, ethoxylated dodecyl alcohol is added drop-wise to State in white suspension, mixture is obtained after 15~20min of stirring, the quality of ethoxylated dodecyl alcohol and white suspension Mass ratio is 1:150, the concentration of ethoxylated dodecyl alcohol is 0.1mol/kg；
Crystallization is carried out Step 4: mixture is transferred in autoclave, temperature in use is 45 DEG C of deionized water pair Material after crystallization carries out multiple times of filtration not sulphate-containing ion, and the pH value of filtrate is 7.0 ± 0.5 into filtrate, to filtering Material afterwards is dried at 60 DEG C, obtains soilless sticking specific area boehmite；
Crystallization is carried out to mixture to concretely comprise the following steps：
First, the autoclave for being loaded with mixture is placed in 30 DEG C of baking oven, regulation heating rate be 0.5 DEG C/ Min, when the temperature of the baking oven reaches 40 DEG C, maintains the temperature, makes the autoclave for being loaded with mixture in the temperature Lower insulation 10min；
Then, under 0.5 DEG C/min heating rate, the temperature of baking oven is increased to 50 DEG C, and makes to be loaded with mixture Autoclave be incubated 20min at such a temperature；
Finally, under 10 DEG C/min heating rate, the temperature of baking oven is increased to 90 DEG C, and makes to be loaded with mixture Autoclave is incubated 8~9h at such a temperature.
Morphologic detection is carried out to boehmite prepared by the embodiment, it was demonstrated that the purity of the boehmite is high, without miscellaneous Matter, uniform particle diameter, more than 95% particle size range is distributed in 2.5~3.5nm, and specific surface area is 550.2m2/ g, pore volume is 1.49cm3/g。
Amount of the invention by sulfate radical in the increase sulfate in aluminum soluble salt and sodium hydroxide course of reaction, and Rate of addition and dropwise addition order between each reactant, beneficial to the boehmite for preparing macropore volume, and by non-ionic The cooperation of the crystallization steps for adding time and later stage of surfactant, can increase thin water aluminium on the basis of soilless sticking is ensured The specific surface area of stone, and the preparation time of boehmite is reduced, production efficiency is improved, production cost is reduced, is easy to Industrialized production, and be the γ-Al in later stage2O3Preparation lay a solid foundation.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, the present invention is not limited In specific details and shown here as the embodiment with description.

Claims (9)

1. a kind of method for preparing soilless sticking specific area boehmite, it is characterised in that comprise the following steps：
Step 1: the sodium hydroxide powder after weighing is dissolved in deionized water, and it is 5.5~6.0mol/L's to be configured to concentration Sodium hydroxide solution；A certain amount of sodium sulfate powder is weighed, the sulphur that concentration is 6.2~8.5mol/L is configured to using deionized water Acid sodium solution；And weigh a certain amount of aluminum soluble salt, be dissolved in being configured in deionized water concentration for 0.58~ 0.62mol/L soluble aluminum salting liquid；
Step 2: at ambient temperature, the above-mentioned soluble aluminum salting liquid of certain volume is measured, in stirring for 600~700r/min Mix under speed, the sodium hydroxide solution and the metabisulfite solution are 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；Wait to drip Plus the pH value of rear solution to 5~6 when, regulation mixing speed to 800~1000r/min reduces the drop of the sodium hydroxide solution Acceleration, and according to the rate of addition of the rate of addition of the sodium hydroxide solution regulation 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；Wait to be added dropwise When the pH value of solution is 7.9~8.3 afterwards, stop that the sodium hydroxide solution is added dropwise, regulation mixing speed is stirred to 1100r/min Mix and white suspension is obtained after 10min；
Step 3: under room temperature condition and 400r/min mixing speed, by certain mass and certain density non-ionic Surfactant is added drop-wise in the white suspension, and mixture is obtained after 15~20min of stirring；
Crystallization is carried out Step 4: the mixture is transferred in autoclave, the material obtained after crystallization is carried out successively Filtering and drying, obtain soilless sticking specific area boehmite.
2. a kind of method for preparing soilless sticking specific area boehmite according to claim 1, it is characterised in that described In step 4, crystallization is carried out to the mixture and concretely comprised the following steps：
First, the autoclave for being loaded with mixture is placed in 30 DEG C of baking oven, regulation heating rate be 0.2~0.6 DEG C/ Min, when the temperature of the baking oven reaches 40 DEG C, maintains the temperature, makes the autoclave for being loaded with mixture in the temperature Lower insulation 10min；
Then, under 0.2~0.6 DEG C/min heating rate, the temperature of baking oven is increased to 50 DEG C, and makes to be loaded with mixture Autoclave be incubated 20min at such a temperature；
Finally, under 10 DEG C/min heating rate, the temperature of baking oven is increased to 90 DEG C, and makes the high pressure that is loaded with mixture Reactor is incubated 8~9h at such a temperature.
3. a kind of method for preparing soilless sticking specific area boehmite according to claim 2, it is characterised 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.
4. a kind of method for preparing soilless sticking specific area boehmite according to claim 1, it is characterised in that described In step 4, temperature in use carries out multiple times of filtration not containing sulfate radicals into filtrate to the material after crystallization for 45 DEG C of deionized water Ion, and the pH value of filtrate is 7.0 ± 0.5.
5. a kind of method for preparing soilless sticking specific area boehmite according to claim 1, it is characterised in that described The concentration of nonionic surface active agent is 0.1mol/kg.
6. a kind of method for preparing soilless sticking specific area boehmite according to claim 1, it is characterised in that described Aluminum soluble salt is aluminum nitrate, aluminium chloride and aluminum sulfate.
7. a kind of method for preparing soilless sticking specific area boehmite according to claim 1, it is characterised in that described In step 4, drying temperature is 60 DEG C.
8. a kind of method for preparing soilless sticking specific area boehmite according to claim 1, it is characterised in that described Step 2 is specially：
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 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, regulation mixing speed to 800~1000r/min adjusts the sodium hydroxide molten 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 regulation 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.
9. a kind of method for preparing soilless sticking specific area boehmite according to claim 1, it is characterised in that described Nonionic surface active agent is AEO.
CN201710212129.2A 2017-04-01 2017-04-01 A method of preparing soilless sticking high specific area boehmite Expired - Fee Related CN106966417B (en)

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN113666404A (en) * 2021-09-23 2021-11-19 北京智飞绿竹生物制药有限公司 Preparation method of high-concentration nano-scale aluminum hydroxide adjuvant suitable for large-scale production
CN115594207A (en) * 2021-07-08 2023-01-13 北京化工大学（Cn） Large-hole boehmite with large specific surface area and preparation method thereof

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