CN112573552A - Method for preparing boehmite by using high-silicon aluminum-containing material - Google Patents

Method for preparing boehmite by using high-silicon aluminum-containing material Download PDF

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CN112573552A
CN112573552A CN202011571233.9A CN202011571233A CN112573552A CN 112573552 A CN112573552 A CN 112573552A CN 202011571233 A CN202011571233 A CN 202011571233A CN 112573552 A CN112573552 A CN 112573552A
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aluminum
reaction
boehmite
alkali liquor
silicon
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CN112573552B (en
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李光辉
罗骏
曹鹏旭
蒋昊
饶明军
张鑫
姜涛
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Central South University
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Central South University
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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
    • C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
    • C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
    • C01F7/141—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent
    • C01F7/142—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent with carbon dioxide
    • 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
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • 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
    • C01P2006/80—Compositional purity

Abstract

The invention belongs to the technical field of inorganic material preparation, and particularly discloses a boehmite preparation method, which comprises the following steps: step 1): carrying out hydrothermal treatment on the slurry containing the high-silicon aluminum-containing material, lime and MOH, and carrying out solid-liquid separation to obtain aluminum-containing alkali liquor; m is an alkali metal element; controlling the concentration of MOH in the aluminum-containing alkali liquor to be 5-30 g/L; the molar ratio of M to Al is 1-5; step 2): heating the aluminum-containing alkali liquor to 60-160 ℃, and blowing CO-containing solution into the aluminum-containing alkali liquor2When the pH of the solution is reduced to 9.8-11.0, stopping introducing CO2And after the reaction is finished, carrying out solid-liquid separation to obtain boehmite. The invention can adopt low-quality aluminum raw materials to leach alumina with high selectivity and prepare boehmite.

Description

Method for preparing boehmite by using high-silicon aluminum-containing material
Technical Field
The invention relates to a method for preparing boehmite from a high-silicon aluminum-containing material, belonging to the technical field of inorganic material preparation.
Background
China is a large aluminum resource consuming country, the production capacity and consumption of alumina in China account for more than 50% of the total global amount in recent years, and the reserve of aluminum resources available for mining in China is less than 3% of the total global amount. In 2019, the yield of bauxite in China reaches 7500 ten thousand tons, imported bauxite exceeds 10000 ten thousand tons, and the external dependence of aluminum resources exceeds 57 percent. A large amount of low-quality aluminum resources (also called high-silicon aluminum-containing materials) such as high-silicon bauxite, clay, red mud, fly ash, coal gangue, tailings and the like are stored in China, and the low-quality aluminum resources can be developed and utilized to delay the consumption of high-quality bauxite resources, so that the method has important significance on sustainable and healthy development of resources and environment.
Boehmite is a hydrated alumina γ -AlOOH found in bauxite in 1925 by the german chemist john boehm and is named Boehmite under its name. Pure boehmite is a white crystal which tends to contain impurities and to appear yellowish green or brownish red, and decomposes to γ -Al at temperatures exceeding 400 ℃2O3. Since boehmite has special properties such as large specific surface area and porosity, good peptization and dispersibility, high heat-resistant temperature, low hardness and the like, it has been widely used in the fields of flame retardancy, surface coatings, catalysts and carriers, lithium battery separators, ceramics, semiconductors and the like.
Since the source of the natural boehmite is limited and is limited by the purity, the structure, the morphology and the like of raw materials, most of the boehmite used in the production is obtained by artificial synthesis. The existing artificial boehmite synthesis method mainly comprises a hydrothermal method, a sol-gel method, a microemulsion method, an electrochemical method, a hydrothermal coupling method and the like, the used raw materials mainly comprise chemical reagents with high purity, such as aluminum sulfate, aluminum chloride, aluminum nitrate and the like, the production cost is high, and the process is complex. Therefore, research and development of alternative aluminum raw materials to prepare boehmite products with lower cost and better performance show greater competitive advantages in market competition.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for preparing high-quality boehmite by using a high-silicon aluminum-containing material.
The existing boehmite preparation method mainly utilizes chemical pure reagents as raw materials, has high preparation cost and unsatisfactory added value of products. In view of the technical problems, the present invention attempts to prepare boehmite by using a low-quality aluminum-containing material as a raw material, however, in the initial research and development stage, it was found that due to the complex components of the raw material, numerous side reactions exist in the treatment process, and the selectivity, yield and morphology of the target product are not ideal, and the present inventors have conducted intensive research and provide the following technical solutions:
a method for preparing boehmite by utilizing high-silicon aluminiferous materials comprises the following steps:
step 1):
carrying out hydrothermal treatment on the slurry containing the high-silicon aluminum-containing material, lime and MOH, and carrying out solid-liquid separation to obtain aluminum-containing alkali liquor; m is an alkali metal element;
controlling the concentration of MOH in the aluminum-containing alkali liquor to be 5-30 g/L; the molar ratio of M to Al is 1-5;
step 2):
stirring an aluminum-containing alkali liquor, heating to 60-160 ℃, and blowing CO-containing solution into the solution2When the pH (also called the reaction end point pH) of the solution (reaction solution) is reduced to 9.8-11.0, the introduction of CO is stopped2And after the reaction is finished, carrying out solid-liquid separation to obtain boehmite.
In order to solve the problems of complex side reaction, poor selectivity of target reaction, product impurity phase, poor yield/yield and morphology of target product and the like caused by low-grade aluminum-containing material raw materials, the invention innovatively researches and discovers that based on the combined process of the step (1) and the step (2), the synergistic control of the concentration of MOH at the reaction end point of the step (1), the M/Al molar ratio, the temperature of the step (2) and the pH condition at the end point is further matched, the selectivity of the target reaction can be unexpectedly improved, a boehmite crystal phase product can be obtained at high selectivity, and the morphology of the prepared material can be also unexpectedly regulated. The technical scheme of the invention can obtain high-quality boehmite products based on low-value raw materials with high selectivity, and has great industrial utilization value.
According to the technical scheme, the aluminum-containing raw material is limited to be a high-silicon aluminum-containing material in consideration of maximization of industrial application value; but does not exclude the possibility of analyzing pure aluminum compounds or other aluminum materials than silicon.
In the invention, the high-silicon aluminum-containing material is preferably at least one of fly ash, coal gangue, red mud, bauxite, clay and tailings.
Preferably, in the high-silicon aluminum-containing material, Al is2O310-50% of SiO2The content is 20-80%.
In the invention, in the slurry, CaO/SiO2The molar ratio is 0.5 to 1.0.
Preferably, in the step (1), the liquid-solid ratio in the slurry is 5 to 20 mL/g.
In the invention, before hydrothermal reaction, the concentration of MOH at the end point of the reaction and the molar ratio of M/Al can be regulated and controlled by adding the needed MOH; or adding MOH not less than theoretical reaction amount into the slurry, and supplementing MOH into the solution after hydrothermal reaction to control the concentration as required.
Preferably, in the step (1), the MOH added to the slurry is not less than the theoretical reaction amount, and preferably, the concentration of the caustic alkali in the slurry at the end of the reaction is 1 to 1.2 times the concentration of the MOH in the slurry.
Preferably, in the hydrothermal process, the liquid-solid ratio in the slurry is 5-20 mL/g.
Preferably, the temperature of the hydrothermal reaction is 150-200 ℃.
Preferably, the time of the hydrothermal reaction is 0.1-3 h.
In the invention, after the hydrothermal reaction, solid-liquid separation is carried out to obtain the aluminum-containing alkali liquor. The solid-liquid separation can be achieved based on existing means and equipment, and can be filtration or centrifugation, for example.
The research of the invention finds that the technical problem of unsatisfactory product selectivity caused by low-grade raw materials can be unexpectedly and effectively solved based on the cooperative control of the concentration of the end-point MOH, the molar ratio of M/Al, the temperature in the nucleation reaction process of carbon dioxide and the pH of the end-point, the product selectivity of the boehmite phase can be unexpectedly improved, the purity of the boehmite phase can be improved, the morphology of the boehmite phase can be unexpectedly improved, and the industrial application prospect of the boehmite phase can be further improved.
Preferably, the MOH concentration of the aluminum-containing alkali liquor is controlled to be 10-20 g/L; more preferably 10 to 15 g/L. It has been found that control under preferred conditions contributes to further improved cooperativity with other conditions, and to further improved boehmite phase and yield and morphology.
Preferably, M is Na or K.
Preferably, in the aluminum-containing alkali liquor, the molar ratio of M/Al is 1-3.5; more preferably 1 to 1.5. Research finds that under the coordination of the MOH concentration and the M/Al, the synthesis selectivity of boehmite can be further improved.
It has been found that control under preferred conditions contributes to further improved cooperativity with other conditions, and to further improved boehmite phase and yield and morphology.
In the invention, the silicon content index of the aluminum-containing alkali liquor is more than or equal to 200; the preferred silicon content index is greater than or equal to 400.
In the present invention, the carbon dioxide is continuously bubbled into the reaction system during the reaction.
Said CO-containing2The gas of (2) is pure carbon dioxide gas, or a mixed gas of carbon dioxide and at least one of nitrogen, oxygen and inert gas; preferably, it contains CO2In the gas of (2), CO2The volume percentage of (A) is 50-100%. Said CO-containing2The gas being SO-free2、SO3、NO2、N2O5And the impurity gas dissolved in the aluminum-containing alkali liquor.
Preferably, it contains CO2The flow rate of the gas is 0.5L/min to 20L/min; more preferably 2 to 5L/min.
Preferably, the pH value of the reaction end point is controlled to be 9.8-10.5; more preferably 9.8 to 10. In this end-point pH range, MOH has been replaced by CO2The carbonic acid formed by dissolution is neutralized, and the reaction medium is mainly M2CO3(ii) a If further CO is introduced2Then the reaction medium is directed to form MHCO3The direction change of the boehmite is not beneficial to the stability of the prepared boehmite crystal and the regulation and control of the crystal morphology.
In the step 2), the nucleation reaction is an atmospheric nucleation reaction or a hydrothermal nucleation reaction. The research of the invention finds that under the combined control of the MOH and the M/Al ratio, the temperature in the nucleation reaction process is further controlled, which is beneficial to further improving the reaction selectivity of boehmite and is also beneficial to synergistically controlling the morphology of the product.
The normal pressure nucleation reaction is carried out in open reaction equipment or pressure-resistant reaction equipment, and the temperature is lower than 100 ℃; preferably 85 to 95 ℃. It was found that, under the described MOH, M/Al ratio and temperature synergistic control, a product with porous spindle type could be synthesized unexpectedly. In addition, when the reaction temperature is 60-70 ℃; the boehmite product with a lamellar structure can be obtained advantageously.
The hydrothermal nucleation reaction is carried out in a pressure-resistant reaction vessel, and the temperature in the reaction process is 105-160 ℃; preferably 120 to 150 ℃. It has been found that under the preferred hydrothermal conditions it contributes to obtaining a fibrous boehmite product.
The research of the invention finds that the nucleation reaction time is further controlled, which is beneficial to further improving the appearance of the product.
Preferably, the nucleation reaction time is 10-90 min; further preferably 30-70 min; more preferably 50 to 60 min.
In the invention, after the required pH is reached, the reaction is terminated, and the boehmite product can be obtained through solid-liquid separation, deionized water washing and drying.
In the invention, the deionized water for washing can be prepared by purifying tap water by calcium silicate hydrate crystal whiskers prepared by a hydrothermal process.
Preferably, the synthetic boehmite is a porous material having a sheet-like, fibrous, spindle-like morphology.
The invention relates to a method for preparing boehmite from high-silicon aluminum-containing material, wherein the boehmite prepared under the optimized condition is porous spindle-shaped spherical nano-particles, and the specific surface area is as high as 300-600 m2The catalyst has high activity, is suitable for being used as a catalyst and a carrier thereof, a coating material, a battery diaphragm material and the like, and has high economic value.
The invention discloses a preferable method for preparing boehmite from high-silicon aluminum-containing materials, which comprises the following steps:
1) according to CaO/SiO by hydrothermal process2Dissolving alumina in an aluminum-containing material to obtain an aluminum-containing alkali solution under the conditions that the molar ratio is 0.5-1.0, the MOH concentration is 5-30 g/L, and the liquid-solid ratio is 5-20 mL/g, the reaction temperature is 150-200 ℃ and the reaction time is 0.1-3 h; the aluminum-containing materials include, but are not limited to, high-silicon bauxite, red mud, fly ash, coal gangue, clay, tailings and the like; the MOH concentration in the solution is controlled to be 5-30 g/L, and the M/Al ratio is controlled to be 1-5.
2) Stirring and heating the aluminum-containing alkali liquor to 60-160 ℃, and introducing CO while stirring at a flow rate of 0.5-20L/min2Until the pH value of the solution is reduced to 9.8-11.0, stopping introducing CO2And (5) controlling the total time of the whole process to be 10-90 min. After the reaction is finished, a boehmite product is obtained through solid-liquid separation, washing and drying.
The research of the invention finds that hydrothermal reaction in the solution can generate a plurality of silicon-aluminum minerals, wherein the crystallization conditions of calcium silicate hydrate are similar to those of the sodium ternatrolite, analcime, sodalite, hydrogarnet and the like, so that the reaction conditions need to be controlled in particular to ensure that the hydrothermal process is oriented to generate the calcium silicate hydrate. Aiming at the technical problem, the invention innovatively discovers that based on the synergy of all preparation conditions, the boehmite phase reaction can be unexpectedly and selectively promoted to be carried out, the crystal phase purity of the boehmite product can be improved, the morphology of the product can be regulated and controlled, and the application prospect of the boehmite product can be improved.
Advantageous effects
Based on the synergistic control of the MOH concentration, the M/Al molar ratio, the nucleation reaction mode, the temperature and the end-point pH, the method can unexpectedly solve the problems of more side reactions and impurity phase of products caused by low-grade raw materials, and can obtain boehmite with high crystal phase purity and special morphology.
The aluminum-containing materials such as high-silicon bauxite, red mud, fly ash, coal gangue, clay, tailings and the like are used as raw materials, so that the dependence of boehmite production on high-quality bauxite or aluminum chemical reagents can be reduced, and partial solid wastes are cooperatively treated, so that the method has high economic and environmental protection values.
Drawings
FIG. 1 is an XRD of the synthesized product of example 6 of the present invention;
FIG. 2 is a high magnification SEM of the synthesized product of example 6 of the present invention.
FIG. 3 is a high magnification SEM of the synthesized product of example 10 of the present invention.
FIG. 4 is a low magnification SEM of the synthesized product of example 11 of the present invention.
FIG. 5 is a high magnification SEM of the synthesized product of comparative example 1 of the present invention.
As can be seen from fig. 1: the synthesized boehmite product has high crystalline phase purity and dispersed XRD diffraction peaks.
As can be seen from FIG. 2, the boehmite has a spindle-shaped morphology, developed pores and a high specific surface area.
As can be seen from fig. 3, when the synthesis temperature is low, boehmite is generated in a flake form.
As can be seen from fig. 4, when the synthesis temperature is higher, fibrous boehmite is generated.
As can be seen from FIG. 5, when MOH and M/Al of the aluminum-containing alkali solution are relatively high, dawsonite having a flaky morphology is produced.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Example 1:
step 1):
al in gangue2O310% of SiO 270% of Al2O3/SiO2The mass ratio (aluminum-silicon ratio) of (a) is 0.14;
in a pressure-resistant reaction device, the pulverized coal gangue, lime and NaOH are mixed according to CaO/SiO2Preparing slurry with the molar ratio of 0.8, the concentration of NaOH of 5g/L and the liquid-solid ratio of 20mL/g, carrying out hydrothermal treatment for 0.1h at the reaction temperature of 200 ℃, and after the reaction is finished, carrying out solid-liquid separation to obtain an aluminum-containing alkali liquor; the dissolution rate of the alumina in the coal gangue reaches 20 percent, the concentration of NaOH in the aluminum-containing alkali liquor is controlled to be 4g/L, and the molar ratio of Na/Al is 2;
step 2):
heating aluminum-containing alkali liquor to 90 ℃, and blowing CO-containing solution into the aluminum-containing alkali liquor2Controlled introduction of a gas containing CO2The flow rate of the gas is 2L/min, and when the pH of the solution is reduced to 10.0, the introduction of CO is stopped2And (3) controlling the nucleation reaction time to be 60 min. After the reaction is finished, filtering and drying the obtained slurry to obtain the boehmite with the spindle-shaped morphology, wherein the diameter of the product is about 100nm, the purity reaches 96.52 percent, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 94 percent.
Example 2:
compared with the example 1, the difference is mainly that the concentration of NaOH in the aluminum-containing alkali liquor is controlled to be 8g/L, and the molar ratio of Na/Al is 2.5;
step 1):
in a pressure-resistant reaction device, the pulverized coal gangue (same as the embodiment 1), lime and NaOH are mixed according to CaO/SiO2Preparing slurry with the molar ratio of 0.8, the concentration of NaOH of 10g/L and the liquid-solid ratio of 15mL/g, carrying out hydrothermal treatment for 0.1h at the reaction temperature of 200 ℃, and after the reaction is finished, carrying out solid-liquid separation to obtain an aluminum-containing alkali liquor; the dissolution rate of alumina in the coal gangue reaches 32 percent, the concentration of NaOH in the aluminum-containing alkali liquor is controlled to be 8g/L, and the molar ratio of Na/Al is 2.5;
step 2):
heating aluminum-containing alkali liquor to 90 ℃, and blowing CO-containing solution into the aluminum-containing alkali liquor2Controlled introduction of a gas containing CO2The flow rate of the gas (2L/min) when the pH of the solution decreases toAfter 10.0, the introduction of CO was stopped2And (3) controlling the nucleation reaction time to be 60 min. After the reaction is finished, filtering and drying the obtained slurry to obtain the boehmite with the spindle-shaped morphology, wherein the diameter of the product is about 10nm, the purity is up to 95.70%, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 94%.
Example 3:
compared with the example 1, the difference is mainly that the concentration of NaOH in the aluminum-containing alkali liquor is controlled to be 15g/L, and the molar ratio of Na/Al is 3.3;
step 1):
in a pressure-resistant reaction device, the pulverized coal gangue (same as the embodiment 1), lime and NaOH are mixed according to CaO/SiO2Preparing slurry with the molar ratio of 0.8, the concentration of NaOH of 20g/L and the liquid-solid ratio of 10mL/g, carrying out hydrothermal treatment for 0.1h at the reaction temperature of 200 ℃, and after the reaction is finished, carrying out solid-liquid separation to obtain an aluminum-containing alkali liquor; the dissolution rate of alumina in the coal gangue reaches 45 percent, the concentration of NaOH in the aluminum-containing alkali liquor is controlled to be 15g/L, and the molar ratio of Na/Al is 3.3;
step 2):
heating aluminum-containing alkali liquor to 90 ℃, and blowing CO-containing solution into the aluminum-containing alkali liquor2Controlled introduction of a gas containing CO2The flow rate of the gas is 2L/min, and when the pH of the solution is reduced to 10.0, the introduction of CO is stopped2And (3) controlling the nucleation reaction time to be 60 min. After the reaction is finished, filtering and drying the obtained slurry to obtain the boehmite with the spindle-shaped morphology, wherein the diameter of the product is about 10nm, the purity is as high as 95.20%, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 92%.
Example 4:
compared with the example 1, the difference is mainly that the concentration of NaOH in the aluminum-containing alkali liquor is controlled to be 22g/L, and the molar ratio of Na/Al is 3.1;
step 1):
in a pressure-resistant reaction device, the pulverized coal gangue (same as the embodiment 1), lime and NaOH are mixed according to CaO/SiO2Preparing slurry with the molar ratio of 0.8, the concentration of NaOH of 30g/L and the liquid-solid ratio of 5mL/g, carrying out hydrothermal treatment for 0.1h at the reaction temperature of 200 ℃, and after the reaction is finished, carrying out solid-liquid separation to obtain an aluminum-containing alkali liquor; oxidation in coal gangueThe dissolution rate of the aluminum reaches 29 percent, the concentration of NaOH in the aluminum-containing alkali liquor is controlled to be 22g/L, and the molar ratio of Na/Al is 3.1;
step 2):
heating aluminum-containing alkali liquor to 90 ℃, and blowing CO-containing solution into the aluminum-containing alkali liquor2Controlled introduction of a gas containing CO2The flow rate of the gas is 2L/min, and when the pH of the solution is reduced to 10.0, the introduction of CO is stopped2And (3) controlling the nucleation reaction time to be 60 min. After the reaction is finished, filtering and drying the obtained slurry to obtain the boehmite with the spindle-shaped morphology, wherein the diameter of the product is about 10nm, the purity is up to 96.40%, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 93%.
Example 5:
step 1):
in a pressure-resistant reaction device, the pulverized coal gangue (same as the embodiment 1), lime and NaOH are mixed according to CaO/SiO2Preparing slurry with the molar ratio of 0.8, the concentration of NaOH of 20g/L and the liquid-solid ratio of 10mL/g, carrying out hydrothermal treatment for 3h at the reaction temperature of 150 ℃, and after the reaction is finished, carrying out solid-liquid separation to obtain an aluminum-containing alkali liquor; the dissolution rate of alumina in the coal gangue reaches 25 percent, the concentration of NaOH in the aluminum-containing alkali liquor is controlled to be 15g/L, and the molar ratio of Na/Al is 1.5;
step 2):
heating aluminum-containing alkali liquor to 90 ℃, and blowing CO-containing solution into the aluminum-containing alkali liquor2Controlled introduction of a gas containing CO2The flow rate of the gas is 2L/min, and when the pH of the solution is reduced to 10.0, the introduction of CO is stopped2And (3) controlling the nucleation reaction time to be 60 min. After the reaction is finished, filtering and drying the obtained slurry to obtain the boehmite with the spindle-shaped morphology, wherein the diameter of the product is about 10nm, the purity is up to 98.50%, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 94%.
Example 6:
step 1):
al in gangue2O310% of SiO 270% of Al2O3/SiO2The mass ratio (aluminum-silicon ratio) of (a) is 0.14;
in a pressure-resistant reaction device, the pulverized coal gangue, lime,NaOH in accordance with CaO/SiO2Preparing slurry with the molar ratio of 0.8, the concentration of NaOH of 20g/L and the liquid-solid ratio of 10mL/g, carrying out hydrothermal treatment for 1h at the reaction temperature of 180 ℃, and after the reaction is finished, carrying out solid-liquid separation to obtain an aluminum-containing alkali liquor; the dissolution rate of alumina in the coal gangue reaches 54 percent, the concentration of NaOH in the aluminum-containing alkali liquor is controlled to be 15g/L, and the molar ratio of Na/Al is 1.0;
step 2):
heating aluminum-containing alkali liquor to 90 ℃, and blowing CO-containing solution into the aluminum-containing alkali liquor2Controlled introduction of a gas containing CO2The flow rate of the gas is 2L/min, and when the pH of the solution is reduced to 10.0, the introduction of CO is stopped2And (3) controlling the nucleation reaction time to be 60 min. After the reaction is finished, filtering and drying the obtained slurry to obtain the boehmite with the spindle-shaped morphology, wherein the diameter of the product is about 10nm, the purity is as high as 99.60%, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 95%.
Example 7
The only difference compared to example 6 is that in step (2), the pH was 9.8. Thus obtaining the boehmite with spindle-shaped morphology, the purity of which is as high as 99.20 percent, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 96 percent.
Example 8
The only difference compared to example 6 is that in step (2), the pH was 10.5. Thus obtaining the boehmite with spindle-shaped morphology, the purity of which is as high as 99.60 percent, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 92 percent.
Example 9
The only difference compared to example 6 is that in step (2), the pH was 11. Thus obtaining the boehmite with spindle-shaped morphology, the purity of which is as high as 99.8 percent and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 80 percent.
Example 10
The only difference compared with example 6 is that in step (2), which was carried out in an atmospheric vessel, the temperature during the treatment was 60 ℃. The boehmite with the sheet shape is obtained, the purity is as high as 97.50 percent, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 93 percent.
Example 11
The only difference compared with example 6 is that in step (2), the treatment was carried out in a pressure-resistant vessel at a temperature of 120 ℃. The boehmite with the fibrous morphology is obtained, the purity is up to 99.20 percent, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 91 percent.
Example 12
The only difference compared with example 6 is that in step (2), the treatment was carried out in a pressure-resistant vessel at a temperature of 160 ℃. The boehmite with the fibrous morphology is obtained, the purity is up to 99.22 percent, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 85 percent.
Example 13
The only difference compared with example 6 is that in step (2), the treatment was carried out in a pressure-resistant vessel, and the holding time in the treatment was 10 min. The boehmite with flaky and spindle-shaped morphology is obtained, the purity is as high as 99.70%, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 88%.
Example 14
The only difference compared with example 6 is that in step (2), the treatment was carried out in a pressure-resistant vessel, and the holding time in the treatment was 30 min. Thus obtaining the boehmite with spindle-shaped morphology, the purity of which is as high as 99.50 percent and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 90 percent.
Example 15
The only difference compared with example 6 is that in step (2), the treatment is carried out in a pressure-resistant vessel, and the holding time in the treatment process is 90 min. Thus obtaining the boehmite with spindle and fiber shapes, the purity of which is up to 99.20 percent, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 95 percent.
Example 16:
raw materials are changed, and the steps are as follows:
step 1):
al in red mud2O3Content of 15% SiO220% of Al2O3/SiO2The mass ratio (aluminum-silicon ratio) of (a) is 0.75; removing iron oxide in the red mud by conventional technical means such as reduction roasting-magnetic separation, and removing Al in the red mud after iron removal2O3The content is increased to 22 percent and SiO 270% of Al2O3/SiO2The mass ratio of (a) is still 0.75;
in pressure-resistant equipment, the red mud after iron removal, lime and NaOH are mixed according to CaO/SiO2Preparing slurry with the molar ratio of 0.8, the concentration of NaOH of 20g/L and the liquid-solid ratio of 10mL/g, carrying out hydrothermal treatment for 1h at the reaction temperature of 180 ℃, and after the reaction is finished, carrying out solid-liquid separation to obtain an aluminum-containing alkali liquor; through hydrothermal treatment, the dissolution rate of alumina in the red mud reaches 50 percent; controlling the concentration of NaOH in the aluminum-containing alkali liquor to be 18g/L and the molar ratio of Na/Al to be 2;
step 2):
heating aluminum-containing alkali liquor to 90 ℃, and blowing CO-containing solution into the aluminum-containing alkali liquor2Controlled introduction of a gas containing CO2The flow rate of the gas is 2L/min, and when the pH of the solution is reduced to 10.0, the introduction of CO is stopped2And (3) controlling the nucleation reaction time to be 60 min. After the reaction is finished, filtering and drying the obtained slurry to obtain the boehmite with the spindle-shaped morphology, wherein the diameter of the product is about 10nm, the purity is as high as 99.26%, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 94%.
Example 17:
raw materials are changed, and the steps are as follows:
step 1):
al in kaolin2O335% of SiO 260% of Al2O3/SiO2The mass ratio (aluminum-silicon ratio) of (A) is 0.6;
in a pressure-resistant device, kaolin, lime and NaOH are mixed according to CaO/SiO2Preparing slurry with the molar ratio of 0.8, the concentration of NaOH of 20g/L and the liquid-solid ratio of 10mL/g, carrying out hydrothermal treatment for 1h at the reaction temperature of 180 ℃, and after the reaction is finished, carrying out solid-liquid separation to obtain an aluminum-containing alkali liquor; through hydrothermal treatment, the dissolution rate of alumina in kaolin is as high as 55 percent; controlling the concentration of NaOH in the aluminum-containing alkali liquor to be 14g/L and the molar ratio of Na/Al to be 1.5;
step 2):
heating aluminum-containing alkali liquor to 90 ℃, and blowing CO-containing solution into the aluminum-containing alkali liquor2Controlled introduction of a gas containing CO2The flow rate of the gas is 2L/min, and when the pH of the solution is reduced to 10, the introduction of CO is stopped2And (3) controlling the nucleation reaction time to be 60 min. Reaction junctionAnd finally, filtering and drying the obtained slurry to obtain the boehmite with the spindle-shaped morphology, wherein the diameter of the product is about 10nm, the purity is up to 99.20%, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 96%.
Example 18:
raw materials are changed, and the steps are as follows:
step 1):
al in fly ash2O320% of SiO 250% of Al2O3/SiO2The mass ratio (aluminum-silicon ratio) of (A) is 0.4;
in a pressure-resistant device, fly ash, lime and KOH are mixed according to CaO/SiO2Preparing slurry with the molar ratio of 0.8, the concentration of NaOH of 20g/L and the liquid-solid ratio of 10mL/g, carrying out hydrothermal treatment for 1h at the reaction temperature of 180 ℃, and after the reaction is finished, carrying out solid-liquid separation to obtain an aluminum-containing alkali liquor; through hydrothermal treatment, the dissolution rate of alumina in the fly ash reaches up to 20 percent; controlling the concentration of NaOH in the aluminum-containing alkali liquor to be 16g/L and the molar ratio of Na/Al to be 4.7;
step 2):
heating aluminum-containing alkali liquor to 90 ℃, and blowing CO-containing solution into the aluminum-containing alkali liquor2Controlled introduction of a gas containing CO2The flow rate of the gas is 2L/min, and when the pH of the solution is reduced to 10.0, the introduction of CO is stopped2And (3) controlling the nucleation reaction time to be 60 min. After the reaction is finished, filtering and drying the obtained slurry to obtain the boehmite with the spindle-shaped morphology, wherein the diameter of the product is about 10nm, the purity is as high as 99.00%, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 95%.
Example 19:
raw materials are changed, and the steps are as follows:
step 1):
al in fly ash2O320% of SiO 250% of Al2O3/SiO2The mass ratio (aluminum-silicon ratio) of (A) is 0.4;
in a pressure-resistant device, fly ash, lime and KOH are mixed according to CaO/SiO2Preparing slurry with a molar ratio of 1.0, a KOH concentration of 20g/L and a liquid-solid ratio of 10mL/g, and reacting at 200 deg.CCarrying out hydrothermal treatment for 3h, and after the reaction is finished, carrying out solid-liquid separation to obtain an aluminum-containing alkali liquor; through hydrothermal treatment, the dissolution rate of alumina in the fly ash reaches up to 40 percent; controlling the concentration of KOH in the aluminum-containing alkali liquor to be 15g/L and the molar ratio of K/Al to be 2.2;
step 2):
heating aluminum-containing alkali liquor to 90 ℃, and blowing CO-containing solution into the aluminum-containing alkali liquor2Controlled introduction of a gas containing CO2The flow rate of the gas is 2L/min, and when the pH of the solution is reduced to 10.0, the introduction of CO is stopped2And (3) controlling the nucleation reaction time to be 60 min. After the reaction is finished, filtering and drying the obtained slurry to obtain the boehmite with the spindle-shaped morphology, wherein the diameter of the product is about 10nm, the purity is as high as 99.15%, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 97%.
Example 20:
raw materials are changed, and the steps are as follows:
step 1):
al in high-silicon bauxite2O350% of SiO 220% of Al2O3/SiO2The mass ratio (aluminum-silicon ratio) of (A) is 2.5;
in a pressure-resistant device, high-silicon bauxite, lime and NaOH are mixed according to CaO/SiO2Preparing slurry with the molar ratio of 1.0, the concentration of NaOH of 20g/L and the liquid-solid ratio of 10mL/g, carrying out hydrothermal treatment for 1h at the reaction temperature of 180 ℃, and after the reaction is finished, carrying out solid-liquid separation to obtain an aluminum-containing alkali liquor; through hydrothermal treatment, the dissolution rate of alumina in the high-silicon bauxite reaches up to 35 percent; controlling the concentration of NaOH in the aluminum-containing alkali liquor to be 12g/L and the molar ratio of Na/Al to be 2;
step 2):
heating aluminum-containing alkali liquor to 90 ℃, and blowing CO-containing solution into the aluminum-containing alkali liquor2Controlled introduction of a gas containing CO2The flow rate of the gas is 2L/min, and when the pH of the solution is reduced to 10.0, the introduction of CO is stopped2And (3) gas, wherein the nucleation reaction time is controlled to be 90 min. After the reaction is finished, filtering and drying the obtained slurry to obtain the boehmite with the spindle-shaped morphology, wherein the diameter of the product is about 10nm, the purity is as high as 99.02%, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 96%.
Example 21:
raw materials are changed, and the steps are as follows:
step 1):
al in tailings2O320% of SiO265% of Al2O3/SiO2The mass ratio (aluminum-silicon ratio) of (a) is 0.3;
in pressure-resistant equipment, aluminum-containing tailings, lime and NaOH are mixed according to CaO/SiO2Preparing slurry with the molar ratio of 0.8, the concentration of NaOH of 20g/L and the liquid-solid ratio of 10mL/g, carrying out hydrothermal treatment for 1h at the reaction temperature of 180 ℃, and after the reaction is finished, carrying out solid-liquid separation to obtain an aluminum-containing alkali liquor; through hydrothermal treatment, the dissolution rate of alumina in tailings reaches up to 45 percent; controlling the concentration of NaOH in the aluminum-containing alkali liquor to be 15g/L and the molar ratio of Na/Al to be 1.8;
step 2):
heating aluminum-containing alkali liquor to 90 ℃, and blowing CO-containing solution into the aluminum-containing alkali liquor2Controlled introduction of a gas containing CO2The flow rate of the gas is 2L/min, and when the pH of the solution is reduced to 10.0, the introduction of CO is stopped2And (3) controlling the nucleation reaction time to be 60 min. After the reaction is finished, filtering and drying the obtained slurry to obtain the boehmite with the spindle-shaped morphology, wherein the diameter of the product is about 10nm, the purity is as high as 99.50%, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 92%.
Comparative example 1:
the only difference compared with example 6 is that the concentration of NaOH and the Na/Al molar ratio are not controlled within the required ranges; the method specifically comprises the following steps:
step 1):
the pulverized coal gangue (same as example 6), lime and NaOH are mixed according to CaO/SiO2Preparing slurry with the molar ratio of 0.8, the concentration of NaOH of 50g/L and the liquid-solid ratio of 10mL/g, carrying out hydrothermal treatment for 1h at the reaction temperature of 180 ℃, and after the reaction is finished, carrying out solid-liquid separation to obtain an aluminum-containing alkali liquor; through hydrothermal treatment, the dissolution rate of alumina in kaolin is 35%; the concentration of NaOH in the aluminum-containing alkali liquor is 40g/L, and the molar ratio of Na to Al is 6.2;
step 2):
heating aluminum-containing alkali liquor to 90 ℃, and blowing CO-containing solution into the aluminum-containing alkali liquor2Controlled introduction of a gas containing CO2The flow rate of the gas is 2L/min, and when the pH of the solution is reduced to 10.0, the introduction of CO is stopped2And (3) controlling the nucleation reaction time to be 60 min. After the reaction is finished, filtering and drying the obtained slurry to obtain the flake-shaped dawsonite, wherein the diameter of the product is about 200nm, and the crystallization rate of the aluminum oxide in the aluminum-containing alkali liquor is 90%.
Comparative example 2:
the difference compared to example 6 is mainly that the concentration of NaOH is not controlled within the required range; such as: in the step 1), the pulverized coal gangue (same as the embodiment 6), lime and NaOH are mixed according to CaO/SiO2Preparing slurry with the molar ratio of 0.8, the concentration of NaOH of 0g/L and the liquid-solid ratio of 10mL/g, carrying out hydrothermal treatment for 1h at the reaction temperature of 180 ℃, and after the reaction is finished, carrying out solid-liquid separation to obtain an aluminum-containing alkali liquor; through hydrothermal treatment, the dissolution rate of alumina in kaolin is 0%;
comparative example 3:
the difference compared to example 6 is mainly that the nucleation temperature is not controlled within the range claimed by the present invention, such as: in the step 2), heating the aluminum-containing alkali liquor to 30 ℃, and blowing CO into the solution2Controlled introduction of a gas containing CO2The flow rate of the gas is 2L/min, and when the pH of the solution is reduced to 10, the introduction of CO is stopped2And (3) controlling the nucleation reaction time to be 60 min. After the reaction is finished, the obtained slurry is filtered and dried to obtain an amorphous substance, and the crystallization rate of the alumina in the aluminum-containing alkali liquor is 80 percent.
Comparative example 4:
the difference compared to example 6 is mainly that the nucleation temperature is not controlled within the range claimed by the present invention, such as: in the step 2), heating the aluminum-containing alkali liquor to 200 ℃, and blowing CO into the solution2Controlled introduction of a gas containing CO2The flow rate of the gas is 2L/min, and when the pH of the solution is reduced to 10, the introduction of CO is stopped2And (3) controlling the nucleation reaction time to be 60 min. After the reaction is finished, filtering and drying the obtained slurry to obtain fibrous aluminum hydroxide containing aluminumThe crystallization rate of alumina in the alkali liquor is 75 percent.
Comparative example 5:
the difference compared to example 6 is mainly that the pH of nucleation is not controlled within the claimed range of the invention, such as: in the step 2), heating the aluminum-containing alkali liquor to 90 ℃, and blowing CO into the solution2Controlled introduction of a gas containing CO2The flow rate of the gas is 2L/min, and when the pH value of the solution is reduced to 12, the introduction of CO is stopped2And (3) controlling the nucleation reaction time to be 60 min. After the reaction, the crystallization rate of alumina in the aluminum-containing alkali solution was almost 0%, and almost no precipitation occurred.
Comparative example 6:
the difference compared to example 6 is mainly that the pH of nucleation is not controlled within the claimed range of the invention, such as: in the step 2), heating the aluminum-containing alkali liquor to 90 ℃, and blowing CO into the solution2Controlled introduction of a gas containing CO2The flow rate of the gas is 2L/min, and when the pH of the solution is reduced to 9, the introduction of CO is stopped2And (3) controlling the nucleation reaction time to be 60 min. After the reaction is finished, filtering and drying the obtained slurry to obtain flaky and fibrous dawsonite, wherein the crystallization rate of the aluminum oxide in the aluminum-containing alkali liquor is 93 percent.

Claims (10)

1. A method for preparing boehmite by using high-silicon aluminum-containing materials is characterized by comprising the following steps:
step 1):
carrying out hydrothermal treatment on the slurry containing the high-silicon aluminum-containing material, lime and MOH, and carrying out solid-liquid separation to obtain aluminum-containing alkali liquor; m is an alkali metal element;
controlling the concentration of MOH in the aluminum-containing alkali liquor to be 5-30 g/L; the molar ratio of M to Al is 1-5;
step 2):
heating the aluminum-containing alkali liquor to 60-160 ℃, and blowing CO-containing solution into the aluminum-containing alkali liquor2When the pH of the solution is reduced to 9.8-11.0, stopping introducing CO2And after the reaction is finished, carrying out solid-liquid separation to obtain boehmite.
2. The process of claim 1 for preparing boehmite from a high-silicon aluminous material, wherein: the high-silicon aluminum-containing material comprises at least one of fly ash, coal gangue, red mud, bauxite, clay and tailings;
preferably, in the high-silicon aluminum-containing material, Al is2O310-50% of SiO2The content is 20-80%.
3. The process of claim 1 for preparing boehmite from a high-silicon aluminous material, wherein: in the slurry, CaO/SiO2The molar ratio is 0.5 to 1.0.
4. The process of claim 1 for preparing boehmite from a high-silicon aluminous material, wherein: in the step (1), the MOH added into the slurry is not lower than the theoretical reaction amount, and preferably, the concentration of the MOH in the slurry is 1-2 times of the concentration of the MOH at the reaction end point;
in the hydrothermal process, the liquid-solid ratio in the slurry is 5-20 mL/g;
preferably, the temperature of the hydrothermal reaction is 150-200 ℃;
preferably, the time of the hydrothermal reaction is 0.1-3 h.
5. The process of claim 1 for preparing boehmite from a high-silicon aluminous material, wherein: controlling the MOH concentration of the aluminum-containing alkali liquor to be 10-20 g/L; further preferably 10-15 g/L;
preferably, in the aluminum-containing alkali liquor, the molar ratio of M/Al is 1-3.5; more preferably 1 to 1.5.
6. A method for preparing boehmite from high-silicon aluminous material according to any one of claims 1-5, characterized by: in the step 2), the nucleation reaction is normal pressure nucleation reaction or hydrothermal nucleation reaction;
carrying out normal-pressure nucleation in open reaction equipment or pressure-resistant reaction equipment, wherein the temperature is lower than 100 ℃, preferably 85-95 ℃, and synthesizing to obtain spindle-type boehmite; the temperature is 60-70 ℃, and boehmite with a lamellar structure is obtained;
the hydrothermal nucleation reaction is carried out in a pressure-resistant reaction vessel, the temperature in the reaction process is 105-160 ℃, the preferable temperature is 120-150 ℃, and the fiber type boehmite is obtained by synthesis.
7. A method for preparing boehmite from a high-silicon aluminous material according to any one of claims 1-6, characterized by: controlling the pH value of the reaction end point to be 9.8-10.5; more preferably 9.8 to 10.
8. The process of claim 1 for preparing boehmite from a high-silicon aluminous material, wherein: said CO-containing2The gas of (2) is pure carbon dioxide gas, or a mixed gas of carbon dioxide and at least one of nitrogen, oxygen and inert gas; preferably, it contains CO2In the gas of (2), CO2The volume percentage of (A) is preferably 50-100%;
preferably, it contains CO2The flow rate of the gas (2) is 0.5L/min to 20L/min.
9. The process of claim 1 for preparing boehmite from a high-silicon aluminous material, wherein: the nucleation reaction time is 10-90 min; further preferably 30-70 min; more preferably 50 to 60 min.
10. The process of claim 1 for preparing boehmite from a high-silicon aluminous material, wherein: the synthesized boehmite is a porous material with sheet-shaped, spindle-shaped and fiber-shaped appearance.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113231010A (en) * 2021-06-03 2021-08-10 中南大学 Polytype zeolite/C-S-H composite adsorption material and preparation method and application thereof
CN115448342A (en) * 2022-08-26 2022-12-09 雅安百图高新材料股份有限公司 Boehmite powder and preparation method thereof
CN116081668A (en) * 2023-03-06 2023-05-09 成都超纯应用材料有限责任公司 Boehmite sol dispersing agent, preparation method and application thereof
CN116534886A (en) * 2023-04-27 2023-08-04 中国石油大学(华东) Method for carbon fixation and simultaneous production of dawsonite

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101633511A (en) * 2009-08-07 2010-01-27 淄博万霖化工科技有限公司 Hydrated alumina and preparation method thereof
CN101657384A (en) * 2007-03-27 2010-02-24 美铝澳大利亚有限公司 Method for precipitating boehmite
US20120051988A1 (en) * 2010-08-25 2012-03-01 Meena Marafi PROCESS FOR RECOVERING BOEHMITE AND y-Al2O3 FROM SPENT HYDROPROCESSING CATALYSTS
CN102476820A (en) * 2010-11-25 2012-05-30 中国科学院过程工程研究所 Method for extracting alumina from coal ash through wet process
CN106745016A (en) * 2016-11-24 2017-05-31 河北工程大学 A kind of method of separation and concentration lithium, aluminium, silicon from flyash

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101657384A (en) * 2007-03-27 2010-02-24 美铝澳大利亚有限公司 Method for precipitating boehmite
CN101633511A (en) * 2009-08-07 2010-01-27 淄博万霖化工科技有限公司 Hydrated alumina and preparation method thereof
US20120051988A1 (en) * 2010-08-25 2012-03-01 Meena Marafi PROCESS FOR RECOVERING BOEHMITE AND y-Al2O3 FROM SPENT HYDROPROCESSING CATALYSTS
CN102476820A (en) * 2010-11-25 2012-05-30 中国科学院过程工程研究所 Method for extracting alumina from coal ash through wet process
CN106745016A (en) * 2016-11-24 2017-05-31 河北工程大学 A kind of method of separation and concentration lithium, aluminium, silicon from flyash

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113231010A (en) * 2021-06-03 2021-08-10 中南大学 Polytype zeolite/C-S-H composite adsorption material and preparation method and application thereof
CN113231010B (en) * 2021-06-03 2022-07-29 中南大学 Multi-type zeolite/C-S-H composite adsorption material and preparation method and application thereof
CN115448342A (en) * 2022-08-26 2022-12-09 雅安百图高新材料股份有限公司 Boehmite powder and preparation method thereof
CN116081668A (en) * 2023-03-06 2023-05-09 成都超纯应用材料有限责任公司 Boehmite sol dispersing agent, preparation method and application thereof
CN116534886A (en) * 2023-04-27 2023-08-04 中国石油大学(华东) Method for carbon fixation and simultaneous production of dawsonite
CN116534886B (en) * 2023-04-27 2024-03-29 中国石油大学(华东) Method for carbon fixation and simultaneous production of dawsonite

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