CN110304644B - Method for producing high-purity high-viscosity pseudo-boehmite - Google Patents
Method for producing high-purity high-viscosity pseudo-boehmite Download PDFInfo
- Publication number
- CN110304644B CN110304644B CN201910586107.1A CN201910586107A CN110304644B CN 110304644 B CN110304644 B CN 110304644B CN 201910586107 A CN201910586107 A CN 201910586107A CN 110304644 B CN110304644 B CN 110304644B
- Authority
- CN
- China
- Prior art keywords
- purity
- boehmite
- pseudo
- sodium aluminate
- aluminate solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Catalysts (AREA)
Abstract
The invention provides a method for producing high-purity high-viscosity pseudo-boehmite, which comprises the following steps: the high-purity high-viscosity pseudo-boehmite is obtained by the reaction of a high-purity sodium aluminate solution and carbon dioxide gas and then is obtained by a method of deep sodium removal by hydrothermal high-temperature high-pressure aging treatment. The high-purity high-viscosity pseudo-boehmite produced by the method has the advantages of good crystal form, easily controlled large pores in specific surface area, high purity, low production cost and good product quality. The method meets the national requirement of environmental protection, improves the application of petroleum refining catalyst, reforming catalyst and catalyst for purifying production tail gas and automobile tail gas in a wider range, is widely applied to the field of catalysis, and fills up the technical blank in the aspect of domestic catalyst.
Description
Technical Field
The invention belongs to the technical field of preparation of pseudo-boehmite, and particularly relates to a method for producing high-purity high-viscosity pseudo-boehmite.
Background
Foreign high-purity pseudo-boehmite is produced by adopting an aluminum alkoxide method, namely high-purity aluminum reacts with isopropanol to generate aluminum isopropoxide, and then reacts with water to generate isopropanol and high-purity pseudo-boehmite through a hydrolysis reaction. Domestic carbonization method, i.e. using sodium aluminate solution and introducing CO2The gas is carbonated and decomposed to generate pseudo-boehmite slurry, and the pseudo-boehmite is filtered and washed to obtain the common pseudo-boehmite.
With the increase of national environmental protection, the dosage of petroleum refining (desulfurization, denitrification and alkylation) catalysts, reforming catalysts, production tail gas and automobile tail gas purification catalysts is increased sharply, and the catalysts adopt high-purity pseudo-boehmite as a binder or a carrier. In the current-stage industrial production, the purity of the sodium aluminate solution and the purity of the washing water can meet the production of common pseudo-boehmite, but the performance of the common pseudo-boehmite can not meet the requirements of some high-quality catalysts due to higher impurity content, lower caking property, lower crystallinity and the like.
At present, the pseudo-boehmite is mainly produced by an aluminum alkoxide hydrolysis method of Sasol company. The product SB powder of the company has good crystal form, easily controlled pore structure, large specific surface area and high purity, and is widely applied to the field of catalysis, but the organic solvent used by the method has certain toxicity and higher import cost, and is not easy to widely popularize.
Disclosure of Invention
In view of the above, the invention provides a method for producing high-purity high-viscosity pseudo-boehmite, which comprises the steps of preparing high-purity pseudo-boehmite by reacting a high-purity sodium aluminate solution with carbon dioxide gas, and deeply removing sodium by hydrothermal high-temperature high-pressure aging treatment to obtain the high-purity high-viscosity pseudo-boehmite.
In a first aspect of the present invention, there is provided a process for producing a high-purity high-viscosity pseudoboehmite, comprising the steps of:
s1, preparing a high-purity sodium aluminate solution: pre-decomposing the sodium aluminate solution, controlling the aluminum oxide loss to be 5-10%, and filtering to obtain a high-purity sodium aluminate solution;
s2, preparing high-purity pseudo-boehmite: diluting high-purity sodium aluminate solution and mixing with CO2Reacting to obtain high-purity pseudo-boehmite slurry; filtering and washing the high-purity pseudo-boehmite slurry to obtain a high-purity pseudo-boehmite wet filter cake;
s3, preparing high-purity high-viscosity pseudo-boehmite: adding water into the high-purity pseudo-boehmite wet filter cake, stirring and slurrying, adding a high-carbon alcohol additive, carrying out heat preservation reaction at the temperature of 100-200 ℃ and under the pressure of 0.5-1MPa for 2-24h, cooling and discharging after the reaction is finished, filtering, washing and drying to obtain the high-purity high-viscosity pseudo-boehmite.
The high-purity sodium aluminate solution obtained by pre-decomposing and purifying the sodium aluminate solution is subjected to subsequent reaction, so that the possibility of impurity generation is solved from a production source, the product quality is more stable, and the application range is wider. Further, the high-purity sodium aluminate solution is reacted with carbon dioxide gas to prepare the high-purity pseudo-boehmite. Further, the high-purity high-viscosity pseudo-boehmite is obtained by adding an additive to act on the high-purity pseudo-boehmite, carrying out polycondensation reaction at high temperature and high pressure, and deeply removing sodium.
Preferably, in step S1, the method for preparing sodium aluminate solution includes: reacting aluminum hydroxide with alkali liquor at the temperature of 105-120 ℃ for 2-4h to obtain sodium aluminate solution. The Na in the high-purity sodium aluminate solution is obtained by pre-decomposition and purification of the sodium aluminate solution prepared by the method2O≤100ppm，Fe2O3≤20ppm，SiO2Less than or equal to 50ppm, and the impurity content basically reaches the standard.
The method continuously utilizes the reaction of the high-purity sodium aluminate solution and carbon dioxide gas to prepare the high-purity pseudo-boehmite, the carbonation decomposition of the sodium aluminate solution is a complex multiphase reaction involving three phases of gas, liquid and solid, the method comprises the processes of absorption of the carbon dioxide for the sodium aluminate solution, chemical reaction between the sodium aluminate solution and the carbon dioxide, precipitation of the pseudo-boehmite and the like, the precipitation of silicon dioxide is accompanied in the carbonation process, particularly in the later stage, and dawsonite compounds are generated, so that the possibility of generating impurities in the high-purity sodium aluminate solution with basically up to standard impurity content is solved from a production source, and the generation of the impurities in the subsequent reaction can be avoided. In the whole process of the invention, new impurities are not introduced as far as possible, so that the finally obtained high-purity high-viscosity pseudo-boehmite has extremely low impurity content.
In the step S2 of preparing high purity pseudoboehmite, the final form of the carbonation decomposition reaction of the sodium aluminate solution is aluminum hydroxide, and the pseudoboehmite is only an intermediate transition state, so the present invention requires a relatively strict control of the process conditions.
Preferably, the high purity sodium aluminate solution diluted in step S2 is mixed with CO2Carrying out a reaction under conditions comprising: the initial reaction temperature is 20-30 ℃, and CO is introduced2Controlling CO concentration at 30-50%2The flow rate of (A) is 1.0-5.0m3H, the reaction time is 30-80 minutes, and the final reaction temperature is 25-50 ℃.
More preferably, in step S2, the diluted high purity sodium aluminate solution is controlled to be mixed with CO2Al in the reaction product of (1)2O33-9g/L of residue remained.
More preferably, in step S2, the high purity sodium aluminate solution is diluted to Al2O3The content is 40-60 g/L.
Preferably, in step S2, the washing is performed by washing with high-purity water at 80-100 ℃ until the pH of the wet cake is 7.0-7.5.
In the step S3 of preparing the high-purity high-viscosity pseudo-boehmite, the subsequent hydrothermal polycondensation reaction at high temperature and high pressure must be performed using the wet cake, and the dried sample cannot be used. The high-purity high-viscosity pseudo-boehmite can lose the high-purity high-viscosity pseudo-boehmite by using a dry product reactionHigh adhesion. The high-temperature high-pressure polycondensation reaction mainly utilizes the added auxiliary agent to carry out polymerization recrystallization on the pseudoboehmite, two dissociated water molecules generate a binuclear double-bridge type complex, and then the complex loses two H groups+The water molecule in the dioxy double-bridge complex is separated into OH group and H2The O molecule forms a double-bridge complex, and further forms a tetra-oxo bridge polynuclear complex (the structure is shown as follows):
preferably, the O-O groups are alternately arranged to further form a reticular or locked polynuclear complex, and the obtained high-purity high-viscosity pseudo-boehmite has the following reticular or locked polynuclear complex structure:
the structure enables the high-purity high-viscosity pseudo-boehmite to have higher and more stable cohesiveness, the main peak value of the pseudo-boehmite in the XRD diffraction pattern of the pseudo-boehmite is sharper, the peak height is higher, the peak width is narrowed, the alumina content is increased, the water molecule content is reduced, the grain size is increased, the crystallinity is higher, the pore size distribution is more uniform, the formed form is more perfect, and the practicability is wider.
Preferably, in step S3, the added mass of the higher alcohol additive is 0.5-2% of the mass of the high-purity pseudo-boehmite wet cake.
More preferably, in step S3, the higher alcohol additive is urea or choline.
The second aspect of the invention provides the high-purity high-viscosity pseudo-boehmite prepared by the method.
Compared with the prior art, the invention has the following advantages:
(1) the invention utilizes the reaction of high-purity sodium aluminate solution and carbon dioxide gas to prepare high-purity pseudoboehmite, and then the high-temperature reaction is carried outHigh-pressure hydrothermal treatment is carried out to obtain the high-purity high-viscosity pseudo-boehmite with high purity and SiO2、Fe2O3、Na2Low content of impurities such as O and the like, good crystal form, large and controllable specific surface area and pore volume, and good product quality.
(2) The high-purity high-viscosity pseudo-boehmite obtained by the invention has a net-shaped or lock-shaped multi-core complex structure, has higher and more stable cohesiveness, larger crystal grain size, higher crystallinity, more uniform pore size distribution and more complete formed form, realizes the technical innovation and structure adjustment of the pseudo-boehmite, expands the application field of the pseudo-boehmite, improves the application of petroleum refining catalysts, reforming catalysts and catalysts for producing tail gas and purifying automobile tail gas in a wider range, is widely applied to the catalysis field, and fills the technical blank in the aspect of domestic catalysts.
(3) The process for preparing the high-purity high-viscosity pseudo-boehmite is simple and controllable, does not need to adopt toxic solvents, meets the national requirement on environmental protection, has low production cost, and has good industrial popularization and application prospects.
Drawings
FIG. 1 is a process flow diagram of a method for producing high-purity high-viscosity pseudo-boehmite according to the present invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If there is a conflict, the present specification will control.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
The invention provides a method for producing high-purity high-viscosity pseudo-boehmite, which comprises the following steps:
s1, preparation of high-purity sodium aluminate solution:
firstly, selecting an aluminum hydroxide raw material, adding 30% of alkali liquor containing sodium hydroxide into a stainless steel reaction tank, specifically, adding 4L of alkali liquor into each kilogram of aluminum hydroxide, placing the aluminum hydroxide raw material on an electric hot plate for heating, controlling the temperature of the reaction tank between 105 ℃ and 120 ℃, and controlling the reaction time between 2 hours and 4 hours to obtain a sodium aluminate solution.
Secondly, adding the sodium aluminate solution into a decomposition tank for pre-decomposition and purification, and controlling Al2O3Loss is within 5-10%, filtering to obtain high-purity sodium aluminate solution, diluting and blending with high-purity water, and controlling the concentration of the sodium aluminate solution: with Al2O3The content is 40-60 g/l.
S2, preparing high-purity pseudo-boehmite:
using high-purity sodium aluminate solution as raw material, introducing CO2Gas is gelatinized and decomposed, the initial temperature of the high-purity sodium aluminate solution is controlled at 20-30 ℃, and CO with the concentration of 30-50 percent is introduced2Gas, the flow rate per hour is controlled to be 1.0-5.0m3Reaction time is controlled to be 30-80 minutes, and Al is controlled2O33-9g/l of residue is remained, the final temperature is controlled to be 25-50 ℃, after the decomposition is finished, the pseudo-boehmite filter cake is separated and washed, and then the pseudo-boehmite filter cake is washed by high-purity water with the temperature of 80-100 ℃ until the pH value of the filter cake is 7.0-7.5, and the high-purity pseudo-boehmite wet filter cake is obtained.
S3, preparing high-purity high-viscosity pseudo-boehmite:
adding high-purity water with the temperature of 80-100 ℃ into the prepared high-purity pseudo-boehmite filter cake, stirring and pulping at a high speed, adding the high-purity water for dilution and stirring after the slurry is uniform, and adding a high-carbon alcohol additive in the process. Specifically, 1L of high-purity water is correspondingly added into each 2kg of filter cake, then the high-speed stirring is carried out, and then 3L of high-purity water is added for dilution, wherein the addition amount of the high-alcohol additive is 10-40 g.
Stirring for 30-60min, transferring the slurry into 5-10L high-pressure autoclave equipment, performing high-temperature high-pressure treatment at 110-200 ℃, the pressure of 0.5-1MPa, keeping the temperature for 2-24h to control the reaction, cooling, discharging, filtering, washing and drying after the reaction is finished, controlling the pH value of a filter cake to be 7.0-7.5 according to the water consumption during washing, drying at 100-200 ℃ to control the water content of the product to be 10-20%, and crushing to obtain the final product, namely the high-purity high-viscosity pseudo-boehmite. The whole process flow process does not bring new impurities as much as possible.
The following will explain a method for producing high-purity high-viscosity pseudo-boehmite according to the present invention with reference to specific 3 examples.
Example 1
The embodiment provides a method for producing high-purity high-viscosity pseudo-boehmite, which comprises the following steps:
preparing high-purity sodium aluminate solution. Firstly, 1Kg of aluminum hydroxide raw material and 4L of 30% sodium hydroxide-containing alkali liquor (model number is 50SP) are selected and added into a 5L stainless steel reaction tank, the stainless steel reaction tank is placed on an electric hot plate for heating, the temperature of the reaction tank is controlled at 110 ℃, and the reaction time is controlled at 3 hours, so that the sodium aluminate solution is obtained. Secondly, adding the sodium aluminate solution into a decomposition tank for pre-decomposition and purification, and controlling Al2O3The loss is 7%, filtering to obtain high-purity sodium aluminate solution, diluting and blending with high-purity water, and controlling the concentration of the sodium aluminate solution: with Al2O3The content is 45 g/L.
Preparing high-purity pseudo-boehmite: using 10L of high-purity sodium aluminate solution as raw material, introducing CO2Gas is gelatinized and decomposed, the initial temperature of the high-purity sodium aluminate solution is controlled at 25 ℃, and CO with the concentration of 40 percent is introduced2Gas, the flow rate per hour is controlled to be 3.0m3Reaction time is controlled to be 40 minutes, and Al is controlled2O35g/l of residual water is kept, the final temperature is controlled at 35 ℃, after the decomposition is finished, the separation and washing are carried out, and then the pseudo-boehmite filter cake is washed by high-purity water with the temperature of 85 ℃ until the pH value of the filter cake is 7.0, so that the high-purity pseudo-boehmite wet filter cake is obtained.
Preparing high-purity high-viscosity pseudo-boehmite: using 5L of reaction tank to melt slurry, adding 1L of high-purity water at 90 ℃ into 2Kg of the prepared high-purity pseudo-boehmite filter cake, stirring the slurry at a high speed, adding 3L of high-purity water to dilute and stir the slurry uniformly, adding a high-carbon alcohol additive to ensure that the concentration of the additive is 8g/L in the process, stirring the high-carbon alcohol additive to 50min, transferring the slurry into high-pressure kettle equipment, carrying out high-temperature and high-pressure treatment, controlling the kettle temperature to be 160 ℃, the pressure to be 0.6MPa, keeping the temperature for 4h for reaction, cooling, discharging, filtering and washing the slurry, controlling the pH value of the filter cake to be 7.0 when the water consumption is used for washing, drying the filter cake at 100 ℃ to control the water content of the product to be 15%, and crushing the product to obtain the final product of the high-purity and high-viscosity pseudo-boehmite. The whole process flow process does not bring new impurities as much as possible. The high-purity high-viscosity pseudo-boehmite prepared by the embodiment has the following reticular multi-core complex structure:
the high-purity high-viscosity pseudo-boehmite prepared in the example was subjected to a performance test, and for comparison, the SB powder of Sasol company was subjected to a performance test under the same conditions, and the test results are shown in table 1.
TABLE 1 comparison table of SB powder testing indexes of sample and Sasol company in this example
Example 2
The embodiment provides a method for producing high-purity high-viscosity pseudo-boehmite, which comprises the following steps:
preparing high-purity sodium aluminate solution. 1Kg of aluminum hydroxide raw material and 4L of 30% sodium hydroxide-containing alkali liquor (model number is 50SP) are added into a 5L stainless steel reaction tank, the stainless steel reaction tank is placed on an electric hot plate for heating, the temperature of the reaction tank is controlled at 115 ℃, and the reaction time is controlled at 2 hours, so that the sodium aluminate solution is obtained. Adding sodium aluminate solution into a decomposition tank for pre-decomposition and purification, and controlling Al2O3Loss is 7%, filtering to obtain high-purity sodium aluminate solution, diluting with high-purity water, and controllingConcentration of sodium aluminate solution: with Al2O3The content is 55 g/L.
Preparing high-purity pseudo-boehmite: using 10L of high-purity sodium aluminate solution as raw material, introducing CO2Gas is gelatinized and decomposed, the initial temperature of the high-purity sodium aluminate solution is controlled at 28 ℃, and CO with the concentration of 35 percent is introduced2Gas, the flow rate per hour is controlled to be 2.0m3Reaction time is controlled to be 60 minutes, and Al is controlled2O37g/l of residual water is kept, the final temperature is controlled at 40 ℃, after the decomposition is finished, the pseudo-boehmite filter cake is separated and washed, and then the pseudo-boehmite filter cake is washed by high-purity water with the temperature of 90 ℃ until the pH value of the filter cake is 7.5, and the high-purity pseudo-boehmite wet filter cake is obtained.
Preparing high-purity high-viscosity pseudo-boehmite: using 5L of reaction tank to melt slurry, adding 1L of high-purity water at 90 ℃ into 2Kg of the prepared high-purity pseudo-boehmite filter cake, stirring the slurry at a high speed, adding 3L of high-purity water to dilute and stir the slurry uniformly, adding a high-carbon alcohol additive to ensure that the concentration of the additive is 8g/L in the process, stirring the high-carbon alcohol additive to 50min, transferring the slurry into high-pressure kettle equipment, carrying out high-temperature and high-pressure treatment, controlling the kettle temperature to be 120 ℃, the pressure to be 0.8MPa, keeping the temperature for 20h for reaction, cooling, discharging, filtering and washing the reaction product after the reaction is finished, controlling the pH value of the filter cake to be 7.5, drying the product at 150 ℃ to control the water content of the product to be 12%, and crushing the product to obtain the final product of high-purity and high-viscosity pseudo-boehmite. The whole process flow process does not bring new impurities as much as possible. The structure and performance of the high-purity high-viscosity pseudo-boehmite prepared by the embodiment are basically consistent with those of the embodiment 1.
TABLE 2 comparison table of SB powder testing indexes of sample and Sasol company in this example
Example 3
The embodiment provides a method for producing high-purity high-viscosity pseudo-boehmite, which comprises the following steps:
preparing high-purity sodium aluminate solution. Firstly, selecting aluminium hydroxide1Kg of raw material and 4L of 30% sodium hydroxide-containing lye (model number 50SP) were added to a 5L stainless steel reaction tank, which was placed on an electric hot plate for heating, the temperature of the reaction tank was controlled at 115 ℃ and the reaction time was controlled at 2 hours, to obtain sodium aluminate solution. Secondly, adding the sodium aluminate solution into a decomposition tank for pre-decomposition and purification, and controlling Al2O3The loss is 10%, filtering to obtain high-purity sodium aluminate solution, diluting and blending with high-purity water, and controlling the concentration of the sodium aluminate solution: with Al2O3The content is 50 g/L.
Preparing high-purity pseudo-boehmite: using 10L of high-purity sodium aluminate solution as raw material, introducing CO2Gas is gelatinized and decomposed, the initial temperature of the high-purity sodium aluminate solution is controlled at 30 ℃, and CO with the concentration of 35 percent is introduced2Gas, the flow rate per hour is controlled to be 4.5m3Reaction time is controlled to be 50 minutes, and Al is controlled2O39g/l of residual water is kept, the final temperature is controlled at 45 ℃, after the decomposition is finished, the pseudo-boehmite filter cake is separated and washed, and then the pseudo-boehmite filter cake is washed by high-purity water with the temperature of 90 ℃ until the pH value of the filter cake is 7.0, and the high-purity pseudo-boehmite wet filter cake is obtained.
Preparing high-purity high-viscosity pseudo-boehmite: using 5L of reaction tank to melt slurry, adding 1L of high-purity water at 90 ℃ into 2Kg of the prepared high-purity pseudo-boehmite filter cake, stirring the slurry at a high speed, adding 3L of high-purity water to dilute and stir the slurry uniformly, adding a high-carbon alcohol additive to ensure that the concentration of the additive is 8g/L in the process, stirring the high-carbon alcohol additive to be urea for 50min, transferring the slurry into high-pressure kettle equipment, carrying out high-temperature and high-pressure treatment, controlling the kettle temperature to be 120 ℃, the pressure to be 1MPa, keeping the temperature for 18h for reaction, cooling, discharging, filtering and washing the slurry after the reaction is finished, controlling the pH value of the filter cake to be 7.0 when the water consumption is used for washing, drying the product at 100 ℃ to control the water content to be 20%, and crushing the product to obtain the final product of the high-purity and high-viscosity pseudo-boehmite. The whole process flow process does not bring new impurities as much as possible. The structure and performance of the high-purity high-viscosity pseudo-boehmite prepared by the embodiment are basically consistent with those of the embodiment 1.
TABLE 3 comparison table of SB powder testing indexes of sample and Sasol company in this example
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (4)
1. A method for producing a high purity, high viscosity pseudo-boehmite, the method comprising:
s1, preparing a high-purity sodium aluminate solution: pre-decomposing the sodium aluminate solution, controlling the aluminum oxide loss to be 5-10%, and filtering to obtain a high-purity sodium aluminate solution;
s2, preparing high-purity pseudo-boehmite: diluting high-purity sodium aluminate solution and mixing with CO2Reacting to obtain high-purity pseudo-boehmite slurry; filtering and washing the high-purity pseudo-boehmite slurry to obtain a high-purity pseudo-boehmite wet filter cake, diluting the high-purity sodium aluminate solution and then mixing with CO2The reaction conditions include: the initial reaction temperature is 20-30 ℃, and CO is introduced2Controlling CO concentration at 30-50%2The flow rate of (A) is 1.0-5.0m3The reaction time is 30-80 minutes, the final reaction temperature is 25-50 ℃, and the diluted high-purity sodium aluminate solution is mixed with CO2Al in the reaction product2O33-9g/L of residues are left, and the washing is carried out by adopting high-purity water at 80-100 ℃ until the pH value of a wet filter cake is 7.0-7.5;
s3, preparing high-purity high-viscosity pseudo-boehmite: adding water into the high-purity pseudo-boehmite wet filter cake, stirring and pulping, adding a high-carbon alcohol additive, carrying out heat preservation reaction for 2-24h at the temperature of 100-200 ℃ and under the pressure of 0.5-1MPa, cooling and discharging after the reaction is finished, filtering, washing and drying to obtain the high-purity high-viscosity pseudo-boehmite, wherein the adding mass of the high-carbon alcohol additive is 0.5-2% of the mass of the high-purity pseudo-boehmite wet filter cake, the high-purity high-viscosity pseudo-boehmite is a net-shaped or lock-shaped polynuclear complex, the high-carbon alcohol additive is choline, and the high-purity high-viscosity pseudo-boehmite has the following structure:
2. the process for producing high purity highly viscous pseudo-boehmite according to claim 1, characterized by: in step S1, the method for preparing sodium aluminate solution includes: reacting aluminum hydroxide with alkali liquor at the temperature of 105-120 ℃ for 2-4h to obtain sodium aluminate solution.
3. The process for producing highly pure highly viscous pseudo-boehmite according to claim 1 or 2, characterized by: in step S2, the high purity sodium aluminate solution is diluted to Al2O3The content is 40-60 g/L.
4. Highly pure highly viscous pseudo-boehmite prepared by the method according to any one of claims 1 to 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910586107.1A CN110304644B (en) | 2019-07-01 | 2019-07-01 | Method for producing high-purity high-viscosity pseudo-boehmite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910586107.1A CN110304644B (en) | 2019-07-01 | 2019-07-01 | Method for producing high-purity high-viscosity pseudo-boehmite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110304644A CN110304644A (en) | 2019-10-08 |
| CN110304644B true CN110304644B (en) | 2022-03-25 |
Family
ID=68078144
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910586107.1A Active CN110304644B (en) | 2019-07-01 | 2019-07-01 | Method for producing high-purity high-viscosity pseudo-boehmite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110304644B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115974113A (en) * | 2022-12-23 | 2023-04-18 | 中科催化新技术(大连)股份有限公司 | Method for synthesizing high-peptization pseudo-boehmite by taking carbon dioxide as raw material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001073143A1 (en) * | 2000-03-28 | 2001-10-04 | Alcoa Of Australia Limited | Agglomeration of alumina and binder therefor |
| CN1752005A (en) * | 2005-10-25 | 2006-03-29 | 湘潭大学 | Preparation method of ultrafine active aluminium oxide |
| CN1843924A (en) * | 2006-04-17 | 2006-10-11 | 厦门大学 | Method for preparing unformed aluminium hydroxide |
| CN103787394A (en) * | 2012-11-01 | 2014-05-14 | 中国石油化工股份有限公司 | Preparation method of alumina carrier |
-
2019
- 2019-07-01 CN CN201910586107.1A patent/CN110304644B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001073143A1 (en) * | 2000-03-28 | 2001-10-04 | Alcoa Of Australia Limited | Agglomeration of alumina and binder therefor |
| CN1752005A (en) * | 2005-10-25 | 2006-03-29 | 湘潭大学 | Preparation method of ultrafine active aluminium oxide |
| CN1843924A (en) * | 2006-04-17 | 2006-10-11 | 厦门大学 | Method for preparing unformed aluminium hydroxide |
| CN103787394A (en) * | 2012-11-01 | 2014-05-14 | 中国石油化工股份有限公司 | Preparation method of alumina carrier |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110304644A (en) | 2019-10-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| RU2463108C2 (en) | Amorphous aluminium silicate composition, its production and application | |
| CN110127736B (en) | Preparation method of high-viscosity macroporous pseudo-boehmite | |
| CN102161004B (en) | Hydrotreating catalyst and application thereof | |
| CN102092749A (en) | Preparation method of boehmite | |
| WO2001026805A1 (en) | Catalyst for hydrorefining distillate oil, its carrier and preparation thereof | |
| CN110304644B (en) | Method for producing high-purity high-viscosity pseudo-boehmite | |
| CN104588076B (en) | Hydrocracking catalyst and preparation method thereof | |
| CN104588074B (en) | A kind of preparation method of catalytic hydro-dearomatization catalyst | |
| CN104588078B (en) | Hydrocracking catalyst and preparation method thereof | |
| CN111410206A (en) | Preparation method of Y-type molecular sieve with high silica-alumina ratio | |
| CN115124056B (en) | Pseudo-boehmite and preparation method and application thereof | |
| CN115920961A (en) | Preparation method of silicon-containing pseudo-boehmite slurry | |
| CN104826653B (en) | A kind of method for preparing hydrocracking catalyst | |
| CN104588077B (en) | The preparation method of hydrocracking catalyst | |
| CN104826651B (en) | The preparation method of hydrocracking catalyst | |
| CN116060108A (en) | Diesel oil hydro-upgrading catalyst and preparation method and application thereof | |
| CN102160996B (en) | Composition of boehmite and silicon-containing compound and silicon oxide-alumina prepared from same | |
| CN114506866B (en) | Preparation method for continuously preparing silicon-containing pseudo-boehmite | |
| CN114314607A (en) | MCM-22 molecular sieve, preparation method thereof and benzene alkylation reaction method adopting molecular sieve catalysis | |
| CN114713271B (en) | Modified Y molecular sieve and preparation method thereof | |
| CN111086998B (en) | Preparation method of high-crystallinity Y-type molecular sieve containing mesopores | |
| CN114920260B (en) | Preparation method of nano H-Beta molecular sieve | |
| CN115180642B (en) | Method for improving pore volume and pore diameter of pseudo-boehmite | |
| CN116059987B (en) | Preparation method of amorphous silicon aluminum | |
| CN112744845B (en) | Pseudo-boehmite, preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |