CN116002733A - Pseudo-boehmite with adjustable grain size and preparation method and application thereof - Google Patents

Pseudo-boehmite with adjustable grain size and preparation method and application thereof Download PDF

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CN116002733A
CN116002733A CN202111216663.3A CN202111216663A CN116002733A CN 116002733 A CN116002733 A CN 116002733A CN 202111216663 A CN202111216663 A CN 202111216663A CN 116002733 A CN116002733 A CN 116002733A
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boehmite
pseudo
aging
washing
grain size
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刘雨晴
袁帅
于善青
刘博�
邱中红
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Abstract

A method of preparing grain size adjustable pseudo-boehmite comprising: (1) Neutralizing the sodium metaaluminate solution with carbon dioxide gas to form gel; (2) The slurry after the gel formation is subjected to sectional temperature raising and aging in a closed container; (3) Filtering the aged slurry and washing with deionized water; and (4) drying the filter cake obtained after washing. The pseudo-boehmite prepared by the method has: crystallinity not less than 90%, adjustable grain size of 5-12 nm, 100-300 m 2 Specific surface area per gram and pore volume of 0.4-1.0 mL/g. The method is prepared by adopting a carbonization method with environmental protection and low cost, does not need any auxiliary agent, and has simple process. By controlling proper pH value of gel forming and sectional temperature raising and aging conditionsThe pseudo-boehmite has good colloid solubility, pure crystalline phase and less impurities, and can be widely applied to the petrochemical industry field, in particular to the preparation of catalysts.

Description

Pseudo-boehmite with adjustable grain size and preparation method and application thereof
Technical Field
The invention relates to a preparation method of pseudo-boehmite, in particular to a method for preparing pseudo-boehmite with adjustable grain size and high crystallinity by using a carbonization method, the pseudo-boehmite obtained by the method and application thereof.
Background
The chemical formula of the pseudo-boehmite is AlOOH.nH 2 O(0<n<1) Is an aluminum oxide compound with water content greater than boehmite and grain size smaller than boehmite. It is a crystalline phase which is easy to generate in the process of synthesizing aluminum hydroxide, the crystallization is incomplete, and the typical crystal form is very thin wrinkled lamellar crystal. It is widely used in petroleum refining processes, is often used as a binder for catalytic cracking catalysts, and hydrogenation catalyst supports (gamma-Al 2 O 3 ) Is a precursor of (a). The preparation method of pseudo-boehmite mainly comprises an aluminum alkoxide hydrolysis method, a precipitation method and the like, and the precipitation method is divided into an acid method and an alkali method.
The aluminum alkoxide hydrolysis method takes aluminum metal and higher alcohols (n-amyl alcohol, n-hexyl alcohol and isopropyl alcohol) as raw materials, aluminum alkoxide is formed by reacting the aluminum metal with the alcohols in the presence of a catalyst, and then the aluminum alkoxide is hydrolyzed to obtain pseudo-boehmite. The aluminum alkoxide hydrolysis method can prepare pseudo-boehmite with high purity and high crystallinity, but the method has high production cost and complex production process. The alkali precipitation method is a method for preparing pseudo-boehmite by utilizing alkali to neutralize and precipitate acidic aluminum salt, and the common aluminum salt comprises Al 2 (SO 4 ) 3 ,Al(NO 3 ) 3 ,AlCl 3 And the like, and common alkali precipitants are NaOH and NH 3 ·H 2 O,NaAlO 2 ,Na 2 CO 3 Etc. Wherein, naAlO which takes intermediate product alkali sodium aluminate solution of aluminum factory as precipitant is widely used 2 -Al 2 (SO 4 ) 3 The process is also called double aluminium process, its raw material NaAlO 2 , Al 2 (SO 4 ) 3 Can provide an aluminum source, has high reaction efficiency and relatively lower production cost, and is a technical route mainly adopted by the production of refining catalysts, especially pseudo-boehmite for hydrogenation catalysts in China at present. The acid precipitation method is a method for preparing pseudo-boehmite by neutralizing and precipitating alkaline aluminate, which is typically sodium aluminate, with acid which may be strong acid (HNO) 3 ,H 2 SO 4 Etc.) may be a weak acid (NH 4 HCO 3 , NaHCO 3 Etc.) and CO 2 Etc. Wherein NaAlO 2 -CO 2 The method is also called carbonization method, the carbonization method can be used for producing alumina by sintering method, and intermediate product NaAlO is utilized 2 Solution and aluminium plant exhaust gas CO 2 As a reaction raw material, the process is simple, byproducts, waste liquid and the like in the production process can be returned to the production flow of the alumina for recycling, and the method is the method with the lowest cost for industrially producing the pseudo-boehmite at present. And, the method and the CO 2 The gathering and utilizing theme is fit and meets the time requirement of green development. However, the pseudo-boehmite prepared by the carbonization method is easy to generate a triple-water mixed crystal and has low crystallinity. However, the particle size, morphology and crystallinity of the pseudo-boehmite have important influence on the bonding property of the hydrogenation catalyst carrier and the catalytic cracking agent, and are main indexes for measuring the quality of the pseudo-boehmite.
CN110304644a discloses a method for producing high-purity high-viscosity pseudo-boehmite by carbonization. The high-purity pseudo-boehmite is obtained by pre-decomposing and purifying sodium aluminate solution to obtain high-purity sodium aluminate solution and then reacting with carbon dioxide gas. And further introducing high-carbon alcohol additive (urea or choline) in the preparation process, and performing high-temperature high-pressure polycondensation reaction to obtain pseudo-boehmite with crystallinity of 80-90%, grain size of 5-6 nm, good viscosity and high purity.
CN105645446a discloses an aging method for preparing pseudo-boehmite by carbonization method. After the pseudo-boehmite is glued, the solid-liquid separation is rapidly carried out, and the obtained filter cake is aged for 2-4 hours at 70-100 ℃. The crystallinity of the prepared pseudo-boehmite is 70-80%, the impurities are few, and the peptization index is good.
The crystallinity of the pseudo-boehmite product prepared by the existing method needs to be improved, and the attention to the grain size of the pseudo-boehmite is lacking. In fact, the grain size changes the way primary particles are stacked, thereby having an important effect on the pore structure of pseudo-boehmite and subsequent alumina.
Disclosure of Invention
Aiming at the defects of the prior art, the inventor discovers that the pseudo-boehmite with good colloid solubility, pure crystalline phase, less impurities and adjustable grain size can be prepared by controlling the proper colloid forming pH value and the sectional temperature-raising aging condition through a large number of experiments.
Accordingly, in one aspect, the present invention provides a method for preparing a grain size-adjustable pseudo-boehmite comprising the steps of:
(1) Neutralizing the sodium metaaluminate solution with carbon dioxide gas to form gel;
(2) The slurry after the gel formation is subjected to sectional temperature raising and aging in a closed container;
(3) Filtering the aged slurry and washing with deionized water; a kind of electronic device with high-pressure air-conditioning system
(4) And drying the filter cake obtained after washing to obtain the pseudo-boehmite with adjustable grain size.
In one embodiment of the process according to the invention, the sodium metaaluminate solution in step (1) has a concentration of 10 to 80gAl 2 O 3 Preferably 15 to 60g Al 2 O 3 L; the volume concentration of the carbon dioxide gas is 15-50%, preferably 25-50%; the glue forming temperature is lower than 50 ℃; the final pH value of the gel is 9-11.
In another embodiment of the method according to the present invention, the step (2) of staged heat aging comprises: firstly, programming to 50-100 ℃ and aging for 30-120 min, preferably programming to 60-80 ℃ and aging for 40-80 min; and then the temperature is programmed to 100-220 ℃ for aging for 1-10 h, preferably 120-180 ℃ for aging for 2-6 h.
In another embodiment of the method according to the present invention, step (3) may be an intermittent washing in which the filter cake obtained by filtering the aged slurry is slurried with deionized water and filtered, and then the thus obtained filter cake is slurried with deionized water and filtered; or continuously washing the filter cake obtained by filtering the aged slurry with deionized water; continuous washing is preferably employed.
In another embodiment of the method according to the invention, the deionized water has a temperature of 60 to 90 ℃, preferably 80 to 90 ℃.
In another embodiment of the method according to the invention, the intermittent washing may be performed 1 to 4 times.
In another embodiment of the process according to the invention, the drying described in step (4) is carried out at a temperature of 60 to 120 ℃, preferably at a temperature of 70 to 100 ℃ for 2 to 4 hours.
In another aspect, the present invention provides a pseudo-boehmite prepared according to the method of the previous embodiment, the pseudo-boehmite having: crystallinity not less than 90%, grain size of 5-12 nm, 100-300 m 2 Specific surface area per gram and pore volume of 0.4-1.0 mL/g.
In one embodiment of the pseudo-boehmite according to the invention, the pseudo-boehmite has: crystallinity of 90-97%, grain size of 5-10 nm, 120-250 m 2 Specific surface area per gram and pore volume of 0.5-0.8 mL/g.
In a further aspect, the present invention provides the use of the aforementioned pseudo-boehmite in the preparation of a catalyst.
The method for preparing pseudo-boehmite is prepared by a carbonization method which is environment-friendly and low in cost, does not need any auxiliary agent, and is simple in process. The pseudo-boehmite has good solubility, pure crystalline phase and less impurities by controlling the proper pH value of the gel and the sectional temperature-raising aging conditions, and can be widely applied to the petrochemical industry field, in particular to the preparation of the catalyst.
Compared with the prior art, the invention breaks through the limitation that the high-quality pseudo-boehmite is difficult to prepare by the carbonization method in the traditional sense, shows great economic benefit, and can be widely applied to the petrochemical industry field, in particular to the binder, the hydrogenation catalyst carrier and the reforming catalyst carrier used as the catalytic cracking catalyst.
Drawings
The foregoing and other features and advantages of the present application will become more apparent from the following detailed description of the present application when taken in conjunction with the accompanying drawings in which:
FIG. 1 is an XRD spectrum of pseudo-boehmite;
Detailed Description
The following examples are provided to further illustrate the invention and are intended to aid the reader in better understanding the benefits that the essence of the invention resides in and is brought about, but should not be construed as limiting the scope of the invention in any way.
The method for preparing the pseudo-boehmite with adjustable grain size comprises the following steps of:
(1) Neutralizing the sodium metaaluminate solution with carbon dioxide gas to form gel;
(2) The slurry after the gel formation is subjected to sectional temperature raising and aging in a closed container;
(3) Filtering the aged slurry and washing with deionized water; a kind of electronic device with high-pressure air-conditioning system
(4) And drying the filter cake obtained after washing to obtain the pseudo-boehmite with adjustable grain size.
In one embodiment of the process according to the invention, the sodium metaaluminate solution in step (1) has a concentration of 10 to 80gAl 2 O 3 Preferably 15 to 60g Al 2 O 3 L; the volume concentration of the carbon dioxide gas is 15-50%, preferably 25-50%; the glue forming temperature is lower than 50 ℃; the final pH value of the gel is 9-11.
In the present application, the volume concentration of the carbon dioxide gas refers to the volume ratio of carbon dioxide to nitrogen; the gel forming temperature refers to the neutralization reaction temperature of sodium metaaluminate and carbon dioxide; the final pH of the gel is the pH value at which the reaction of sodium metaaluminate and carbon dioxide is terminated.
In another embodiment of the method according to the present invention, the step (2) of staged heat aging comprises: firstly, programming to 50-100 ℃ and aging for 30-120 min, preferably programming to 60-80 ℃ and aging for 40-80 min; and then the temperature is programmed to 100-220 ℃ for aging for 1-10 h, preferably 120-180 ℃ for aging for 2-6 h.
In the application, the container in the step (2) is generally a container resistant to high temperature, pressure and acid and alkali corrosion, and a glass container, a stainless steel container, a reaction kettle and the like can be adopted; the temperature programming speed is generally controlled within the range of 4-6 ℃/min. Suitable aging temperatures and aging times have a significant effect on grain nucleation and growth, which is also why the present invention employs the aforementioned staged elevated temperature aging.
In another embodiment of the method according to the present invention, step (3) may be an intermittent washing in which the filter cake obtained by filtering the aged slurry is slurried with deionized water and filtered, and then the thus obtained filter cake is slurried with deionized water and filtered; or continuously washing the filter cake obtained by filtering the aged slurry with deionized water; continuous washing is preferably employed.
In the application, the washing mode in the step (3) can be divided into intermittent washing and continuous washing, wherein the former refers to that the filter cake is pulped to be filtered into one washing, and repeated for a plurality of times, such as 4 times of washing, namely pulping for 4 times and filtering for 4 times; the latter means that deionized water is added continuously in the filtering process, and beating is not repeated after the first beating until washing is completed. In continuous washing, the water and solid system are always in dynamic balance, which is more beneficial to reducing Na in pseudo-boehmite products 2 O content, and promotes grain growth.
In another embodiment of the method according to the invention, the deionized water has a temperature of 60 to 90 ℃, preferably 80 to 90 ℃.
In another embodiment of the process according to the invention, the drying described in step (4) is carried out at a temperature of 60 to 120 ℃, preferably at a temperature of 70 to 100 ℃ for 2 to 4 hours.
In another aspect, the present invention provides a pseudo-boehmite prepared according to the method of the previous embodiment, the pseudo-boehmite having: crystallinity not less than 90%, grain size of 5-12 nm, 100-300 m 2 Specific surface area per gram, and 0.4 to the whole1.0mL/g pore volume.
In one embodiment of the pseudo-boehmite according to the invention, the pseudo-boehmite has: crystallinity of 90-97%, grain size of 5-10 nm, 120-250 m 2 Specific surface area per gram and pore volume of 0.5-0.8 mL/g.
In the present application, the crystallinity refers to a percentage of the mass of the crystalline state in the material to the total mass, and is measured by an X-ray powder diffraction (XRD).
In the present application, the grain size refers to a dimension of a crystal grain size, and is measured by an X-ray powder diffraction method (XRD).
In the present application, the crystallinity and grain size of the sample were measured by X-ray powder diffraction (XRD) using RIPP145-90 and RIPP146-90 standard methods (see "petrochemical analysis method (RIPP test method) Yang Cuiding et al, scientific Press, 1990). The calculation formula of the grain size is as follows:
Figure BDA0003311024080000051
where k=1.075, λ is the anode radiation kα 1 Wavelength of spectral line beta 1 The integral width of the diffraction peak is pseudo-boehmite 041, 130, and θ is the Bragg diffraction angle of the diffraction peak.
In the present application, the specific surface area and the total pore volume of the sample were determined by the BET method, i.e., the low temperature static nitrogen adsorption capacity method using ASAP 2405N.1.01 auto-adsorbent apparatus from Micromeritics, america, sample size of 1.33X10 -2 Vacuum degassing at 300 deg.C under Pa for 4 hr, and mixing with N 2 The adsorption-desorption isotherms of the samples were determined at 77.4K for the adsorption media. Calculating the specific surface area of the sample according to the BET formula (S BET ) Sample adsorption N when the relative pressure p/p0=0.98 was measured 2 Is converted to a liquid nitrogen volume, i.e. the total pore volume.
In the present application, na 2 The O content was determined by X-ray fluorescence spectroscopy.
Example 1
Concentration of 60gAl 2 O 3 Sodium metaaluminate solution/L with 50% by volume of diAnd (3) performing gelling reaction on carbon dioxide gas, controlling the flow rate of the carbon dioxide gas to be 3L/min, and controlling the pH value of the end point to be 10. After transferring the obtained slurry to a reaction kettle, firstly heating up to 60 ℃ for aging for 50min at a temperature programming rate of 5 ℃/min, then heating up to 120 ℃ for aging for 3h at a temperature programming rate of 5 ℃/min, carrying out solid-liquid separation on the obtained slurry after the aging is finished, continuously washing with deionized water at 80 ℃ for half an hour to obtain a product filter cake with impurities removed, drying at 100 ℃ for 3h, and crushing to obtain pseudo-boehmite powder A1, wherein the physicochemical properties are shown in the table 1 below.
Example 2
The concentration of Al is 40g 2 O 3 And (3) carrying out gel forming reaction on the sodium metaaluminate solution/L and 45% carbon dioxide gas by volume, wherein the flow rate of the carbon dioxide gas is 2L/min, and the end point pH value is controlled to be 10.5. After transferring the obtained slurry to a reaction kettle, firstly heating up to 65 ℃ for ageing for 45min at a temperature programming rate of 5 ℃/min, then heating up to 135 ℃ for ageing for 4h at a temperature programming rate of 5 ℃/min, carrying out solid-liquid separation on the obtained slurry after the ageing is finished, continuously washing with deionized water at 80 ℃ for half an hour to obtain a product filter cake with impurities removed, drying at 100 ℃ for 3h, and crushing to obtain pseudo-boehmite powder A2, wherein the physicochemical properties are shown in the table 1 below.
Example 3
Concentration of 30gAl 2 O 3 And (3) carrying out gel forming reaction on the sodium metaaluminate solution/L and 45% carbon dioxide gas by volume, wherein the flow rate of the carbon dioxide gas is 2L/min, and the end point pH value is controlled to be 10.5. After transferring the obtained slurry to a reaction kettle, firstly heating up to 70 ℃ for aging for 50min at a temperature programming rate of 5 ℃/min, then heating up to 150 ℃ for aging for 4h at a temperature programming rate of 5 ℃/min, carrying out solid-liquid separation on the obtained slurry after aging, continuously washing with deionized water at 90 ℃ for half an hour to obtain a product filter cake with impurities removed, drying at 100 ℃ for 3h, and crushing to obtain pseudo-boehmite powder A3, wherein the physicochemical properties are shown in the table 1 below.
Example 4
Concentration of 20gAl 2 O 3 And (3) carrying out gel forming reaction on the sodium metaaluminate solution/L and carbon dioxide gas with the volume fraction of 33%, wherein the flow rate of the carbon dioxide gas is 2L/min, and the end point pH value is controlled to be 10.5. After transferring the obtained slurry to a reaction kettle, the temperature is programmed (the temperature rising rate is 5 ℃/min) to 70 ℃ and then the slurry is aged for 60minAnd (3) heating to 170 ℃ for aging for 5 hours at a temperature programming rate of 5 ℃/min, carrying out solid-liquid separation on the obtained slurry after aging, continuously washing with deionized water at 90 ℃ for half an hour to obtain a product filter cake with impurities removed, drying at 100 ℃ for 3 hours, and crushing to obtain pseudo-boehmite powder A4, wherein the physicochemical properties are shown in the table 1 below.
Example 5
Concentration of 15gAl 2 O 3 And (3) carrying out gelling reaction on the sodium metaaluminate solution/L and carbon dioxide gas with the volume fraction of 25%, wherein the flow rate of the carbon dioxide gas is 1L/min, and the end point pH value is controlled to be 11. After transferring the obtained slurry to a reaction kettle, firstly heating to 75 ℃ for aging for 70min at a temperature programming rate of 5 ℃/min, then heating to 180 ℃ for aging for 5h at a temperature programming rate of 5 ℃/min, after the aging is finished, carrying out solid-liquid separation on the obtained slurry, continuously washing with 90 ℃ water ion water for half an hour to obtain a product filter cake with impurities removed, drying at 100 ℃ for 3h, and crushing to obtain pseudo-boehmite powder A5, wherein the physicochemical properties are shown in the following table 1.
Comparative example 1
Concentration of 40gAl 2 O 3 And (3) carrying out gel forming reaction on the sodium metaaluminate solution/L and 45% carbon dioxide gas by volume, wherein the flow rate of the carbon dioxide gas is 2L/min, and the end point pH value is controlled to be 10.5. Transferring the obtained slurry to a reaction kettle, carrying out hydrothermal aging for 3 hours at 100 ℃, carrying out solid-liquid separation on the obtained slurry after the aging is finished, continuously washing with deionized water at 80 ℃ for half an hour to obtain a product filter cake with impurities removed, drying for 3 hours at 100 ℃, and crushing to obtain pseudo-boehmite powder D1, wherein the physicochemical properties are shown in the table 1 below.
Comparative example 2
Pseudo-boehmite was prepared as in example 1 except that deionized water was intermittently washed 4 times at 80 ℃. Pseudo-boehmite powder D2 was obtained, and its physicochemical properties are shown in Table 1 below.
Comparative example 3
This comparative example pseudo-boehmite was prepared according to the method described in example 4 of CN105645446a, with the following specific steps:
taking refined sodium aluminate solution as a raw material, introducing carbon dioxide gas with the volume concentration of 30-40% into the refined sodium aluminate solution with the alumina content of 60g/l, and rapidly carrying out liquid-solid separation on the obtained slurry when the pH value of the slurry is 12. The separated filter cake was put into a sealed flask, aged in a water bath at 95 ℃ for 3.5 hours, then added with hot water at 95 ℃ to form slurry, repeatedly stirred and washed to remove impurities, and dried in an oven to obtain pseudo-boehmite D3, the physicochemical properties of which are shown in Table 1 below.
Comparative example 4
This comparative example pseudo-boehmite was prepared according to the method described in example 1 of CN110304644a, with the following specific steps:
firstly purifying sodium aluminate solution, then using Al 2 O 3 45g/L high-purity sodium aluminate solution is taken as raw material, and CO with the concentration of 40 percent is introduced 2 The gas is subject to a gel forming reaction, and the flow rate per hour is controlled to be 3.0m 3 Reaction time is controlled to be 40 minutes, and Al is controlled 2 O 3 5g/l remained, and the final temperature was controlled at 35 ℃. The slurry after the reaction was subjected to separation washing, and the filter cake was washed with high purity water at 85 ℃ until the filter cake pH was 7.0. Adding high-purity water into the obtained filter cake, stirring to obtain slurry, adding urea with the concentration of 8g/L, stirring for 50min, transferring the slurry into an autoclave device, controlling the temperature of the autoclave to 160 ℃, controlling the pressure to 0.6MPa, keeping the temperature for 4h for reaction, cooling, discharging, filtering and washing after the reaction is finished, controlling the pH value of the filter cake to 7.0, drying at 100 ℃ to control the water content of the product to 15%, and crushing to obtain the final product pseudo-boehmite D4, wherein the physical and chemical properties are shown in the table 1 below.
TABLE 1 pseudo-boehmite Performance index
Examples Crystallinity, percent Grain size, nm Na 2 O,% Specific surface area, m 2 /g Total pore volume, mL/g
A1 93.3 5.7 0.0723 252.36 0.53
A2 92.7 6.7 0.0692 204.58 0.58
A3 94.1 7.5 0.0633 189.33 0.63
A4 96.4 8.5 0.0572 177.21 0.67
A5 95.6 9.2 0.049 128.41 0.74
D1 78.2 3.7 0.0671 329.24 0.43
D2 90.9 4.9 0.0884 250.76 0.5
D3 75.8 3.4 0.07534 351.75 0.42
D4 88.1 4.9 0.03895 182.4 0.50
The data in Table 1 shows that the crystallinity of pseudo-boehmite prepared by the method of the invention is significantly higher than pseudo-boehmite prepared by other methods, and the grain size of the pseudo-boehmite is adjustable.
The present application has been described in connection with the preferred embodiments, but these embodiments are merely exemplary and serve only as illustrations. On the basis of this, many alternatives and improvements can be made to the present application, which fall within the scope of protection of the present application.

Claims (10)

1. A method for preparing grain size-adjustable pseudo-boehmite, comprising the steps of:
(1) Neutralizing the sodium metaaluminate solution with carbon dioxide gas to form gel;
(2) The slurry after the gel formation is subjected to sectional temperature raising and aging in a closed container;
(3) Filtering the aged slurry and washing with deionized water; a kind of electronic device with high-pressure air-conditioning system
(4) And drying the filter cake obtained after washing to obtain the pseudo-boehmite with adjustable grain size.
2. The process according to claim 1, wherein the sodium metaaluminate solution in step (1) has a concentration of 10 to 80gAl 2 O 3 Preferably 15 to 60g Al 2 O 3 L; the volume concentration of the carbon dioxide gas is 15-50%, preferably 25-50%; the glue forming temperature is lower than 50 ℃; the final pH value of the gel is 9-11.
3. The method according to claim 1 or 2, wherein the staged elevated temperature ageing in step (2) comprises: firstly, programming to 50-100 ℃ and aging for 30-120 min, preferably programming to 60-80 ℃ and aging for 40-80 min; and then the temperature is programmed to 100-220 ℃ for aging for 1-10 h, preferably 120-180 ℃ for aging for 2-6 h.
4. A method according to claim 3, wherein step (3) is performed by beating a cake obtained by filtering the aged slurry with deionized water and filtering, and then intermittently washing the cake obtained thereby by beating and filtering with deionized water; or continuously washing the filter cake obtained by filtering the aged slurry with deionized water; continuous washing is preferably employed.
5. The process according to claim 4, wherein the deionized water has a temperature of 60 to 90 ℃, preferably 80 to 90 ℃.
6. The method according to claim 5, wherein the intermittent washing may be performed 1 to 4 times.
7. The process according to claim 1, wherein the drying in step (4) is carried out at a temperature of 60 to 120 ℃, preferably 70 to 100 ℃, for 2 to 4 hours.
8. A pseudo-boehmite prepared according to the method of any one of the preceding claims characterized in that it has: crystallinity not less than 90%, grain size of 5-12 nm, 100-300 m 2 Specific surface area per gram and pore volume of 0.4-1.0 mL/g.
9. Pseudo-boehmite according to claim 8 characterized in that it has: crystallinity of 90-97%, grain size of 5-10 nm, 120-250 m 2 Specific surface area per gram and pore volume of 0.5-0.8 mL/g.
10. Use of pseudo-boehmite according to claim 8 or 9 in the preparation of a catalyst.
CN202111216663.3A 2021-10-19 2021-10-19 Pseudo-boehmite with adjustable grain size and preparation method and application thereof Pending CN116002733A (en)

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