CN112520768B - Preparation method of rod-shaped high-purity pseudoboehmite - Google Patents
Preparation method of rod-shaped high-purity pseudoboehmite Download PDFInfo
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- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 104
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 17
- 230000032683 aging Effects 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000004537 pulping Methods 0.000 claims abstract description 11
- 238000001694 spray drying Methods 0.000 claims abstract description 11
- 150000007524 organic acids Chemical class 0.000 claims abstract description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims description 8
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 8
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 6
- 235000015165 citric acid Nutrition 0.000 claims description 6
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 4
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims description 4
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 4
- 239000000174 gluconic acid Substances 0.000 claims description 4
- 235000012208 gluconic acid Nutrition 0.000 claims description 4
- 239000004310 lactic acid Substances 0.000 claims description 4
- 235000014655 lactic acid Nutrition 0.000 claims description 4
- 239000001630 malic acid Substances 0.000 claims description 4
- 235000011090 malic acid Nutrition 0.000 claims description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- 235000010443 alginic acid Nutrition 0.000 claims description 3
- 239000000783 alginic acid Substances 0.000 claims description 3
- 229960001126 alginic acid Drugs 0.000 claims description 3
- 229920000615 alginic acid Polymers 0.000 claims description 3
- -1 succinic acid, alginic acid Chemical class 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- 239000008214 highly purified water Substances 0.000 claims 1
- 239000011148 porous material Substances 0.000 abstract description 12
- 239000012498 ultrapure water Substances 0.000 abstract description 10
- 238000009826 distribution Methods 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 5
- 238000004064 recycling Methods 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 description 17
- 239000003054 catalyst Substances 0.000 description 9
- 239000002253 acid Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000006356 dehydrogenation reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001935 peptisation Methods 0.000 description 2
- 238000002407 reforming Methods 0.000 description 2
- 239000001384 succinic acid Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 150000004781 alginic acids Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical group [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004517 catalytic hydrocracking Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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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
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
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- 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
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- C01P2006/17—Pore diameter distribution
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Abstract
The invention discloses a preparation method of rod-shaped high-purity pseudoboehmite. The method comprises the following steps: dissolving aluminum isopropoxide with the purity of 99.99 percent in isopropanol to prepare solution; mixing high-purity water, isopropanol and organic acid to prepare another solution; leading the two solutions into inlets of two channels of a T-shaped microreactor by an advection pump, and aging slurry obtained from an outlet of the reactor for 2h at 80-90 ℃; and filtering, pulping and spray-drying the aged slurry to obtain a rod-shaped high-purity pseudo-boehmite powder, and recycling the isopropanol. The high-purity pseudo-boehmite obtained by the method has the characteristics of controllable pore structure, concentrated pore size distribution, narrow particle size distribution and the like.
Description
Technical Field
The invention belongs to the technical field of catalytic materials, and particularly relates to a preparation method of rod-shaped high-purity pseudo-boehmite.
Background
The pseudo-boehmite is aluminum hydroxide which is incomplete in crystallization and has a thin folded lamellar layer, has the characteristics of good peptization performance, strong cohesiveness, large specific surface area, large pore volume and the like, is mainly used as a production raw material of a catalyst carrier, and is used as a hydrocracking catalyst, a reforming catalyst, an alkane dehydrogenation catalyst, an automobile exhaust purification catalyst and the like in the field of petrochemical industry.
The pseudo-boehmite production method mainly comprises a double-aluminum method, a carbonization method and an aluminum alkoxide method. The double aluminum method and the carbonization method are used for producing the pseudo-boehmite, the synthesis steps mainly comprise the processes of gelatinizing, aging, washing, drying and the like, the process flow is simple, the cost is low, but the product has the problems of high content of impurity elements such as Na, S and Si, large washing water consumption, wide pore size distribution and unstable product; the pseudo-boehmite produced by the alcoaluminum method has the characteristics of environment-friendly production process, low water consumption and the like, has the advantages of high purity, good peptization and the like, is widely applied to the fields of reforming catalysts, dehydrogenation catalysts and hydrogenation catalysts, and has the problems of difficult control of the pore structure of the product, unstable quality and non-centralized distribution of pore diameters and particle sizes.
Disclosure of Invention
The invention aims to overcome the defects of the prior art for producing the pseudoboehmite by the alchol-aluminum method, provides a preparation method of the rod-shaped high-purity pseudoboehmite, obtains the rod-shaped high-purity pseudoboehmite, and better meets the requirements of domestic and foreign enterprises in the field of petrochemical catalysts.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of rod-shaped high-purity pseudo-boehmite comprises the following steps:
1) Dissolving 99.99% pure aluminum isopropoxide in isopropanol to prepare a solution with the aluminum isopropoxide content of 40-60% by weight;
2) Mixing high-purity water, isopropanol and organic acid to prepare another solution, wherein the mass percent of the isopropanol is 20-50 percent, and the addition amount of the organic acid is 10-20 percent of the mass of the isopropanol;
3) Introducing the solution obtained in the step 1) and the solution obtained in the step 2) into inlets of two channels of a T-shaped microreactor by an advection pump, and aging the slurry obtained at an outlet of the reactor; the inner diameter of the T-shaped micro-reactor is 0.2-2 mm;
4) Filtering, pulping and spray drying the aged slurry in the step 3) to obtain the rod-shaped high-purity pseudo-boehmite powder.
In the preparation method of the invention, the flow rate of the solution in the step (1) in the step (3) is 0.5 ml/min-5 ml/min.
In the preparation method of the invention, the flow rate of the solution in the step (2) in the step (3) is 5 ml/min-20 ml/min.
In the preparation method of the present invention, in the solution in step (2), the organic acid is one or more of lactic acid, citric acid, malic acid, tartaric acid, succinic acid, alginic acid and gluconic acid.
In the above preparation method of the present invention, the temperature of the solution obtained in the step (1) in the step (3) is 60 ℃ to 90 ℃.
In the above preparation method of the present invention, the temperature of the solution obtained in the step (2) in the step (3) is 20 ℃ to 40 ℃.
In the above preparation method of the present invention, the aging temperature of the solution in the step (3) is 80 ℃ to 90 ℃.
According to the preparation method of the rod-shaped high-purity pseudo-boehmite, aluminum isopropoxide and hydrolysate are respectively introduced into the two inlets of the T-shaped micro-channel, so that the reacted materials are quickly and efficiently mixed, and the characteristics of controllable specific surface and pore volume, concentrated pore size distribution and narrow particle size distribution of a product are realized. The experimental result shows that the specific surface of the pseudo-boehmite provided by the invention is 200-500 m 2 The pore volume is controllable between 0.4 and 1.4ml/g, the pore size distribution is concentrated, more than 80 percent of pores are concentrated and distributed within the range of most probable pore size +/-3 nm; the particle size distribution is narrow, and is mainly concentrated on 2-10 mu m. In addition, the whole preparation process is environment-friendly and pollution-free, the isopropanol can be recycled, the production cost is low, and the method has excellent industrial production value and economic benefit.
Drawings
FIG. 1 is a schematic reaction flow diagram of a method for preparing a rod-shaped high-purity pseudoboehmite according to the present invention;
in the figure, 1 is a constant flow pump, 2 is a T-shaped microreactor, 21 is a T-shaped microreactor inlet, and 22 is a T-shaped microreactor outlet;
FIG. 2 is an SEM image of pseudo-boehmite prepared by the preparation method of the invention;
FIG. 3 is a graph showing the particle size distribution of the product prepared by the different preparation methods (example 1 and comparative example 1).
Detailed Description
In order to further understand the present invention, the following detailed description is made with reference to the embodiments, which are implemented according to the technical solutions described in the summary of the invention.
Example 1:
1) Dissolving aluminum isopropoxide with the purity of 4N in anhydrous isopropanol at 70 ℃ to form a transparent solution with the mass fraction of the aluminum isopropoxide of 50%, keeping the liquid temperature at 70 ℃, and introducing the solution into an inlet of a T-shaped reactor at the flow rate of 2ml/min, wherein the inner diameter of the T-shaped microreactor is 0.6mm;
2) Mixing high-purity water and isopropanol to prepare a solution with the mass fraction of the isopropanol being 20%, adding lactic acid with the mass fraction of 10% of the isopropanol to prepare another solution, keeping the temperature of the liquid at 30 ℃, and feeding the liquid into the other inlet of the T-shaped reactor at the flow rate of 16 ml/min;
3) Collecting slurry at the outlet of the T-shaped reactor, and aging for 2h at 90 ℃;
4) And filtering, pulping and spray-drying the aged slurry to obtain a rod-shaped high-purity pseudo-boehmite powder, wherein the physicochemical properties of the high-purity pseudo-boehmite powder are shown in a table 1, and the isopropanol is recycled.
Example 2:
1) Dissolving aluminum isopropoxide with the purity of 4N in anhydrous isopropanol at 60 ℃ to form a transparent solution with the mass fraction of the aluminum isopropoxide being 40%, keeping the liquid temperature at 60 ℃, and introducing the solution into an inlet of a T-shaped reactor at the flow rate of 4ml/min, wherein the inner diameter of the T-shaped microreactor is 1.5mm;
2) Mixing high-purity water and isopropanol to prepare a solution with the mass fraction of the isopropanol being 30%, adding mixed acid of malic acid and citric acid with the mass being 15% of that of the isopropanol to prepare another solution, keeping the temperature of the liquid at 20 ℃, and feeding the liquid into the other inlet of the T-shaped reactor at the flow rate of 20 ml/min;
3) Collecting slurry at the outlet of the T-shaped reactor, and aging for 2h at 90 ℃;
4) And filtering, pulping and spray-drying the aged slurry to obtain a rod-shaped high-purity pseudo-boehmite powder with the physical and chemical properties shown in table 1, and recycling the isopropanol.
Example 3:
1) Dissolving aluminum isopropoxide with the purity of 4N in anhydrous isopropanol at the temperature of 80 ℃ to form a transparent solution with the mass fraction of the aluminum isopropoxide being 40%, keeping the liquid temperature at 70 ℃, and introducing the solution into an inlet of a T-shaped reactor at the flow rate of 3ml/min, wherein the inner diameter of the T-shaped microreactor is 1.0mm;
2) Mixing high-purity water and isopropanol to prepare a solution with the mass fraction of the isopropanol being 20%, adding tartaric acid with the mass being 15% of the mass of the isopropanol to prepare another solution, keeping the temperature of the liquid at 40 ℃, and feeding the liquid into the other inlet of the T-shaped reactor at the flow rate of 15 ml/min;
3) Collecting slurry at the outlet of the T-shaped reactor, and aging for 2h at 90 ℃;
4) And filtering, pulping and spray-drying the aged slurry to obtain a rod-shaped high-purity pseudo-boehmite powder with the physical and chemical properties shown in table 1, and recycling the isopropanol.
Example 4:
1) Dissolving aluminum isopropoxide with the purity of 4N in anhydrous isopropanol at 90 ℃ to form a transparent solution with the mass fraction of the aluminum isopropoxide being 40%, keeping the liquid temperature at 90 ℃, and introducing the solution into an inlet of a T-shaped reactor at a flow rate of 2ml/min, wherein the inner diameter of the T-shaped microreactor is 0.8mm;
2) Mixing high-purity water and isopropanol to prepare a solution with the mass fraction of the isopropanol being 40%, adding mixed acid of citric acid and succinic acid with the mass fraction of 15% of the isopropanol to prepare another solution, keeping the temperature of the liquid at 20 ℃, and feeding the liquid into the other inlet of the T-shaped reactor at the flow rate of 10 ml/min;
3) Collecting slurry at the outlet of the T-shaped reactor, and aging for 2h at 90 ℃;
4) And filtering, pulping and spray-drying the aged slurry to obtain a rod-shaped high-purity pseudo-boehmite powder with the physical and chemical properties shown in table 1, and recycling the isopropanol.
Example 5:
1) Dissolving aluminum isopropoxide with the purity of 4N in anhydrous isopropanol at 90 ℃ to form a transparent solution with the aluminum isopropoxide mass fraction of 50%, keeping the liquid temperature at 80 ℃, and introducing the solution into an inlet of a T-shaped reactor at a flow rate of 1ml/min, wherein the inner diameter of the T-shaped microreactor is 0.6mm;
2) Mixing high-purity water and isopropanol to prepare a solution with the mass fraction of the isopropanol being 30%, adding a mixed acid of alginic acid and gluconic acid with the mass fraction of the isopropanol being 12% to prepare another solution, keeping the temperature of the liquid at 30 ℃, and feeding the liquid into the other inlet of the T-shaped reactor at the flow rate of 10 ml/min;
3) Collecting slurry at the outlet of the T-shaped reactor, and aging for 2h at 90 ℃;
4) And filtering, pulping and spray-drying the aged slurry to obtain a rod-shaped high-purity pseudo-boehmite powder, wherein the physicochemical properties of the high-purity pseudo-boehmite powder are shown in a table 1, and the isopropanol is recycled.
Example 6:
1) Dissolving aluminum isopropoxide with the purity of 4N in anhydrous isopropanol at 90 ℃ to form a transparent solution with the mass fraction of the aluminum isopropoxide of 45%, keeping the liquid temperature at 90 ℃, and introducing the solution into an inlet of a T-shaped reactor at the flow rate of 4ml/min, wherein the inner diameter of the T-shaped microreactor is 1.8mm;
2) Mixing high-purity water and isopropanol to prepare a solution with the mass fraction of the isopropanol being 30%, adding mixed acid of lactic acid and gluconic acid with the mass fraction of the isopropanol being 12% to prepare another solution, keeping the liquid temperature at 20 ℃, and entering the other inlet of the T-shaped reactor at the flow rate of 20 ml/min;
3) Collecting slurry at the outlet of the T-shaped reactor, and aging for 2h at 85 ℃;
4) And filtering, pulping and spray-drying the aged slurry to obtain a rod-shaped high-purity pseudo-boehmite powder with the physical and chemical properties shown in table 1, and recycling the isopropanol.
Comparative example 1:
1) Dissolving aluminum isopropoxide with the purity of 4N in anhydrous isopropanol at 60 ℃ to form a transparent solution 1 with the mass fraction of the aluminum isopropoxide of 40%;
2) Mixing high-purity water and isopropanol to prepare a solution with the mass fraction of the isopropanol being 30%, and adding mixed acid of malic acid and citric acid with the mass being 15% of that of the isopropanol to prepare another solution 2;
3) Under the condition of rapid stirring of a stirring kettle, adding the solution 1 into the kettle at a flow rate of 4ml/min at 60 ℃ and the solution 2 at a flow rate of 20ml/min at 20 ℃ in a parallel flow manner;
4) Aging the slurry at 90 deg.C for 2h;
5) And filtering, pulping and spray-drying the aged slurry to obtain the high-purity pseudo-boehmite powder, wherein the physicochemical properties of the pseudo-boehmite powder are shown in a table 1, and the isopropanol is recycled.
Comparative example 2:
1) Dissolving aluminum isopropoxide with the purity of 4N in anhydrous isopropanol at 90 ℃ to form a transparent solution 1 with the mass fraction of the aluminum isopropoxide of 40%;
2) Mixing high-purity water and isopropanol to prepare a solution with the mass fraction of the isopropanol being 40%, and adding mixed acid of citric acid and succinic acid with the mass fraction of 15% of the isopropanol to prepare another solution 2;
3) Under the condition of rapid stirring of a stirring kettle, adding the solution 1 into the kettle at the temperature of 90 ℃ at the flow rate of 2ml/min and the solution 2 at the temperature of 20 ℃ at the flow rate of 10ml/min in a parallel flow manner;
4) Aging the slurry at 90 deg.C for 2h;
5) And filtering, pulping and spray-drying the aged slurry to obtain the high-purity pseudo-boehmite powder, wherein the physicochemical properties of the pseudo-boehmite powder are shown in a table 1, and the isopropanol is recycled.
TABLE 1 physicochemical Properties of the products of the examples and comparative examples
Claims (5)
1. A preparation method of rod-shaped high-purity pseudo-boehmite is characterized by comprising the following steps:
1) Dissolving 99.99% pure aluminum isopropoxide in isopropanol to prepare a solution with the aluminum isopropoxide content of 40-60% by weight;
2) Mixing highly purified water, isopropanol and an organic acid to make another solution, wherein the mass percentage of isopropanol is 20-50% wt, the amount of organic acid added is 10-20% of the mass of isopropanol;
3) Introducing the solution obtained in the step 1) and the solution obtained in the step 2) into inlets of two channels of a T-shaped microreactor by an advection pump, and aging the slurry obtained at an outlet of the reactor; the inner diameter of the T-shaped micro-reactor is 0.2-2 mm; the aging temperature in the step (3) is 80-90 ℃, and the aging time is 2-4 h;
4) Filtering, pulping and spray drying the aged slurry in the step 3) to obtain a rod-shaped high-purity pseudo-boehmite powder;
in the solution in the step 2), the organic acid is one or more of lactic acid, citric acid, malic acid, tartaric acid, succinic acid, alginic acid and gluconic acid.
2. The method for preparing a rod-shaped highly pure pseudoboehmite according to claim 1, wherein the flow rate of the solution of the step 1) in the step 3) is 0.5ml/min to 5ml/min.
3. The method for preparing a rod-shaped highly pure pseudoboehmite according to claim 1, wherein the flow rate of the solution of the step 2) in the step 3) is 5ml/min to 20ml/min.
4. The method for preparing a rod-shaped highly pure pseudoboehmite according to claim 1, characterized in that the temperature of the solution of step 1) in step 3) is 60 ℃ to 90 ℃.
5. The method for preparing a rod-shaped high-purity pseudoboehmite according to claim 1, characterized in that the temperature of the solution of step 2) in step 3) is 20 ℃ to 40 ℃.
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