CN112520768A - Preparation method of rod-shaped high-purity pseudo-boehmite - Google Patents
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Abstract
The invention discloses a preparation method of rod-shaped high-purity pseudo-boehmite. The method comprises the following steps: dissolving aluminum isopropoxide with the purity of 99.99% in isopropanol to prepare a 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 aluminum alkoxide method has the characteristics of environment-friendly production process, low water consumption and the like, and the product 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, but has the problems of difficult control of the pore structure of the product, unstable quality and non-centralized pore size distribution and particle size distribution.
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 aluminum isopropoxide with the purity of 99.99% in isopropanol to prepare a solution with the mass percentage of the aluminum isopropoxide of 40-60% by weight;
2) mixing high-purity water, isopropanol and organic acid to prepare another solution, wherein the mass percentage of the isopropanol is 20-50 wt%, and the addition amount of the organic acid is 10-20 wt% 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 obtained 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 invention, 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.
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 ℃.
The preparation method of the rod-shaped high-purity pseudo-boehmite guides the aluminum isopropoxide and the hydrolysate into two inlets of the T-shaped micro-channel respectively, realizes the quick and efficient mixing of the materials after the reaction, and simultaneously realizes the control of the specific surface and the pore volume of the product, the centralized pore size distribution and the particle size neutralizationNarrow distribution of degree. Experimental results show that the specific surface of the pseudo-boehmite provided by the invention is 200-500 m2The pore volume is controllable within 0.4-1.4 ml/g, the pore size distribution is concentrated, and more than 80% of pores are concentrated and distributed within the range of most probable pore size +/-3 nm; the particle size distribution is narrow, and the particle size distribution is mainly concentrated at 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 0.6 mm;
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 1.5 mm;
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, wherein the physicochemical properties of the high-purity pseudo-boehmite powder are shown in a table 1, and the isopropanol is recycled.
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 of 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 1.0 mm;
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 fraction of 15% 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, wherein the physicochemical properties of the high-purity pseudo-boehmite powder are shown in a table 1, and the isopropanol is recycled.
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 temperature of the liquid at 90 ℃, and introducing the liquid 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 0.8 mm;
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, wherein the physicochemical properties of the high-purity pseudo-boehmite powder are shown in a table 1, and the isopropanol is recycled.
Example 5:
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 50%, keeping the liquid temperature at 80 ℃, and introducing the solution into an inlet of a T-shaped reactor at the flow rate of 1ml/min, wherein the inner diameter of the T-shaped microreactor is 0.6 mm;
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 1.8 mm;
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 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 85 ℃;
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.
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 a flow rate of 20ml/min at 20 ℃ in a parallel flow manner;
4) aging the slurry at 90 deg.C for 2 h;
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 2 h;
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 (7)
1. A preparation method of rod-shaped high-purity pseudo-boehmite is characterized by comprising the following steps:
1) dissolving aluminum isopropoxide with the purity of 99.99% in isopropanol to prepare a solution with the mass percentage of the aluminum isopropoxide of 40-60% by weight;
2) mixing high-purity water, isopropanol and organic acid to prepare another solution, wherein the mass percentage of the isopropanol is 20-50 wt%, and the addition amount of the organic acid is 10-20 wt% 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 obtained in the step 3) to obtain the rod-shaped high-purity pseudo-boehmite powder.
2. The method for preparing a rod-shaped highly pure pseudoboehmite according to claim 1, characterized in that the flow rate of the solution of the step (1) in the step (3) is 0.5ml/min to 5 ml/min.
3. The method for preparing a rod-shaped highly pure pseudoboehmite according to claim 1, characterized in that the flow rate of the solution of the step (2) in the step (3) is 5ml/min to 20 ml/min.
4. The method for preparing the rod-shaped high-purity pseudoboehmite according to claim 1, characterized in that 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.
5. The method for preparing a rod-shaped highly pure pseudoboehmite according to claim 1, characterized in that the temperature of the solution of the step (1) in the step (3) is 60 ℃ to 90 ℃.
6. The method for preparing a rod-shaped highly pure pseudoboehmite according to claim 1, characterized in that the temperature of the solution of the step (2) in the step (3) is 20 ℃ to 40 ℃.
7. The method for preparing the rod-shaped high-purity pseudoboehmite according to claim 1, characterized in that the aging temperature in the step (3) is 80 ℃ to 90 ℃ and the aging time is 2h to 4 h.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0113796A1 (en) * | 1982-11-23 | 1984-07-25 | Degussa Aktiengesellschaft | Hydrous alumina essentially consisting of pseudoboehmite, process for producing it and its use |
| CN101450812A (en) * | 2007-12-07 | 2009-06-10 | 中国科学院大连化学物理研究所 | Method for preparing nano pseudo boehmite and microchannel reactor |
| CN104192880A (en) * | 2014-07-18 | 2014-12-10 | 大连理工大学 | Method for preparing high-purity pseudo-boehmite |
| CN104671265A (en) * | 2013-11-26 | 2015-06-03 | 中国石油化工股份有限公司 | A method of preparing pseudoboehmite |
| CN106348325A (en) * | 2016-11-11 | 2017-01-25 | 清华大学 | Gamma-alumina and preparation method thereof |
| CN109721088A (en) * | 2017-10-27 | 2019-05-07 | 中国石油化工股份有限公司 | A kind of aluminium hydroxide and preparation method thereof |
| CN109721087A (en) * | 2017-10-27 | 2019-05-07 | 中国石油化工股份有限公司 | A kind of boehmite and preparation method thereof |
-
2020
- 2020-12-13 CN CN202011458083.0A patent/CN112520768B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0113796A1 (en) * | 1982-11-23 | 1984-07-25 | Degussa Aktiengesellschaft | Hydrous alumina essentially consisting of pseudoboehmite, process for producing it and its use |
| CN101450812A (en) * | 2007-12-07 | 2009-06-10 | 中国科学院大连化学物理研究所 | Method for preparing nano pseudo boehmite and microchannel reactor |
| CN104671265A (en) * | 2013-11-26 | 2015-06-03 | 中国石油化工股份有限公司 | A method of preparing pseudoboehmite |
| CN104192880A (en) * | 2014-07-18 | 2014-12-10 | 大连理工大学 | Method for preparing high-purity pseudo-boehmite |
| CN106348325A (en) * | 2016-11-11 | 2017-01-25 | 清华大学 | Gamma-alumina and preparation method thereof |
| CN109721088A (en) * | 2017-10-27 | 2019-05-07 | 中国石油化工股份有限公司 | A kind of aluminium hydroxide and preparation method thereof |
| CN109721087A (en) * | 2017-10-27 | 2019-05-07 | 中国石油化工股份有限公司 | A kind of boehmite and preparation method thereof |
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