CN110395756B - Method for preparing pseudoboehmite with large pore volume, multiple pore channels and wide distribution - Google Patents
Method for preparing pseudoboehmite with large pore volume, multiple pore channels and wide distribution Download PDFInfo
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- CN110395756B CN110395756B CN201910535925.9A CN201910535925A CN110395756B CN 110395756 B CN110395756 B CN 110395756B CN 201910535925 A CN201910535925 A CN 201910535925A CN 110395756 B CN110395756 B CN 110395756B
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- C—CHEMISTRY; METALLURGY
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- 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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- C01F7/00—Compounds of aluminium
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- C01P2006/14—Pore volume
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a method for preparing pseudoboehmite with large pore volume, multiple pore channels and wide distribution, which comprises the following operation steps: (1) reacting 2N-5N aluminum raw material with alcohol under catalysis to obtain aluminum alkoxide, and preserving heat; (2) distilling and purifying, transferring the aluminum alkoxide obtained after purification to a hydrolysis reaction kettle, adding 1-8 per mill of nano-boehmite seed crystals, adding an alcohol solution, and keeping the temperature; (3) hydrolyzing, adding an auxiliary agent, and preserving heat to obtain the pseudo-boehmite product with large pore volume, multiple pore passages and wide distribution. The method adopts 2N-5N aluminum products, and meets the requirements of 1.0-1.3cc/g of pseudo-boehmite products with large pore volume and double-peak distribution multi-pore channels, and the products obtained by the method have larger pore volume, more abundant pore channels, are not easy to collapse by adding acid, and have better strength of the molded carrier.
Description
Technical Field
The invention relates to a method for preparing pseudoboehmite, in particular to a method for preparing pseudoboehmite with large pore volume, multiple pore channels and wide distribution.
Background
Pseudo-boehmite, also known as monohydrate alumina, is an important catalyst raw material and is widely applied in the petrochemical field such as catalytic cracking, hydrogenation, reforming and the like. Besides being an important catalyst carrier, the pseudoboehmite is also a main adhesive for preparing other various catalysts and has a non-negligible effect.
At present, due to the heavy cracking of raw materials in the petroleum and petrochemical industry, for a hydrotreating catalyst such as heavy crude oil, coal tar, shale oil and tar sand oil, an active alumina carrier used by the catalyst has to have a sufficiently large pore volume and a suitable pore structure to show good catalytic activity, and can effectively reduce coking and avoid activity reduction or inactivation caused by deposition of heavy metal impurities. Therefore, the alkoxide pseudo-boehmite product with large pore volume and good pore channels is lacked in the market.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
Aiming at the technical problems, the invention provides a method for preparing pseudoboehmite with large pore volume, multiple pore passages and wide distribution, aiming at obtaining the pseudoboehmite with large pore volume, multiple pore passages and wide distribution, which has the advantages of low cost, simple process and easy operation.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a method for preparing pseudoboehmite with large pore volume, multiple pore paths and wide distribution comprises the following operation steps:
(1) reacting 2N-5N aluminum raw material with alcohol under the catalysis of mercuric chloride or aluminum chloride to obtain aluminum alkoxide, and preserving heat for 5-12h at the temperature of 100-;
(2) distilling and purifying the substance obtained after heat preservation in the step (1) at the temperature of 160-200 ℃ for 10-16h, transferring the aluminum alkoxide obtained after purification to a hydrolysis reaction kettle, simultaneously adding 1-8 per mill of nano-diaspore seed crystals according to the mass percentage, adding an alcohol solution according to the mol ratio of 1:20-65, and preserving heat at the temperature of 60-240 ℃ for 2-24 h;
(3) hydrolyzing the substance obtained in the step (2) for 4-12h, wherein the hydrolyzed mixture is the mixture of alcohol and high-purity water or deionized water, the alcohol content is 55-95%, 0.3-1% of auxiliary agent is added, and the heat preservation is carried out for 2-24h at the temperature of 60-240 ℃ to obtain the pseudoboehmite product with large pore volume, multiple pore channels and wide distribution.
Preferably, the aluminum raw material in the step (1) is one of high-purity aluminum products such as aluminum sheets, aluminum blocks, aluminum particles, aluminum ingots or waste electronic aluminum foils.
Preferably, the 3N aluminium feedstock of step (1) is reacted with an alcohol under catalysis of mercuric chloride or aluminium chloride.
Preferably, the alcohol in step (1) is one of isopropanol, n-butanol, isobutanol, n-pentanol and isoamyl alcohol.
Preferably, the reaction in step (1) is carried out at 83-84 ℃ for 6-10 h.
Preferably, the hydrolysis temperature in step (2) is 65-95 ℃.
Preferably, the hydrolysis in the step (2) is carried out by mixing aluminum alkoxide and alcohol solution according to the molar ratio of 1: 20-65; the alcohol solution is prepared by mixing water and alcohol in a molar ratio of 1: 1-6, wherein the alcohol is one of isopropanol, n-butanol, isobutanol, n-pentanol and isoamylol.
Preferably, the nano diaspore seed crystals added in the step (2) are diaspore raw powder with the crystallinity of 75-80 percent and the grain size of 10-50 nanometers.
Preferably, the auxiliary agent in step (3) is one or a mixture of two of nitric acid, hydrochloric acid, citric acid, glacial acetic acid, hydrogen peroxide, water glass, silicate, oleic acid, urea, ammonia, lauryl alcohol and dodecane esters.
Compared with the prior art, the invention has the following beneficial effects:
the method adopts 2N-5N aluminum products, and meets the requirements of 1.0-1.3cc/g of pseudo-boehmite products with large pore volume and double-peak distribution multi-pore channels, and the products obtained by the method have larger pore volume, more abundant pore channels, are not easy to collapse by adding acid, and have better strength of the molded carrier.
Drawings
FIGS. 1 and 2 show the pore distribution, pore channel adsorption and desorption of the product prepared by the method of the present invention by BET method.
Detailed Description
The following detailed description is to be read in connection with the accompanying drawings, but it is to be understood that the scope of the invention is not limited to the specific embodiments.
Example 1
A method for preparing pseudoboehmite with large pore volume, multiple pore paths and wide distribution comprises the following operation steps:
(1) putting 150g of 4N waste electronic aluminum foil with the thickness of 1-5mm and 1000g of isopropanol into a 5L reactor, reacting for 7h at 83 ℃ under the catalysis of mercuric chloride to obtain aluminium isopropoxide alkoxide, and preserving heat for 10h at 180 ℃;
(2) transferring the substance obtained after heat preservation in the step (1) into a 3L container, distilling and purifying for 10h at the temperature of 160-200 ℃, removing waste residues to obtain purified isopropanol aluminum alkoxide, transferring the purified isopropanol aluminum alkoxide into a hydrolysis reaction kettle, adding nano-diaspore seed crystals (diaspore raw powder with the crystallinity of 75-80 percent and the grain size of 10-50 nm) with the mass of 5 per mill of the isopropanol aluminum alkoxide, and performing the following steps in a molar ratio of 1: 20-25 adding an alcohol solution (the alcohol solution is obtained by mixing deionized water and isopropanol according to the molar ratio of 1: 6), and then preserving heat for 7-8h at 150 +/-10 ℃;
(3) and (3) mechanically stirring and hydrolyzing the substance obtained after heat preservation in the step (2) for 8h at 75 ℃, adding an auxiliary agent citric acid which is 0.5 percent of the mass of the substance obtained after hydrolysis and has the alcohol content of 70 percent to the mixture obtained by hydrolysis, and preserving the heat for 8-10h at 160 +/-10 ℃ to obtain the pseudo-boehmite product with the pore volume of 1.25cc/g, the purity of 99.99 percent and multiple pores and wide distribution.
Example 2
A method for preparing pseudoboehmite with large pore volume, multiple pore paths and wide distribution comprises the following operation steps:
(1) putting 150g of 3N aluminum blocks with the thickness of 3-5mm and 1000g of N-butyl alcohol into a 5L reactor, reacting for 8h at 84 ℃ under the catalysis of aluminum chloride to obtain N-butanol aluminum alkoxide, and preserving heat for 12h at 160 ℃;
(2) transferring the substance obtained after heat preservation in the step (1) into a 3L container, distilling and purifying for 12h at 180-200 ℃, removing waste residues to obtain purified n-butanol aluminum alkoxide, transferring the purified n-butanol aluminum alkoxide into a hydrolysis reaction kettle, adding nano seed crystals (monohydrate aluminum powder with the crystallinity of 75-80 percent and the grain size of 10-50 nm) with the mass of 8 per mill of the n-butanol aluminum alkoxide, and performing the following steps in a molar ratio of 1: 30-45 adding alcohol solution (the alcohol solution is obtained by mixing high-purity water and n-butanol at a molar ratio of 1: 4), and keeping the temperature at 120 +/-10 ℃ for 16-18 h;
(3) and (3) mechanically stirring and hydrolyzing the substance obtained after heat preservation in the step (2) at 65 ℃ for 12h, adding nitric acid which is an auxiliary agent and is 0.3 percent of the mass of the substance obtained after hydrolysis, and preserving the heat at 230 +/-10 ℃ for 2-4h to obtain the pseudo-boehmite product with the pore volume of 1.15cc/g and the purity of 99.95 percent, wherein the mixed solution is formed by alcohol and high-purity water and the alcohol content is 80 percent.
Example 3
A method for preparing pseudoboehmite with large pore volume, multiple pore paths and wide distribution comprises the following operation steps:
(1) putting 150g of 5N aluminum particles with the thickness of 3-5mm and 1000 parts of isoamyl alcohol into a 5L reactor, reacting for 6 hours at 83 ℃ under the catalysis of mercuric chloride to obtain isoamyl alcohol aluminum alkoxide, and preserving heat for 5 hours at 100 ℃;
(2) transferring the substance obtained after the heat preservation in the step (1) into a 3L container, distilling and purifying for 16h at the temperature of 160-200 ℃, removing waste residues to obtain purified isoamyl alcohol aluminum alkoxide, transferring the purified isoamyl alcohol aluminum alkoxide into a hydrolysis reaction kettle, adding nano seed crystals (the monohydrate aluminum powder with the crystallinity of 75-80 percent and the grain size of 10-50 nm) with the mass of 1 per mill of the isoamyl alcohol aluminum alkoxide, and mixing the raw powder with the solvent according to the mol ratio of 1: 60-65 adding an alcohol solution (the alcohol solution is obtained by mixing deionized water and isoamylol according to the molar ratio of 1: 1), and then preserving heat for 6-8h at 180 +/-10 ℃;
(3) and (3) mechanically stirring and hydrolyzing the substance obtained after heat preservation in the step (2) at 95 ℃ for 4h, adding glacial acetic acid which is an auxiliary agent and has the mass of 1% of that of the substance obtained after hydrolysis, and preserving the heat at 180 ℃ for 4-6h to obtain the pseudo-boehmite product with the pore volume of 1.30cc/g and the purity of 99.999% and with multiple pores and wide distribution, wherein the mixed solution is a mixed solution of alcohol and deionized water and the alcohol content is 95%.
The pore distribution of the product prepared by the invention measured by a BET method is shown in figures 1 and 2, and the pore absorption and desorption graphs are shown in figures 1 and 2, and the pore size distribution is distributed from 2nm to 300nm, particularly is most widely distributed between 2nm to 4nm and 10 nm to 30nm as can be seen from the nitrogen absorption and desorption curves in figures 1 and 2. The prepared powder has the catalyst carrier performance with both small and medium pore volume and large pore volume, and can meet the requirements of novel catalyst carriers developed by some special processes. And the large pore volume product developed by the process is stable between 1.1 cc/g and 1.3cc/g, has large pore volume and high colloid strength, is not easy to collapse when meeting acid, and solves the problems that the large pore volume product prepared by the prior alkoxide method is rarely more than 1.0cc/g, and the collapse of the pore channel is reduced to medium and small pore channels when meeting acid.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (6)
1. A method for preparing pseudoboehmite with large pore volume, multiple pore paths and wide distribution is characterized by comprising the following operation steps:
(1) reacting 2N-5N aluminum raw material with alcohol at 83-84 ℃ for 6-10h under the catalysis of mercuric chloride or aluminum chloride to obtain aluminum alkoxide, and preserving heat at 100-180 ℃ for 5-12 h;
(2) distilling and purifying the substance obtained after the heat preservation in the step (1) at the temperature of 160-200 ℃ for 10-16h, transferring the aluminum alkoxide obtained after the purification to a hydrolysis reaction kettle, simultaneously adding 1-8 per mill of nano-boehmite seed crystals according to the mass percentage, adding an alcohol solution according to the molar ratio of the aluminum alkoxide to the alcohol solution of 1:20-65, and preserving the heat at the temperature of 60-240 ℃ for 2-24 h;
(3) hydrolyzing the substance obtained in the step (2) at 65-95 ℃ for 4-12h, adding 0.3-1% of an auxiliary agent, and keeping the temperature at 60-240 ℃ for 2-24h to obtain a pseudo-boehmite product with large pore volume, multiple pore channels and wide distribution; the auxiliary agent is one or a mixture of two of nitric acid, hydrochloric acid, citric acid, glacial acetic acid, hydrogen peroxide, water glass, silicate, oleic acid, urea, ammonia, lauryl alcohol or dodecane lipid.
2. The method of claim 1, wherein: the aluminum raw material in the step (1) is one of an aluminum sheet, an aluminum block or aluminum particles.
3. The method of claim 1, wherein: and (2) reacting the 3N aluminum raw material and alcohol in the step (1) under the catalysis of mercuric chloride or aluminum chloride.
4. The method of claim 1, wherein: the alcohol in the step (1) is one of isopropanol, n-butanol, isobutanol, n-pentanol and isoamylol.
5. The method of claim 1, wherein: the alcoholic solution in the step (2) is a mixture of water and alcohol with the molar ratio of 1: 1-6, wherein the alcohol is one of isopropanol, n-butanol, isobutanol, n-pentanol and isoamylol.
6. The method of claim 1, wherein: the nano diaspore seed crystal is added in the step (2) and is diaspore raw powder with the crystallinity of 75-80 percent, and the grain size is 10-50 nanometers.
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| CN111689507B (en) * | 2020-06-23 | 2022-11-08 | 萍乡市华顺环保化工填料有限公司 | Automatic production line for chemical raw material carriers and adsorbents |
| CN113998721B (en) * | 2020-07-27 | 2023-05-05 | 中国石油化工股份有限公司 | Preparation method of macroporous alumina |
| CN112062145B (en) * | 2020-09-09 | 2021-09-10 | 中国科学院过程工程研究所 | Alumina and preparation method and application thereof |
| CN113149050B (en) * | 2021-04-13 | 2022-10-11 | 新疆众和股份有限公司 | Method for treating solid waste in high-purity alcohol aluminum salt industry |
| CN113666402B (en) * | 2021-08-13 | 2022-07-08 | 吉林大学 | Hydroxy aluminum oxide nano material and preparation method thereof |
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