CN115784252B - Preparation method of mesoporous ZSM-5 molecular sieve - Google Patents
Preparation method of mesoporous ZSM-5 molecular sieve Download PDFInfo
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- CN115784252B CN115784252B CN202310053044.XA CN202310053044A CN115784252B CN 115784252 B CN115784252 B CN 115784252B CN 202310053044 A CN202310053044 A CN 202310053044A CN 115784252 B CN115784252 B CN 115784252B
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 65
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 34
- 230000002378 acidificating effect Effects 0.000 claims abstract description 23
- 150000003839 salts Chemical class 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- 239000003513 alkali Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 17
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims description 12
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 8
- 235000011056 potassium acetate Nutrition 0.000 claims description 6
- 239000001508 potassium citrate Substances 0.000 claims description 6
- 229960002635 potassium citrate Drugs 0.000 claims description 6
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 claims description 6
- 235000011082 potassium citrates Nutrition 0.000 claims description 6
- 150000007529 inorganic bases Chemical class 0.000 claims description 4
- 239000001632 sodium acetate Substances 0.000 claims description 4
- 235000017281 sodium acetate Nutrition 0.000 claims description 4
- 239000001509 sodium citrate Substances 0.000 claims description 4
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 4
- 235000011083 sodium citrates Nutrition 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 21
- 238000002715 modification method Methods 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 description 12
- 239000002994 raw material Substances 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 229940040526 anhydrous sodium acetate Drugs 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000004523 catalytic cracking Methods 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000013335 mesoporous material Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention relates to a preparation method of a mesoporous molecular sieve, which comprises the following steps: (1) Preparing an alkaline system solution mixed by inorganic alkali and weak acid salt; (2) Adding ZSM-5 molecular sieve into the alkaline system solution prepared in the step (1), and stirring at 25-95 ℃; (3) Filtering, washing and drying the sample prepared in the step (2); (4) Preparing an acidic system solution mixed by weak acid and weak acid salt, and keeping the pH value of the acidic system solution within the range of 2.0-6.0; (5) Adding the sample obtained in the step (3) into the acidic system solution prepared in the step (4) according to the solid-to-liquid ratio of 1-100, stirring at 25-95 ℃, filtering the obtained product, washing with water, and drying to obtain the product. The invention is an economic and efficient molecular sieve post-treatment modification method with high specific surface area and complete micropore structure.
Description
Technical Field
The invention relates to a modification method of a mesoporous molecular sieve, belongs to the field of molecular sieve modification, and in particular relates to a preparation method of a mesoporous ZSM-5 molecular sieve.
Background
The mesoporous ZSM-5 molecular sieve refers to a multi-level pore molecular sieve material with a secondary mesoporous system besides inherent microporous pore channels of the molecular sieve. The introduction of mesopores in the molecular sieve crystals improves the mass transfer rate of reactant or product molecules in the molecular sieve pore channels and increases the number of accessible pores. For the molecules reacting in the micropore canal, the diffusion path length of the guest molecules in the molecular sieve canal is shortened, and the mass transfer rate is improved. For the reaction involving macromolecules, the microporous molecular sieve can only react on the orifice due to the problem of pore canal size limitation, and the mesoporous is introduced into the microporous molecular sieve to expose a large number of active centers on the outer surface of the molecular sieve, so that the accessibility of acid sites on the surface of the molecular sieve is increased, and the effective utilization rate of the active sites is improved. The existence of mesopores in the molecular sieve crystal can make up the defect of the microporous molecular sieve in diffusion restriction, and provides a proper space structure for macromolecular reaction.
Appl catalyst (2001, 219:33-43) forms a relatively regular mesoporous structure in a molecular sieve crystal by selectively removing silicon element in a molecular sieve framework by alkali, and the specific surface area of the mesoporous after modification is from 7m 2 Increase/g to 115m 2 Per gram, the specific surface area of the micropores is from 296m 2 The/g is reduced to 205m 2 And/g. Although the micropore specific surface area remains more, the mesopore content is also lower.
The mesoporous specific surface area of the sample obtained by the patent CN104229824A is only 170m 2 About/g, the total specific surface area is only 410m 2 About/g.
ZSM-5 molecular sieve prepared by patent CN101428817A has mesoporous specific surface up to 217m 2 About/g, the specific surface area of micropores is severely destroyed, but is only 141m 2 And/g, which greatly reduces the reactivity of the molecular sieve.
Patent CN104628011a obtains a maximum of 225m 2 The mesoporous specific surface area per gram is at most 474m 2 /g。
The mesoporous specific surface area of the patent CN102464336A can reach 300m at most 2 Per g, the micropore specific surface area of which can be at least 220m 2 Per g, the pore diameter is only about 3.5 nm.
At present, reported documents and patents related to ZSM-5 molecular sieve aftertreatment mainly use alkali to destroy the framework structure of the ZSM-5 molecular sieve to manufacture mesopores, improve the specific surface area of the mesopores, and enlarge the pore diameter of the ZSM-5 molecular sieve, thereby improving the diffusion of substances in molecular sieve crystals and achieving the purpose of improving the catalytic performance. However, the prior art has serious damage to the crystal structure in the alkali treatment process, and the result is that a great deal of micropores are inevitably lost, so that the reactive center of zeolite is reduced. And the surface of the molecular sieve is enriched with a large amount of extra-framework aluminum species, so that carbon deposition is easy to generate in catalytic cracking, the application of the molecular sieve in the catalytic cracking process is limited, the specific surface area is too low, and the catalytic activity of the molecular sieve is seriously reduced. At present, a ZSM-5 molecular sieve material with a Gao Jiekong specific surface area and a complete micropore structure has yet to be developed.
Disclosure of Invention
The invention aims to provide a preparation method of a mesoporous ZSM-5 molecular sieve. Aiming at the problems of serious damage to the crystal structure, low specific surface area of micropores and low catalytic activity in the prior art, the method for post-treatment modification of the molecular sieve is economical, efficient, high in specific surface area and complete in micropore structure.
The preparation method of the mesoporous ZSM-5 molecular sieve provided by the invention comprises the following steps:
(1) Preparing an alkaline system solution mixed by inorganic alkali and weak acid salt, and keeping the pH value of the alkaline system solution within the range of 7.0-10.0;
(2) Adding ZSM-5 molecular sieve into the alkaline system solution prepared in the step (1) according to the solid-to-liquid ratio of 1-15, and stirring for 60-360 min at 25-95 ℃;
(3) Filtering, washing and drying the sample prepared in the step (2);
(4) Preparing an acidic system solution mixed by weak acid and weak acid salt, and keeping the pH value of the acidic system solution within the range of 2.0-6.0;
(5) Adding the sample obtained in the step (3) into the acidic system solution prepared in the step (4) according to the solid-to-liquid ratio of 1-100, stirring for 60-600 min at 25-95 ℃, filtering, washing and drying the obtained product to obtain the modified mesoporous ZSM-5 molecular sieve.
The ZSM-5 molecular sieve used in the invention is a ZSM-5 molecular sieve which does not contain mesopores and is used as a raw material, and the product is a ZSM-5 molecular sieve which is rich in mesopores.
The inorganic alkali in the alkaline system solution in the step (1) is one or two of sodium hydroxide or potassium hydroxide; the weak acid salt is one or more of sodium acetate, potassium acetate or potassium citrate.
The molar ratio of the weak acid salt to the inorganic base in the alkaline system solution in the step (1) is 1-10.
The molar ratio of the weak acid salt to the inorganic base in the alkaline system solution in the step (1) is 3-6.
The alkaline system solution preferably has a pH of 8.0 to 9.0.
The ZSM-5 molecular sieve in the step (2) is added into the alkaline system solution prepared in the step (1), and the solid-liquid ratio is 1-15, preferably 8-10.
The temperature of stirring the ZSM-5 molecular sieve in the step (2) after adding the alkaline system solution is 25-95 ℃, preferably 55-85 ℃; the stirring time is 60min-360min, preferably 90min-240min.
The weak acid in the acidic system solution in the step (4) is one or two of acetic acid and citric acid; the weak acid salt is one or more of sodium acetate, sodium citrate, potassium acetate or potassium citrate.
The pH of the acidic system solution is in the range of 2.0-6.0, preferably 3.0-4.0.
The molar ratio of the weak acid salt to the weak acid in the acidic system solution in the step (4) is 1-5.
The molar ratio of weak acid salt to weak acid in the acidic system solution in step (4) is preferably 2 to 3.
In the step (5), the sample obtained in the step (3) is added to the acidic system solution prepared in the step (4), and the solid-to-liquid ratio is 1-100, preferably 40-80.
In the step (5), the sample obtained in the step (3) is added into the acid system solution prepared in the step (4) to be stirred, wherein the stirring temperature is 25-95 ℃, preferably 55-85 ℃; the stirring time is 60min-600min, preferably 240min-480min.
Compared with the prior art, the invention has the following beneficial effects:
the mesoporous is generated by simply destroying the micropore structure of the molecular sieve by means of the inorganic alkali solution environment, so that a great deal of micropore loss is necessarily caused, and the reactive center of the molecular sieve is reduced. However, the treatment method provided by the invention is carried out in an alkaline system solution prepared by inorganic alkali and weak acid salt. In the alkali treatment process of the molecular sieve, free weak acid roots can promote the generation of a mesoporous structure and can play a certain role in stabilizing and protecting the microporous structure; the subsequent acid treatment process is carried out in an acidic system solution prepared by weak acid and weak acid salt, and amorphous aluminum in the molecular sieve crystal is eluted, so that the purposes of loosening pore channels and increasing the total specific surface area are achieved. Therefore, the mesoporous ZSM-5 molecular sieve prepared by the invention has outstanding specific surface area and unique structure.
The mesoporous size of the product obtained by the invention is more than 25% larger than that of the product obtained by the invention in patent CN102874840A, and the mesoporous volume is more than 28% larger than that of the product obtained by the invention in patent CN 104628011A. The aperture of the product is more than 42% larger than that of patent CN 102464336A. The mesoporous material has more complete micropores while providing a higher-quality mesoporous product, and the preparation raw materials are cheap and easy to obtain, so that the mesoporous material is suitable for large-scale industrial production.
Drawings
FIG. 1 is an XRD spectrum of a mesoporous ZSM-5 molecular sieve obtained in example 1.
FIG. 2 is a pore size distribution diagram of the mesoporous ZSM-5 molecular sieve obtained in example 1.
FIG. 3 is a drawing showing the adsorption/desorption of the mesoporous ZSM-5 molecular sieve obtained in example 1.
Detailed Description
The present invention will be further illustrated by the following examples, but the present invention is not limited to the following examples.
The raw material ZSM-5 molecular sieve used in the following example has a silica-alumina ratio of 27.5 and a specific surface area of 354m 2 Per g, micropore specific surface area 349m 2 /g, mesoporous specific surface area 5m 2 And/g. The acids, bases and solvents used were all analytical and analytical reagents.
Example 1
10mL of 0.1mol/L NaOH solution, 600mL of deionized water and 2.46g of anhydrous sodium acetate are added into a 2000mL beaker, the temperature of the solution is raised to 60 ℃ in a water bath to obtain an alkaline system solution with the pH value of 10, 60.0g of ZSM-5 molecular sieve raw material is then added, the solution is treated in the water bath for 2 hours, the solution is filtered after being quickly cooled to room temperature, washed to be neutral, and the solution is placed into an oven for drying at 120 ℃ for 12 hours. Adding 1500mL of 0.1mol/L acetic acid solution and 12.3g of anhydrous sodium acetate into a 2000mL beaker, heating the solution to 70 ℃ in a water bath to obtain an acidic system solution with the pH value of 6.0, taking 20.0g of dried sample, placing the dried sample into the beaker, keeping the temperature at 70 ℃ for 6 hours, rapidly cooling, filtering, washing, placing the sample into an oven, and drying the sample at 120 ℃ for 12 hours to obtain a sample number A1.
Example 2
Adding 5mL of 0.1mol/L NaOH solution, 600mL of deionized water and 1.41g of anhydrous sodium acetate into a 2000mL beaker, heating in a water bath to 60 ℃ to obtain an alkaline system solution with a pH value of 9, adding 60.0g of ZSM-5 molecular sieve raw material, treating in the water bath for 2h, quickly cooling to room temperature, filtering, washing to neutrality, and drying in an oven at 120 ℃ for 12h; adding 1500mL of 0.05mol/L acetic acid solution and 6.75g of anhydrous sodium acetate into a 2000mL beaker, heating the solution to 70 ℃ in a water bath to obtain an acidic system solution with the pH value of 5.0, taking 20g of dried sample, placing the sample into the beaker, keeping the temperature at 70 ℃ for 4 hours, rapidly cooling, filtering, washing, placing the sample into an oven, and drying the sample at 120 ℃ for 12 hours to obtain a sample number A2.
Example 3
Adding 10mL of 0.1mol/L NaOH solution, 600mL of deionized water and 5.16g of sodium citrate into a 2000mL beaker, heating in a water bath to 60 ℃ to obtain an alkaline system solution with a pH value of 8, adding 60.0g of ZSM-5 molecular sieve raw material, performing water bath treatment for 3h, quickly cooling to room temperature, filtering, washing to neutrality, and drying in an oven at 120 ℃ for 12h; adding 1500mL of 0.1mol/L citric acid solution and 13.44g of sodium citrate into a 2000mL beaker, heating the water bath to 70 ℃ to obtain an acidic system solution with a pH value of 5.0, taking 20.0g of dried sample, placing the dried sample into the beaker, keeping the temperature at 70 ℃ for 8 hours, rapidly cooling, filtering, washing, placing the sample into an oven, and drying the sample at 120 ℃ for 12 hours to obtain a sample number A3.
Example 4
10mL of 0.1mol/L KOH solution, 600mL of deionized water and 5.16g of potassium citrate are added into a 2000mL beaker, an alkaline system solution with the pH value of 9 is obtained after the temperature is raised to 60 ℃ in a water bath, 60.0g of ZSM-5 molecular sieve raw material is added, the water bath is processed for 3 hours, the temperature is quickly lowered to room temperature, the filtration is carried out, the washing is carried out until the solution is neutral, and the solution is placed into an oven for drying at 120 ℃ for 12 hours. Adding 1500mL of 0.05mol/L citric acid solution and 7.13g of potassium citrate into a 2000mL beaker, heating the solution to 70 ℃ in a water bath to obtain an acidic system solution with the pH value of 4.0, taking 20.0g of dried sample, placing the dried sample into the beaker, keeping the temperature at 70 ℃ for 6 hours, rapidly cooling, filtering, washing, placing the sample into an oven, and drying the sample at 120 ℃ for 12 hours to obtain a sample number A4.
Example 5
10mL of 0.1mol/L KOH solution, 600mL of deionized water and 2.94g of anhydrous potassium acetate are added into a 2000mL beaker, the temperature is raised to 60 ℃ in a water bath to obtain an alkaline system solution with the pH value of 8, 60.0g of ZSM-5 molecular sieve raw material is added, the water bath treatment is carried out for 3 hours, the filtration is carried out after the rapid cooling to the room temperature, the washing is carried out to neutrality, and the alkaline system solution is placed into an oven for drying at 120 ℃ for 12 hours. 1500mL of 0.1mol/L acetic acid solution and 13.03g of anhydrous potassium acetate are added into a 2000mL beaker, the temperature is raised to 70 ℃ in a water bath to obtain an acidic system solution with the pH value of 5.0, then 20.0g of dried sample is taken and put into the beaker, the temperature is kept constant for 6 hours at 70 ℃, the temperature is quickly reduced, the filtration and the washing are carried out, and the sample is dried for 12 hours at 120 ℃ in an oven to obtain a sample with the sample number A5.
The pore structure properties of the ZSM-5 modified zeolite samples prepared in examples 1-5 are shown in Table 1.
TABLE 1 pore structure Properties of the samples involved in examples 1-5
The mesoporous size of the products obtained in examples 1-5 is more than 25% larger than that of patent CN102874840A, and the mesoporous volume is more than 28% larger than that of patent CN 104628011A.
The products obtained in examples 1-5 were more than 42% larger than the pore size of patent CN102464336 a.
Claims (7)
1. A preparation method of a mesoporous ZSM-5 molecular sieve is characterized in that: the method is realized by the following steps:
(1) Preparing an alkaline system solution mixed by inorganic alkali and weak acid salt, and keeping the pH value of the alkaline system solution within the range of 7.0-10.0;
(2) Adding ZSM-5 molecular sieve into the alkaline system solution prepared in the step (1) according to the solid-to-liquid ratio of 1-15, and stirring for 60-360 min at 25-95 ℃;
(3) Filtering, washing and drying the sample prepared in the step (2);
(4) Preparing an acidic system solution mixed by weak acid and weak acid salt, and keeping the pH value of the acidic system solution within the range of 2.0-6.0;
(5) Adding the sample obtained in the step (3) into the acidic system solution prepared in the step (4) according to the solid-to-liquid ratio of 1-100, stirring for 60-600 min at 25-95 ℃, filtering, washing and drying the obtained product to obtain the modified mesoporous ZSM-5 molecular sieve.
2. The method for preparing the mesoporous ZSM-5 molecular sieve according to claim 1, wherein the method comprises the following steps: the inorganic alkali in the alkaline system solution in the step (1) is one or two of sodium hydroxide or potassium hydroxide; the weak acid salt is one or more of sodium acetate, potassium acetate or potassium citrate.
3. The method for preparing the mesoporous ZSM-5 molecular sieve according to claim 1, wherein the method comprises the following steps: the molar ratio of the weak acid salt to the inorganic base in the alkaline system solution in the step (1) is 1-10.
4. The method for preparing the mesoporous ZSM-5 molecular sieve according to claim 3, wherein the method comprises the following steps: the molar ratio of the weak acid salt to the inorganic base in the alkaline system solution in the step (1) is 3-6.
5. The method for preparing the mesoporous ZSM-5 molecular sieve according to claim 1, wherein the method comprises the following steps: the weak acid in the acidic system solution in the step (4) is one or two of acetic acid and citric acid; the weak acid salt is one or more of sodium acetate, sodium citrate, potassium acetate or potassium citrate.
6. The method for preparing the mesoporous ZSM-5 molecular sieve according to claim 1 or 5, wherein: the molar ratio of the weak acid salt to the weak acid in the acidic system solution in the step (4) is 1-5.
7. The method for preparing the mesoporous ZSM-5 molecular sieve according to claim 1 or 5, wherein: the molar ratio of the weak acid salt to the weak acid in the acidic system solution in the step (4) is 2-3.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108654678A (en) * | 2018-05-31 | 2018-10-16 | 上海绿强新材料有限公司 | One type Fenton oxidation catalyst and its application |
| CN108927213A (en) * | 2018-06-26 | 2018-12-04 | 上海绿强新材料有限公司 | A kind of catalyst and preparation method thereof for preparing propylene by dehydrogenating propane |
| CN111375444A (en) * | 2018-12-27 | 2020-07-07 | 中国科学院广州能源研究所 | Core-shell iron-based catalyst for directly producing aromatic hydrocarbon from synthesis gas and preparation method and application thereof |
| CN112892582A (en) * | 2019-12-03 | 2021-06-04 | 中国石油化工股份有限公司 | Light gasoline cracking catalyst containing all-silicon three-hole spherical mesoporous composite material and preparation method and application thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108654678A (en) * | 2018-05-31 | 2018-10-16 | 上海绿强新材料有限公司 | One type Fenton oxidation catalyst and its application |
| CN108927213A (en) * | 2018-06-26 | 2018-12-04 | 上海绿强新材料有限公司 | A kind of catalyst and preparation method thereof for preparing propylene by dehydrogenating propane |
| CN111375444A (en) * | 2018-12-27 | 2020-07-07 | 中国科学院广州能源研究所 | Core-shell iron-based catalyst for directly producing aromatic hydrocarbon from synthesis gas and preparation method and application thereof |
| CN112892582A (en) * | 2019-12-03 | 2021-06-04 | 中国石油化工股份有限公司 | Light gasoline cracking catalyst containing all-silicon three-hole spherical mesoporous composite material and preparation method and application thereof |
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