CN112897548A - Production process of 4A zeolite - Google Patents
Production process of 4A zeolite Download PDFInfo
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- CN112897548A CN112897548A CN202110173778.2A CN202110173778A CN112897548A CN 112897548 A CN112897548 A CN 112897548A CN 202110173778 A CN202110173778 A CN 202110173778A CN 112897548 A CN112897548 A CN 112897548A
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- sodium hydroxide
- aluminum ash
- zeolite
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- 239000010457 zeolite Substances 0.000 title claims abstract description 35
- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 32
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 127
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 54
- 238000000034 method Methods 0.000 claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 17
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 13
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 13
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 13
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 abstract description 10
- 239000000243 solution Substances 0.000 description 58
- 238000010438 heat treatment Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910020489 SiO3 Inorganic materials 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000005995 Aluminium silicate Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- -1 aluminum Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910020453 SiO2+2NaOH Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910001610 cryolite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000005120 petroleum cracking Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/14—Type A
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention provides a production process of 4A zeolite, which comprises the following steps: reacting aluminum ash with a sodium hydroxide solution, and separating to obtain a solution A; reacting active SiO2Reacting with sodium hydroxide solution to obtain solution B; and (3) reacting the solution A with the solution B, filtering and drying to obtain a 4A zeolite product. The process takes the aluminum ash as a raw material, so that resources are effectively utilized, the cost is saved, and the environment is protected.
Description
Technical Field
The invention relates to the technical field of cryolite preparation, in particular to a production process of 4A zeolite.
Background
The 4A zeolite is a first artificial zeolite material with Na composition12Al12Si12O48·27H2O, belonging to a cubic system, and the aperture is about 0.4 nm. 4A zeolites have important applications in a number of fields: the washing product taking the 4A zeolite as the auxiliary agent has the characteristics of no phosphorus, no chemical pollution, no residue and strong dirt-removing power, and has very wide and important application in the washing industry; in the catalytic industry, 4A zeolitesWidely applied to petroleum cracking reaction; in the gas separation industry, 4A zeolites are used to prepare adsorbents for high purity gases.
The sources of raw materials for synthesizing the 4A zeolite currently mainly comprise two types: the chemical raw materials are mainly sodium silicate and sodium aluminate solution; the second is natural mineral raw materials, such as kaolin, bentonite, coal gangue, natural epidesmine and the like. The process for producing the 4A zeolite by the chemical raw material method is mature, but has high cost and poor economic benefit. The 4A zeolite synthesized by using kaolin has great environmental pollution because of discharging a large amount of alkaline slag. In addition, a large amount of aluminum ash containing fluorine and nitrogen is generated in the electrolytic aluminum production process, which is a great harm to the environment, and how to reasonably treat the aluminum ash is also an important problem to be solved.
Disclosure of Invention
The invention provides a production process of 4A zeolite, aiming at overcoming the defects in the prior art, and the process takes aluminum ash as a raw material, so that resources are effectively utilized, the cost is saved, and the environment is protected.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a production process of 4A zeolite, which comprises the following steps:
reacting aluminum ash with a sodium hydroxide solution, and separating to obtain a solution A;
reacting active SiO2Reacting with sodium hydroxide solution to obtain solution B;
and (3) reacting the solution A with the solution B, filtering and drying to obtain a 4A zeolite product.
Preferably, the aluminum ash is denitrified aluminum ash.
More preferably, the specific treatment process of the aluminum denitrogenation ash comprises the following steps: crushing the aluminum ash, then carrying out high-temperature oxygen treatment, and cooling to room temperature.
Preferably, the high temperature is 500-700 ℃, and the room temperature is 20-30 ℃.
Preferably, the treatment time is 2-3 h.
Preferably, the mass fraction of the sodium hydroxide solution is 10-20%.
Preferably, the mass ratio of the aluminum ash to the sodium hydroxide in the reaction of the aluminum ash and the sodium hydroxide solution is 1:2-1: 3.
Preferably, the temperature for the reaction of the aluminum ash and the sodium hydroxide solution is 70-90 ℃.
Preferably, the reaction time of the aluminum ash and the sodium hydroxide solution is 1-2 h.
Preferably, the active SiO2Reactive SiO in reaction with sodium hydroxide solution2The mass ratio of the sodium hydroxide to the sodium hydroxide is 1 (1-2).
Preferably, the active SiO2The temperature for reaction with the sodium hydroxide solution is 70-90 ℃.
Preferably, the active SiO2The reaction time with the sodium hydroxide solution is 1-2 h.
Preferably, the reaction temperature of the solution A and the solution B is 80-90 ℃.
Preferably, the reaction time of the solution A and the solution B is 1-3 h.
The invention has the beneficial effects that:
according to the production process of the 4A zeolite, the aluminum ash is used as a raw material, the 4A zeolite is prepared, and meanwhile, the aluminum ash is subjected to harmless treatment, so that the resource utilization of the secondary aluminum ash is realized, the process is cost-saving, the sewage amount is small, and the production process is environment-friendly.
The aluminum ash denitrification process has high denitrification rate, ensures that the generated aluminum oxide can be efficiently utilized, reduces the denitrification cost, and has simple operation and no pollution.
The aluminum ash contains various compounds such as aluminum, alumina, silicon dioxide and the like, and after the aluminum ash reacts with a sodium hydroxide solution, aluminum element exists in the form of meta-aluminate, wherein Na obtained by the reaction of the silicon dioxide and the sodium hydroxide2SiO3The amount of the solution B can be supplemented, the raw materials are saved, and the cost is reduced.
Drawings
FIG. 1 is a process flow diagram of the present invention
FIG. 2 is a flow chart of an embodiment of the process of the present invention
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, the present invention will be further described in detail with reference to the following embodiments.
In order to provide a production process of 4A zeolite, the process takes aluminum ash as a raw material, so that resources are effectively utilized, the cost is saved, and the environment is protected. The invention provides a production process of 4A zeolite, which comprises the following steps: reacting aluminum ash with a sodium hydroxide solution, and separating to obtain a solution A; reacting active SiO2Reacting with sodium hydroxide solution to obtain solution B; and (3) reacting the solution A with the solution B, filtering and drying to obtain a 4A zeolite product.
In the invention, the preferred aluminum ash is denitrified aluminum ash; the specific treatment process of the aluminum denitrogenation ash comprises the following steps: crushing the aluminum ash, then carrying out high-temperature oxygen treatment, and cooling to room temperature; the high temperature is 500-700 ℃, the treatment time is 2-3h, and the room temperature is 20-30 ℃. Under high temperature and aerobic environment, AlN in the aluminium ash and the oxygen in the air can take place oxidation reaction, if in the environment of fluoride, then the fluoride can play the effect of catalyst and accelerate the reaction, through long-time high temperature reaction, realizes aluminium ash denitrogenation, and the reaction formula is: 4AlN +3O2＝2Al2O3+2N2↑。
In the invention, the mass fraction of the sodium hydroxide solution is 10-20%; the mass ratio of the aluminum ash to the sodium hydroxide solution is 1:2-1: 3; the reaction temperature of the aluminum ash and the sodium hydroxide solution is 70-90 ℃; the reaction time is 1-2 h. The invention effectively removes nitrogen element in aluminum ash by denitrification, the aluminum ash contains various compounds such as aluminum, alumina, silicon dioxide and the like, and the aluminum element exists in the form of meta-aluminate after reacting with sodium hydroxide solution, wherein Na obtained by reacting the silicon dioxide with the sodium hydroxide2SiO3The amount of the solution B can be supplemented, the raw materials are saved, the cost is reduced, and the following reactions mainly occur:
2Al+2NaOH+H2O＝2NaAlO2+2H2↑；
Al2O3+2NaOH＝2NaAlO2+H2O；
SiO2+2NaOH＝Na2SiO3+H2O。
in the present invention, the active SiO2Reactive SiO in reaction with sodium hydroxide solution2The mass ratio of the sodium hydroxide to the sodium hydroxide is 1: 1-2; the active SiO2The temperature for reaction with sodium hydroxide solution is 70-90 ℃; the active SiO2The reaction time with the sodium hydroxide solution is 1-2 h.
In the invention, the reaction temperature of the solution A and the solution B is 80-90 ℃; the reaction time of the solution A and the solution B is 1-3 h. The reaction formula is as follows: 12Na2SiO3+12NaAlO2+39H2O＝ Na12Al12Si12O48·27H2O +24NaOH, and then filtering and drying.
In the present invention, the raw materials used are all those commercially available in the art unless otherwise specified.
The foregoing is a detailed description of the invention and the following is an example of the invention.
Example 1
Crushing the aluminum ash, putting the crushed aluminum ash into a heating furnace, introducing oxygen, adjusting the temperature of the heating furnace to 700 ℃, performing denitrification treatment for 2 hours, and cooling to 20 ℃ to obtain denitrified aluminum ash; reacting the denitrified aluminum ash with a sodium hydroxide solution with the mass fraction of 10% for 1h at 70 ℃ according to the mass ratio of 1:2, and separating to obtain a solution A; the active SiO2Reacting the mixed solution with a sodium hydroxide solution at a mass ratio of 1:1 at 70 ℃ for 1h to obtain a solution B; and (3) reacting the solution A with the solution B at the temperature of 80 ℃ for 3h, and filtering and drying to obtain a 4A zeolite product.
Example 2
Crushing the aluminum ash, putting the crushed aluminum ash into a heating furnace, introducing oxygen, adjusting the temperature of the heating furnace to be 500 ℃, performing denitrification treatment for 3 hours, and cooling to 30 ℃ to obtain denitrified aluminum ash; reacting the denitrified aluminum ash with a sodium hydroxide solution with the mass fraction of 20% for 2h at 90 ℃ according to the mass ratio of 1:3, and separating to obtain a solution A; the active SiO2Reacting with sodium hydroxide solution at the temperature of 90 ℃ for 2h according to the mass ratio of 1:2 to obtain solution B; the solution A and the solution B react for 1h at the temperature of 90 DEG CFiltering and drying to obtain the 4A zeolite product.
Example 3
Crushing the aluminum ash, putting the crushed aluminum ash into a heating furnace, introducing oxygen, adjusting the temperature of the heating furnace to 600 ℃, performing denitrification treatment for 2 hours, and cooling to 20 ℃ to obtain denitrified aluminum ash; reacting the denitrified aluminum ash with a sodium hydroxide solution with the mass fraction of 15% for 1h at the temperature of 80 ℃ according to the mass ratio of 1:2, and separating to obtain a solution A; the active SiO2Reacting with sodium hydroxide solution at the temperature of 80 ℃ for 1h according to the mass ratio of 1:1.5 to obtain solution B; and (3) reacting the solution A with the solution B at the temperature of 80 ℃ for 1h, filtering and drying to obtain a 4A zeolite product.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.
Claims (10)
1. A production process of 4A zeolite is characterized by comprising the following steps:
reacting aluminum ash with a sodium hydroxide solution, and separating to obtain a solution A;
reacting active SiO2Reacting with sodium hydroxide solution to obtain solution B;
and (3) reacting the solution A with the solution B, filtering and drying to obtain a 4A zeolite product.
2. The process for producing a 4A zeolite according to claim 1, wherein said aluminum ash is denitrified aluminum ash.
3. The process for producing 4A zeolite according to claim 2, wherein the specific treatment process of the denitrified aluminum ash comprises: crushing the aluminum ash, then carrying out high-temperature oxygen treatment, and cooling to room temperature.
4. The process for producing 4A zeolite as claimed in claim 3, wherein the elevated temperature is 500-700 ℃ and the room temperature is 20-30 ℃.
5. The process for producing a 4A zeolite according to claim 1, wherein the sodium hydroxide solution has a mass fraction of 10% to 20%.
6. The process for producing 4A zeolite according to claim 1, wherein the mass ratio of aluminum ash to sodium hydroxide in the reaction of aluminum ash and sodium hydroxide solution is 1:2 to 1: 3.
7. Process for the production of 4A zeolite according to claim 1, characterized in that the active SiO is2Reactive SiO in reaction with sodium hydroxide solution2The mass ratio of the sodium hydroxide to the sodium hydroxide is 1 (1-2).
8. Process for the production of 4A zeolite according to claim 1, characterized in that the active SiO is2The temperature for reaction with the sodium hydroxide solution is 70-90 ℃.
9. The process for producing 4A zeolite according to claim 1, wherein the reaction temperature of the solution A and the solution B is 80-90 ℃.
10. The process for producing 4A zeolite according to claim 1, wherein the reaction time of the solution A and the solution B is 1-3 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114014332A (en) * | 2021-11-03 | 2022-02-08 | 兰州理工大学 | Method for preparing 4A molecular sieve by using aluminum ash and micro silicon powder |
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| CN101905892A (en) * | 2010-08-13 | 2010-12-08 | 刘德华 | Process method for preparing 4A zeolite by recycling silica slag and aluminium slag |
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| CN111940460A (en) * | 2020-08-10 | 2020-11-17 | 南通大学 | Aluminum ash final ash low-temperature catalytic denitrification method |
| CN112279283A (en) * | 2020-10-29 | 2021-01-29 | 昆明理工大学 | Method for comprehensively utilizing secondary aluminum ash |
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2021
- 2021-02-06 CN CN202110173778.2A patent/CN112897548A/en active Pending
Patent Citations (4)
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| CN101905892A (en) * | 2010-08-13 | 2010-12-08 | 刘德华 | Process method for preparing 4A zeolite by recycling silica slag and aluminium slag |
| CN110548753A (en) * | 2019-09-30 | 2019-12-10 | 河南远润循环发展科技有限公司 | Efficient and clean secondary aluminum ash harmless treatment method |
| CN111940460A (en) * | 2020-08-10 | 2020-11-17 | 南通大学 | Aluminum ash final ash low-temperature catalytic denitrification method |
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| CN114014332A (en) * | 2021-11-03 | 2022-02-08 | 兰州理工大学 | Method for preparing 4A molecular sieve by using aluminum ash and micro silicon powder |
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