CN111268691A - Small-grain chabazite as well as preparation method and application thereof - Google Patents
Small-grain chabazite as well as preparation method and application thereof Download PDFInfo
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- CN111268691A CN111268691A CN202010168074.1A CN202010168074A CN111268691A CN 111268691 A CN111268691 A CN 111268691A CN 202010168074 A CN202010168074 A CN 202010168074A CN 111268691 A CN111268691 A CN 111268691A
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- chabazite
- sodium
- small
- water
- sodium silicate
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- UNYSKUBLZGJSLV-UHFFFAOYSA-L calcium;1,3,5,2,4,6$l^{2}-trioxadisilaluminane 2,4-dioxide;dihydroxide;hexahydrate Chemical compound O.O.O.O.O.O.[OH-].[OH-].[Ca+2].O=[Si]1O[Al]O[Si](=O)O1.O=[Si]1O[Al]O[Si](=O)O1 UNYSKUBLZGJSLV-UHFFFAOYSA-L 0.000 title claims abstract description 38
- 229910052676 chabazite Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- 239000013078 crystal Substances 0.000 claims abstract description 15
- 239000002253 acid Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000002274 desiccant Substances 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 30
- 239000004115 Sodium Silicate Substances 0.000 claims description 30
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 30
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 30
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 22
- 239000011734 sodium Substances 0.000 claims description 22
- 229910052708 sodium Inorganic materials 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 15
- 238000003786 synthesis reaction Methods 0.000 claims description 11
- 230000015572 biosynthetic process Effects 0.000 claims description 10
- 238000002425 crystallisation Methods 0.000 claims description 8
- 230000008025 crystallization Effects 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 5
- 238000005216 hydrothermal crystallization Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000004913 activation Effects 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 claims 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 13
- 239000003463 adsorbent Substances 0.000 abstract description 6
- 239000010457 zeolite Substances 0.000 abstract description 6
- 229920006395 saturated elastomer Polymers 0.000 abstract description 5
- 229910021536 Zeolite Inorganic materials 0.000 abstract description 4
- 230000018044 dehydration Effects 0.000 abstract description 4
- 238000006297 dehydration reaction Methods 0.000 abstract description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000006096 absorbing agent Substances 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
-
- 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
Abstract
The invention belongs to the technical field of zeolite, and particularly relates to small-grain chabazite as well as a preparation method and application thereof. The chabazite is obtained by using a crystal directing agent and adopting a hydrothermal synthesis method without an organic template, and the grain size is 200-600 nm. The adsorbent is used as a dehydration drying agent in a strong acid system, and good results are obtained, and the adsorption quantity of saturated water is up to 15 percent after the adsorbent is soaked in a 10 percent hydrochloric acid solution for 3 days.
Description
Technical Field
The invention belongs to the technical field of zeolite, and particularly relates to small-grain chabazite as well as a preparation method and application thereof.
Background
The researches on the synthesis and the properties of chabazite are not much at home and abroad, and the reports on the literature are less, which are related to the properties and the characteristics of the chabazite. Compared with common and common zeolites such as 4A, 13X and the like, chabazite has inferior adsorption capacity to small molecules such as water, carbon dioxide and the like, and organic amine (tetramethylamine) is used as a template agent, so that the synthesis difficulty and the cost are far higher than those of the common and common zeolites. Of course chabazite is a notable feature: the stability of the three-dimensional pore structure of the framework can be maintained under a strong acid environment, so that the strong adsorption capacity of the framework on small molecules such as water, carbon dioxide and the like is maintained. This is not possessed by 4A, 13X zeolite and the like. The natural chabazite ore is not available at home, and is rare at abroad. It was found that it is associated with other types of zeolite deposits and has low purity and low grade. Therefore, the product made from the natural chabazite ore has general performance, and the quality fluctuates with uncertain factors such as the type, purity and the like of the associated ore. The product made of artificially synthesized chabazite has the advantages of no problem of natural ore, stable performance and higher price.
The main industrial application of chabazite is as adsorbent and catalyst under strong acidic working condition. In many fine chemical synthesis (drug synthesis, pesticide synthesis, synthesis of vinyl chloride and polyvinyl chloride) and semiconductor polysilicon production, strong acid gases involved in the reaction, such as hydrogen chloride, hydrogen fluoride and the like, need to be dehydrated and dried before being introduced into a synthesis system to participate in the chemical reaction. Compared with the traditional concentrated sulfuric acid dehydrating agent, the chabazite adsorbent is safe and environment-friendly. And because the water-absorbing agent is solid particles, the water-absorbing agent is convenient to operate and safe to use, can be repeatedly used after being regenerated after absorbing water, and has a long service life and low use cost. These advantages are particularly important when environmental protection requirements are becoming stricter.
The invention utilizes the crystallization guiding agent, adopts the method without an organic template to synthesize the small-grain chabazite, and uses the small-grain chabazite for dehydration and drying in a strong acid system to obtain better results.
Disclosure of Invention
The invention aims to provide a synthetic method and application of small-grain chabazite.
The small-grain chabazite provided by the invention is obtained by a crystal directing agent and a hydrothermal synthesis method without an organic template, and the grain size is 200-600 nm. The obtained small-grain chabazite is used for dehydration and drying in a strong acid system, and a better result is obtained.
The synthesis method of the small-grain chabazite comprises the following specific steps:
(1) synthesis of crystal directing agent
Dissolving a certain amount of sodium silicate, potassium hydroxide and sodium metaaluminate in water at the temperature of 10-90 ℃, stirring for 4-10h to obtain a crystal directing agent, and storing the crystal directing agent at 10-30 ℃;
(2) synthesis of small crystal grain chabazite by hydrothermal crystallization method
Under the condition of room temperature and stirring, dissolving a certain amount of sodium silicate, sodium hydroxide and sodium metaaluminate in water, adding a certain amount of crystallization directing agent, uniformly stirring, placing into a hydrothermal kettle, crystallizing at 90-110 ℃ for 1-2 days, then crystallizing at 130-160 ℃ for 1-3 days, filtering, washing and drying to obtain the small-grain chabazite.
In the step (1), the molar ratio of the potassium hydroxide to the sodium silicate is 0.05:1-0.13: 1;
in the step (1), the molar ratio of water to sodium silicate is 20:1-60: 1;
in the step (1), the molar ratio of sodium silicate to sodium metaaluminate is 1.5:1-4: 1;
in the step (2), the molar ratio of the sodium hydroxide to the sodium silicate is 0.04:1-0.3: 1;
in the step (2), the molar ratio of water to sodium silicate is 50:1-100: 1;
in the step (2), the molar ratio of the sodium silicate to the sodium metaaluminate is 1.5:1-4: 1;
in the step (2), the dosage of the crystallization guiding agent is 10-20% of the total dosage (mass) of the sodium silicate, the sodium hydroxide, the sodium metaaluminate and the water.
The small-grain chabazite obtained by the invention is used as a drying agent in a strong acid system.
Specifically, the water absorption is measured after soaking in 5% -15% hydrochloric acid for 2-4 days, washing with water, and activating at 400 ℃ for 2 h.
In the invention, the small-grain chabazite is synthesized by a hydrothermal method without an organic template agent, so that the price is low. In addition, the adsorbent is used as a dehydration drying agent in a strong acid system, and good results are obtained, and after the adsorbent is soaked in a 10% hydrochloric acid solution for 3 days, the adsorption amount of saturated water is up to 15%. After absorbing water, the drying agent is heated or activated in vacuum to remove the absorbed water and then is recycled; has good economic operability and obvious environmental protection benefit and social benefit.
Detailed Description
The invention is further illustrated by the following examples.
Example 1
Dissolving a certain amount of sodium silicate, potassium hydroxide and sodium metaaluminate in water at 30 ℃, wherein the molar ratio of the potassium hydroxide to the sodium silicate to the sodium metaaluminate to the water is 0.07:1:0.5:30, stirring for 6 hours to obtain a crystal directing agent, and storing the crystal directing agent at 30 ℃.
Under the condition of room temperature and stirring, dissolving a certain amount of sodium silicate, sodium hydroxide and sodium metaaluminate in water, adding 10% of a crystallization directing agent, wherein the molar ratio of the sodium hydroxide to the sodium silicate to the sodium metaaluminate to the water is 0.2:1:0.5:70, uniformly stirring, putting into a hydrothermal kettle, crystallizing at 100 ℃ for 1 day, then crystallizing at 130 ℃ for 3 days, filtering, washing and drying to obtain the chabazite. The chabazite is soaked in 10% hydrochloric acid for 3 days, washed with water, activated at 400 deg.C for 2h, and the saturated water absorption is measured, with absorption of 15%.
Example 2
Dissolving a certain amount of sodium silicate, potassium hydroxide and sodium metaaluminate in water at 50 ℃, wherein the molar ratio of the potassium hydroxide to the sodium silicate to the sodium metaaluminate to the water is 0.08:1:0.4:30, stirring for 5 hours to obtain a crystal directing agent, and storing the crystal directing agent at 30 ℃.
Under the condition of room temperature and stirring, dissolving a certain amount of sodium silicate, sodium hydroxide and sodium metaaluminate in water, adding 12% of crystallization directing agent, wherein the molar ratio of the sodium hydroxide to the sodium silicate to the sodium metaaluminate to the water is 0.3:1:0.3:60, uniformly stirring, putting into a hydrothermal kettle, crystallizing at 110 ℃ for 1 day, then crystallizing at 140 ℃ for 3 days, filtering, washing and drying to obtain the chabazite. The chabazite is soaked in 12% hydrochloric acid for 3 days, washed with water, activated at 400 deg.C for 2h, and the saturated water absorption is determined, with absorption of 14%.
Example 3
Dissolving a certain amount of sodium silicate, potassium hydroxide and sodium metaaluminate in water at 60 ℃, wherein the molar ratio of the potassium hydroxide to the sodium silicate to the sodium metaaluminate to the water is 0.06:1:0.3:40, stirring for 7 hours to obtain a crystal directing agent, and storing the crystal directing agent at 30 ℃.
Under the condition of room temperature and stirring, dissolving a certain amount of sodium silicate, sodium hydroxide and sodium metaaluminate in water, adding 15% of a crystallization directing agent, wherein the molar ratio of the sodium hydroxide to the sodium silicate to the sodium metaaluminate to the water is 0.15:1:0.4:80, uniformly stirring, putting into a hydrothermal kettle, crystallizing at 100 ℃ for 1 day, then crystallizing at 150 ℃ for 3 days, filtering, washing and drying to obtain the chabazite. After immersing chabazite in 9% hydrochloric acid for 3 days, washing with water, activating at 400 deg.C for 2h, and measuring its saturated water absorption with absorption of 14%.
Claims (6)
1. The preparation method of the small-grain chabazite is characterized by comprising the following specific steps of:
(1) synthesis of crystal directing agent
Dissolving sodium silicate, potassium hydroxide and sodium metaaluminate in water at 10-90 deg.C, stirring for 4-10 hr to obtain crystal directing agent, and storing at 10-30 deg.C;
(2) synthesis of small crystal grain chabazite by hydrothermal crystallization method
Under the condition of room temperature and stirring, dissolving sodium silicate, sodium hydroxide and sodium metaaluminate in water, adding a crystallization guiding agent, uniformly stirring, placing into a hydrothermal kettle, crystallizing at 90-110 ℃ for 1-2 days, then crystallizing at 130-160 ℃ for 1-3 days, filtering, washing and drying to obtain small-grain chabazite; the grain size is 200-600 nm.
2. The method for preparing small-grained chabazite according to claim 1, characterized in that in step (1), the molar ratio of potassium hydroxide to sodium silicate is (0.05-0.13): 1; the molar ratio of water to sodium silicate is (20-60) to 1; the molar ratio of the sodium silicate to the sodium metaaluminate is (1.5-4) to 1.
3. The method for preparing small-grained chabazite according to claim 2, wherein in step (2), the molar ratio of sodium hydroxide to sodium silicate is (0.04-0.3): 1; the molar ratio of water to sodium silicate is (50-100) to 1; the molar ratio of the sodium silicate to the sodium metaaluminate is (1.5-4) to 1; the dosage of the crystallization guiding agent is 10-20% of the total dosage of the sodium silicate, the sodium hydroxide, the sodium metaaluminate and the water.
4. A small grained chabazite obtained by the method of manufacture according to any one of claims 1 to 3.
5. Use of the small grained chabazite according to claim 4 as a drying agent in a strong acid system.
6. The use of small grain chabazite as a drying agent in a strong acid system according to claim 5, wherein said drying agent is capable of being recycled after absorbing water and removing the absorbed water by heating or vacuum activation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010168074.1A CN111268691A (en) | 2020-03-12 | 2020-03-12 | Small-grain chabazite as well as preparation method and application thereof |
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| CN202010168074.1A CN111268691A (en) | 2020-03-12 | 2020-03-12 | Small-grain chabazite as well as preparation method and application thereof |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86108824A (en) * | 1985-12-12 | 1987-07-22 | 联合碳化公司 | Adopt the drying means of Chabazite-type adsorbent |
| US20030069449A1 (en) * | 2001-08-30 | 2003-04-10 | Zones Stacey I. | Small crystallite zeolite CHA |
| CN101254928A (en) * | 2007-02-28 | 2008-09-03 | 中国石油化工股份有限公司 | Method for preparing fine-grain low silica alumina ratio X zeolite |
| JP2010168269A (en) * | 2008-12-22 | 2010-08-05 | Tosoh Corp | Chabazite-type zeolite and method for producing the same |
| CN102285666A (en) * | 2010-06-18 | 2011-12-21 | 江西师范大学 | Method for preparing chabazite and chabazite film |
| JP2013173624A (en) * | 2012-02-23 | 2013-09-05 | Tosoh Corp | Microcrystal chabazite type zeolite, method for producing the same, and application thereof |
| CN103561865A (en) * | 2011-04-18 | 2014-02-05 | Pq公司 | Large crystal, organic-free chabazite, methods of making and using the same |
| JP2017014100A (en) * | 2015-06-29 | 2017-01-19 | 日揮触媒化成株式会社 | Method for producing high silica chabazite-type zeolite and high silica chabazite-type zeolite |
| US20170107114A1 (en) * | 2015-10-20 | 2017-04-20 | Purdue Research Foundation | Methods of synthesizing chabazite zeolites with controlled aluminum distribution and structures made therefrom |
-
2020
- 2020-03-12 CN CN202010168074.1A patent/CN111268691A/en active Pending
Patent Citations (9)
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|---|---|---|---|---|
| CN86108824A (en) * | 1985-12-12 | 1987-07-22 | 联合碳化公司 | Adopt the drying means of Chabazite-type adsorbent |
| US20030069449A1 (en) * | 2001-08-30 | 2003-04-10 | Zones Stacey I. | Small crystallite zeolite CHA |
| CN101254928A (en) * | 2007-02-28 | 2008-09-03 | 中国石油化工股份有限公司 | Method for preparing fine-grain low silica alumina ratio X zeolite |
| JP2010168269A (en) * | 2008-12-22 | 2010-08-05 | Tosoh Corp | Chabazite-type zeolite and method for producing the same |
| CN102285666A (en) * | 2010-06-18 | 2011-12-21 | 江西师范大学 | Method for preparing chabazite and chabazite film |
| CN103561865A (en) * | 2011-04-18 | 2014-02-05 | Pq公司 | Large crystal, organic-free chabazite, methods of making and using the same |
| JP2013173624A (en) * | 2012-02-23 | 2013-09-05 | Tosoh Corp | Microcrystal chabazite type zeolite, method for producing the same, and application thereof |
| JP2017014100A (en) * | 2015-06-29 | 2017-01-19 | 日揮触媒化成株式会社 | Method for producing high silica chabazite-type zeolite and high silica chabazite-type zeolite |
| US20170107114A1 (en) * | 2015-10-20 | 2017-04-20 | Purdue Research Foundation | Methods of synthesizing chabazite zeolites with controlled aluminum distribution and structures made therefrom |
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