CN114768864A - Preparation method of metal modified TS-1 titanium silicalite molecular sieve CO catalyst - Google Patents
Preparation method of metal modified TS-1 titanium silicalite molecular sieve CO catalyst Download PDFInfo
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- CN114768864A CN114768864A CN202210427252.7A CN202210427252A CN114768864A CN 114768864 A CN114768864 A CN 114768864A CN 202210427252 A CN202210427252 A CN 202210427252A CN 114768864 A CN114768864 A CN 114768864A
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- titanium silicalite
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 36
- 239000002184 metal Substances 0.000 title claims abstract description 36
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 29
- 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 29
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000010936 titanium Substances 0.000 title claims abstract description 27
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 27
- 239000003426 co-catalyst Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011259 mixed solution Substances 0.000 claims abstract description 24
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000005342 ion exchange Methods 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 150000003839 salts Chemical class 0.000 claims abstract description 11
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 8
- BGQMOFGZRJUORO-UHFFFAOYSA-M tetrapropylammonium bromide Chemical compound [Br-].CCC[N+](CCC)(CCC)CCC BGQMOFGZRJUORO-UHFFFAOYSA-M 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- ZRBROGSAUIUIJE-UHFFFAOYSA-N azanium;azane;chloride Chemical compound N.[NH4+].[Cl-] ZRBROGSAUIUIJE-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005216 hydrothermal crystallization Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 238000002425 crystallisation Methods 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 4
- 239000012266 salt solution Substances 0.000 claims description 4
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 12
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 6
- 229910002091 carbon monoxide Inorganic materials 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 6
- 125000005842 heteroatom Chemical group 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 3
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 3
- FTXJFNVGIDRLEM-UHFFFAOYSA-N copper;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O FTXJFNVGIDRLEM-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/89—Silicates, aluminosilicates or borosilicates of titanium, zirconium or hafnium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/864—Removing carbon monoxide or hydrocarbons
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
- B01J2229/183—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself in framework positions
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biomedical Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Catalysts (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The embodiment of the invention provides a preparation method of a metal modified TS-1 titanium silicalite CO catalyst, which comprises the following steps: dissolving tetrapropyl ammonium bromide in deionized water to obtain a first mixed solution, and mixing a certain amount of butyl titanate and tetraethoxysilane to obtain a second mixed solution; dripping the second mixed solution into the first mixed solution to obtain gel; putting the gel into a reaction kettle, carrying out hydrothermal crystallization at a certain temperature for a period of time, and filtering, washing and drying to obtain a TS-1 precursor; dissolving metal salt in deionized water, adding a TS-1 precursor, adjusting the pH to 5-6 by using ammonium chloride-ammonia water, stirring at a certain temperature for ion exchange for a certain time, filtering, washing, drying, and roasting at 550 ℃ for 5 hours to obtain the metal modified TS-1 titanium silicalite molecular sieve CO catalyst. The invention can maintain the porous structure of the molecular sieve while adding new active sites, thereby being beneficial to improving the catalytic effect.
Description
Technical Field
The invention relates to the technical field of catalyst preparation, in particular to a preparation method of a metal modified TS-1 titanium silicalite molecular sieve CO catalyst.
Background
The titanium-silicon molecular sieve is a heteroatom molecular sieve, and is a novel catalytic material for embedding titanium atoms into a molecular sieve framework. The titanium silicalite molecular sieve has excellent catalytic activity and selectivity when used as a catalyst, and has wide application in fields of petrochemical industry, fine chemical industry and the like. It has been found that the introduction of different heteroatoms into the framework of a molecular sieve imparts catalytic properties to the molecular sieve for different reactions.
Aiming at carbon monoxide (CO) pollution, catalytic oxidation is a simple and effective solution. However, the existing carbon monoxide catalyst usually has a porous structure of a molecular sieve, but has the defects of insufficient active point positions, insufficient catalytic effect and the like.
Disclosure of Invention
The embodiment of the invention aims to provide a preparation method of a metal modified TS-1 titanium silicalite molecular sieve CO catalyst, which introduces framework heteroatoms by an ion exchange method, can increase new active sites and simultaneously keep the porous structure of the molecular sieve, and is beneficial to improving the catalytic effect.
The preparation method of the metal modified TS-1 titanium silicalite molecular sieve CO catalyst provided by the embodiment of the invention comprises the following steps:
s10: dissolving tetrapropylammonium bromide in deionized water at a certain temperature to obtain a first mixed solution, and mixing a certain amount of butyl titanate and tetraethoxysilane to obtain a second mixed solution;
s20: slowly dripping the second mixed solution into the first mixed solution, uniformly stirring to obtain gel, and regulating the pH value to be 10-11 by using sodium hydroxide in the dripping process;
s30: putting the gel into a reaction kettle, carrying out hydrothermal crystallization for a period of time at a certain temperature, filtering, washing and drying to obtain a TS-1 precursor;
s40: dissolving a certain amount of metal salt in deionized water, adding the TS-1 precursor, adjusting the pH to 5-6 by using ammonium chloride-ammonia water, stirring at a certain temperature for ion exchange for a certain time, filtering, washing, drying, and roasting at 550 ℃ for 5 hours to obtain the metal modified TS-1 titanium silicalite molecular sieve CO catalyst.
Preferably, the molar ratio of the ethyl orthosilicate to the butyl titanate to the tetrapropylammonium bromide to the deionized water is (1: 0.05) - (0.1: 0.2) - (1: 20) respectively.
Preferably, the crystallization temperature in S30 is 150-200 ℃, and the crystallization time is 24-72 h.
Preferably, the metal salt is a mixed salt of copper nitrate and manganese nitrate, and the molar ratio of the mixed salt to the manganese nitrate is 1 (1-5).
Preferably, the concentration of the salt solution after the metal salt is dissolved in the deionized water is 0.01-0.05 mol/L.
Preferably, in the S40, the ion exchange time is 1-5h, and the temperature is 60-80 ℃.
The beneficial effects of the invention are:
according to the preparation method of the metal modified TS-1 titanium silicalite CO catalyst provided by the embodiment of the invention, the gel prepared in advance is subjected to hydrothermal crystallization, a TS-1 precursor is obtained after filtration, washing and drying, then the TS-1 precursor is added into the prepared metal salt solution, stirring is carried out for ion exchange for a certain time, and the metal modified TS-1 titanium silicalite CO catalyst is obtained after filtration, washing, drying and roasting. The introduction of framework heteroatoms through an ion exchange method can maintain the porous structure of the molecular sieve while adding new active sites, thereby being beneficial to improving the catalytic effect.
In order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive efforts based on the embodiments of the present invention, are within the scope of protection of the present invention. Thus, the following detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention.
Wherein the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or to implicitly indicate the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Example 1
The preparation method of the metal modified TS-1 titanium silicalite molecular sieve CO catalyst provided by the embodiment of the invention mainly comprises the following steps:
step S10: dissolving 5g of tetrapropyl ammonium bromide in 50mL of deionized water at room temperature to obtain a first mixed solution; stirring and mixing 10mL of ethyl orthosilicate and 2mL of tetrabutyl titanate to obtain a second mixed solution.
Step S20: and slowly dripping the second mixed solution into the first mixed solution, and uniformly stirring to obtain the gel. The pH was kept at 10-11 during the addition with sodium hydroxide.
Step S30: and (3) putting the gel into a reaction kettle, crystallizing for 48 hours at 160 ℃, and performing suction filtration, washing and drying to obtain a TS-1 precursor.
Step S40: dissolving 0.28g of 50% manganese nitrate aqueous solution and 0.07g of copper nitrate hexahydrate in 100mL of deionized water, adding the obtained TS-1 precursor, adjusting the pH to 5-6 by using ammonium chloride-ammonia water, stirring in a water bath at 80 ℃ for ion exchange for 3 hours, filtering, washing, drying, and roasting at 550 ℃ for 5 hours to obtain the metal modified TS-1 titanium silicalite molecular sieve CO catalyst.
Example 2
The preparation method of the metal modified TS-1 titanium silicalite molecular sieve CO catalyst provided by the embodiment of the invention mainly comprises the following steps:
step S10: dissolving 5g of tetrapropyl ammonium bromide in 50mL of deionized water at room temperature to obtain a first mixed solution; stirring and mixing 10mL of ethyl orthosilicate and 1mL of tetrabutyl titanate to obtain a second mixed solution.
Step S20: and slowly dripping the second mixed solution into the first mixed solution, and uniformly stirring to obtain the gel. The pH was kept at 10-11 during the dropwise addition by adjusting with sodium hydroxide.
Step S30: and (3) putting the gel into a reaction kettle, crystallizing for 48 hours at 160 ℃, and performing suction filtration, washing and drying to obtain a TS-1 precursor.
Step S40: dissolving 0.5g of 50% manganese nitrate aqueous solution and 0.1g of copper nitrate hexahydrate in 100mL of deionized water, adding the obtained TS-1 precursor, adjusting the pH to 5-6 by using ammonium chloride-ammonia water, stirring in a water bath at 80 ℃ for ion exchange for 3 hours, filtering, washing, drying, and roasting at 550 ℃ for 5 hours to obtain the metal modified TS-1 titanium silicalite CO molecular sieve catalyst.
Example 3
The preparation method of the metal modified TS-1 titanium silicalite molecular sieve CO catalyst provided by the embodiment of the invention mainly comprises the following steps:
step S10: dissolving 5g of tetrapropyl ammonium bromide in 50mL of deionized water at room temperature to obtain a first mixed solution; stirring and mixing 10mL of ethyl orthosilicate and 2mL of tetrabutyl titanate to obtain a second mixed solution.
Step S20: and slowly dripping the second mixed solution into the first mixed solution, and uniformly stirring to obtain the gel. The pH was kept at 10-11 during the dropwise addition by adjusting with sodium hydroxide.
Step S30: and (3) putting the gel into a reaction kettle, crystallizing for 48 hours at 160 ℃, and performing suction filtration, washing and drying to obtain a TS-1 precursor.
Step S40: dissolving 0.8g of 50% manganese nitrate aqueous solution and 0.15g of copper nitrate hexahydrate in 100mL of deionized water, adding the obtained TS-1 precursor, adjusting the pH to 5-6 by using ammonium chloride-ammonia water, stirring in a water bath at 80 ℃ for ion exchange for 3 hours, filtering, washing, drying, and roasting at 550 ℃ for 5 hours to obtain the metal modified TS-1 titanium silicalite CO molecular sieve catalyst.
Evaluation examples
The metal modified TS-1 titanium silicalite molecular sieve CO catalysts prepared in the examples 1 to 3 were placed in fixed bed reactors, respectively, and their catalytic oxidation performance was tested.
The raw material gas contains CO with the concentration of 2000mg/Nm3Air (2) with test airspeed of 10000h-1The pressure is normal pressure. The test results are detailed in the following table.
| Catalyst and process for preparing same | Example 1 | Example 2 | Example 3 |
| Ignition temperature | 61℃ | 63℃ | 57℃ |
| Catalytic efficiency T98 | 86℃ | 91℃ | 82℃ |
As can be seen from the table, the metal modified TS-1 titanium silicalite molecular sieve CO catalyst prepared by the embodiment of the invention has better catalytic effect.
In summary, according to the preparation method of the metal modified TS-1 titanium silicalite CO catalyst provided by the embodiment of the present invention, a gel prepared in advance is subjected to hydrothermal crystallization, and is filtered, washed and dried to obtain a TS-1 precursor, and then the TS-1 precursor is added into a prepared metal salt solution, and is stirred to perform ion exchange for a certain time, and after filtering, washing, drying and roasting, the metal modified TS-1 titanium silicalite CO catalyst is obtained. The introduction of the framework heteroatom through the ion exchange method can maintain the porous structure of the molecular sieve while adding new active sites, thereby being beneficial to improving the catalytic effect.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A preparation method of a metal modified TS-1 titanium silicalite molecular sieve CO catalyst is characterized by comprising the following steps:
s10: dissolving tetrapropylammonium bromide in deionized water at a certain temperature to obtain a first mixed solution, and mixing a certain amount of butyl titanate and tetraethoxysilane to obtain a second mixed solution;
s20: slowly dripping the second mixed solution into the first mixed solution, uniformly stirring to obtain gel, and regulating the pH value to be 10-11 by using sodium hydroxide in the dripping process;
s30: putting the gel into a reaction kettle, carrying out hydrothermal crystallization at a certain temperature for a period of time, and filtering, washing and drying to obtain a TS-1 precursor;
s40: dissolving a certain amount of metal salt in deionized water, adding the TS-1 precursor, adjusting the pH to 5-6 by using ammonium chloride-ammonia water, stirring at a certain temperature for ion exchange for a certain time, filtering, washing, drying, and roasting at 550 ℃ for 5 hours to obtain the metal modified TS-1 titanium silicalite molecular sieve CO catalyst.
2. The preparation method of the metal modified TS-1 titanium silicalite CO catalyst of claim 1, wherein the molar ratio of the ethyl orthosilicate to the butyl titanate to the tetrapropylammonium bromide to the deionized water is (1: 0.05) - (0.1: 0.2) - (1: 20), respectively.
3. The method for preparing the metal modified TS-1 titanium silicalite molecular sieve CO catalyst as claimed in claim 1, wherein the crystallization temperature in S30 is 150-200 ℃, and the crystallization time is 24-72 h.
4. The preparation method of the metal modified TS-1 titanium silicalite CO catalyst according to claim 1, wherein the metal salt is a mixed salt of copper nitrate and manganese nitrate, and the molar ratio of the metal salt to the manganese nitrate is 1 (1-5).
5. The method of claim 1, wherein the concentration of the corresponding salt solution of the metal salt dissolved in deionized water is 0.01 to 0.05 mol/L.
6. The preparation method of the metal modified TS-1 titanium silicalite CO catalyst according to claim 1, wherein in the S40, the time of ion exchange is 1-5h, and the temperature is 60-80 ℃.
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Cited By (1)
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| CN116497476A (en) * | 2023-05-17 | 2023-07-28 | 百事基材料（青岛）股份有限公司 | Dacron large biological fiber containing saussurea involucrata active ingredient and preparation method thereof |
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| CN116497476A (en) * | 2023-05-17 | 2023-07-28 | 百事基材料（青岛）股份有限公司 | Dacron large biological fiber containing saussurea involucrata active ingredient and preparation method thereof |
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