CN112062137A - Preparation method of MAZ zeolite molecular sieve - Google Patents
Preparation method of MAZ zeolite molecular sieve Download PDFInfo
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- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 31
- 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 31
- 239000010457 zeolite Substances 0.000 title claims abstract description 31
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 24
- 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 24
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims abstract description 24
- 235000019743 Choline chloride Nutrition 0.000 claims abstract description 24
- 229960003178 choline chloride Drugs 0.000 claims abstract description 24
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims abstract description 24
- 238000002425 crystallisation Methods 0.000 claims abstract description 22
- 230000008025 crystallization Effects 0.000 claims abstract description 22
- 239000008367 deionised water Substances 0.000 claims abstract description 18
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 239000003513 alkali Substances 0.000 claims abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 5
- 239000010703 silicon Substances 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 51
- 239000002994 raw material Substances 0.000 claims description 18
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical group [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims description 17
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical group O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 17
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 16
- 230000007935 neutral effect Effects 0.000 claims description 15
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 15
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 15
- 229910001220 stainless steel Inorganic materials 0.000 claims description 15
- 239000010935 stainless steel Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims 7
- 238000001816 cooling Methods 0.000 claims 6
- 238000001914 filtration Methods 0.000 claims 6
- -1 polytetrafluoroethylene Polymers 0.000 claims 6
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims 1
- 229910052593 corundum Inorganic materials 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- 238000000967 suction filtration Methods 0.000 claims 1
- 229910001845 yogo sapphire Inorganic materials 0.000 claims 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract 1
- 210000000941 bile Anatomy 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 8
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 238000005120 petroleum cracking Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
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- 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
- C01B39/46—Other types characterised by their X-ray diffraction pattern and their defined composition
- C01B39/48—Other types characterised by their X-ray diffraction pattern and their defined composition using at least one organic template directing agent
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- 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
- C01B39/04—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 using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Silicates, Zeolites, And Molecular Sieves (AREA)
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Abstract
本发明公开了一种MAZ沸石分子筛的制备方法，将铝源、碱源与去离子水混合均匀，在搅拌下加入硅源；继续搅拌直到溶液均匀形成硅铝凝胶，将一定量氯化胆碱加入硅铝凝胶后搅拌；然后置于反应釜中，晶化温度为100～180℃，晶化时间为0.5～2.5天，产物抽滤、洗涤、烘干，即可得到MAZ沸石分子筛原粉。本发明以氯化胆碱作为模板剂，在水热合成条件下合成棒状MAZ沸石分子筛，具有环境友好、成本低廉的优势。
The invention discloses a preparation method of MAZ zeolite molecular sieve. The aluminum source, the alkali source and the deionized water are mixed uniformly, and the silicon source is added under stirring; the stirring is continued until the solution is uniformly formed into a silica-alumina gel, and a certain amount of bile chloride is added. The alkali is added to the silica-alumina gel and then stirred; then placed in a reaction kettle, the crystallization temperature is 100-180 ° C, the crystallization time is 0.5-2.5 days, the product is suction filtered, washed and dried to obtain the original MAZ zeolite molecular sieve. pink. The invention uses choline chloride as a template agent to synthesize rod-shaped MAZ zeolite molecular sieves under hydrothermal synthesis conditions, and has the advantages of environmental friendliness and low cost.
Description
技术领域technical field
本发明属于分子筛制备方法，特别涉及一种制备MAZ沸石分子筛的绿色模板剂。The invention belongs to a method for preparing molecular sieves, in particular to a green template agent for preparing MAZ zeolite molecular sieves.
背景技术Background technique
沸石分子筛是一类具有骨架结构、独特孔道结构的微孔晶体材料。此外，沸石分子筛因其高的比表面积、大的孔容、可调节的酸密度等特点，被广泛应用于吸附、催化等重要领域。MAZ沸石分子筛具有一维12元环孔道结构，属于P63/mmc空间群。MAZ沸石广泛应用于芳烃烷基化、加氢异构、石油裂化、链烷烃和芳烃的异构化反应中。Zeolite molecular sieve is a kind of microporous crystalline material with framework structure and unique pore structure. In addition, zeolite molecular sieves are widely used in important fields such as adsorption and catalysis due to their high specific surface area, large pore volume, and adjustable acid density. The MAZ zeolite molecular sieve has a one-dimensional 12-membered ring channel structure and belongs to the P6 3 /mmc space group. MAZ zeolite is widely used in aromatic alkylation, hydroisomerization, petroleum cracking, isomerization of paraffins and aromatics.
目前合成MAZ沸石分子筛的过程中，常用的有机模板剂有四甲基氢氧化铵，二氧六环，哌嗪等。其中四甲基氢氧化铵的使用最为广泛。然而，四甲基氢氧化铵具有毒性和较强的腐蚀性，二氧六环具有毒性和化学致癌性，哌嗪遇高热可燃，分解释放有毒气体。使用以上模板剂不仅成本较高，而且污染环境。开发环境友好的绿色模板剂制备MAZ沸石分子筛具有十分重要的研究意义。研究者近年来发现氯化胆碱具有导向合成沸石分子筛的能力，虽然现有技术中有记载氯化胆碱用于制备CHA沸石、SSZ沸石等，但是无制备MAZ沸石的报道。At present, in the process of synthesizing MAZ zeolite molecular sieves, the commonly used organic templates are tetramethylammonium hydroxide, dioxane, piperazine, etc. Among them, tetramethylammonium hydroxide is the most widely used. However, tetramethylammonium hydroxide is toxic and highly corrosive, dioxane is toxic and chemically carcinogenic, and piperazine is flammable when exposed to high heat, and decomposes to release toxic gases. The use of the above templating agents is not only costly, but also pollutes the environment. It is of great research significance to develop environmentally friendly green templates to prepare MAZ zeolite molecular sieves. In recent years, researchers have found that choline chloride has the ability to guide the synthesis of zeolite molecular sieves. Although there are records in the prior art that choline chloride is used to prepare CHA zeolite, SSZ zeolite, etc., there is no report on the preparation of MAZ zeolite.
发明内容SUMMARY OF THE INVENTION
本发明主要目的在于克服现有技术中的不足，首次提出使用氯化胆碱作为模板剂合成棒状MAZ沸石分子筛的方法。The main purpose of the present invention is to overcome the deficiencies in the prior art, and for the first time proposes a method for synthesizing rod-shaped MAZ zeolite molecular sieves by using choline chloride as a template agent.
本发明提供一种MAZ沸石分子筛的制备方法，具体如下：The invention provides a preparation method of MAZ zeolite molecular sieve, which is specifically as follows:
控制各反应原料的添加量，使SiO2:Al2O3:Na2O:R:H2O的摩尔比范围为8～20:1:2.65～3.44:4.46～9.82:93～250，将铝源、碱源与去离子水混合均匀，在搅拌下加入硅源；继续搅拌直到溶液均匀形成硅铝凝胶，将一定量模板剂R加入硅铝凝胶后搅拌，所述模板剂R为氯化胆碱；然后置于反应釜中，晶化温度为100～180℃，晶化时间为0.5～2.5天，产物抽滤、洗涤、烘干，即可得到MAZ沸石分子筛原粉。The addition amount of each reaction raw material is controlled, so that the molar ratio of SiO 2 :Al 2 O 3 :Na 2 O:R:H 2 O is in the range of 8～20:1:2.65～3.44:4.46～9.82:93～250. The aluminum source, the alkali source and the deionized water are evenly mixed, and the silicon source is added under stirring; the stirring is continued until the solution uniformly forms a silica-alumina gel, and a certain amount of template agent R is added to the silica-alumina gel and stirred, and the template agent R is Choline chloride; then placed in a reaction kettle, the crystallization temperature is 100-180 DEG C, the crystallization time is 0.5-2.5 days, the product is suction filtered, washed and dried to obtain the original powder of MAZ zeolite molecular sieve.
特别的，所述铝源为铝酸钠。Particularly, the aluminum source is sodium aluminate.
特别的，所述碱源为氢氧化钠。Particularly, the alkali source is sodium hydroxide.
特别的，所述硅源为硅溶胶。Particularly, the silicon source is silica sol.
本发明的有益效果在于：本发明首次提出氯化胆碱作为模板剂，在水热合成条件下合成棒状MAZ沸石分子筛。目前关于合成MAZ沸石分子筛的报道，所用的模板剂主要为四甲基氢氧化铵、二氧六环、哌嗪，以上模板剂有毒性、致癌性与可燃性等生产隐患，未满足绿色可持续发展的要求。本申请通过调节起始原料的配比和晶化条件，首次使用氯化胆碱成功制备了棒状MAZ沸石分子筛。The beneficial effects of the present invention are as follows: the present invention proposes choline chloride as a template agent for the first time to synthesize rod-shaped MAZ zeolite molecular sieves under hydrothermal synthesis conditions. The current reports on the synthesis of MAZ zeolite molecular sieves mainly use tetramethylammonium hydroxide, dioxane, and piperazine. The above template agents have production hidden dangers such as toxicity, carcinogenicity and flammability, and do not meet the requirements of green sustainable development. development requirements. In the present application, the rod-shaped MAZ zeolite molecular sieve was successfully prepared by using choline chloride for the first time by adjusting the ratio of starting materials and the crystallization conditions.
与现有技术相比，本发明具有如下优点：Compared with the prior art, the present invention has the following advantages:
1、本发明使用氯化胆碱作为模板剂制备MAZ沸石分子筛的方法，不仅极大地减少了污染物的排放，而且降低了合成的成本，符合绿色、可持续发展的需求。1. The present invention uses choline chloride as a template to prepare the method for MAZ zeolite molecular sieve, which not only greatly reduces the discharge of pollutants, but also reduces the cost of synthesis, and meets the needs of green and sustainable development.
2、本发明制备的产品不仅保持了良好的结晶度和纯度，具有良好的吸附能力。另外，所采用的无机原料均对环境友好、成本低廉，因而本发现在实际化学化工生产领域具有重要意义。2. The product prepared by the present invention not only maintains good crystallinity and purity, but also has good adsorption capacity. In addition, the inorganic raw materials used are all environmentally friendly and low in cost, so the present invention has great significance in the field of actual chemical and chemical production.
附图说明Description of drawings
图1：MAZ沸石分子筛产品的XRD图。Figure 1: XRD pattern of MAZ zeolite molecular sieve product.
图2：MAZ沸石分子筛产品的SEM图。Figure 2: SEM image of MAZ zeolite molecular sieve product.
具体实施方式Detailed ways
实施例1:MAZ沸石样品的制备Example 1: Preparation of MAZ Zeolite Samples
首先，将0.94g铝酸钠加入至6.8g水中混合均匀，向其中加入0.53g氢氧化钠，待溶液澄清后，逐滴加入8.4g硅溶胶，继续搅拌，再加入3.5g氯化胆碱后搅拌至均匀凝胶；将反应原料加入聚四氟乙烯不锈钢反应釜中，在150℃下晶化1天即完成晶化，室温冷却，用去离子水洗涤至中性，产物抽滤、在100℃空气中干燥后得到产品。First, 0.94g of sodium aluminate was added to 6.8g of water and mixed evenly, and 0.53g of sodium hydroxide was added to it. After the solution was clarified, 8.4g of silica sol was added dropwise, stirring was continued, and 3.5g of choline chloride was added. Stir until the gel is uniform; add the reaction raw materials to the PTFE stainless steel reaction kettle, crystallize at 150 ° C for 1 day to complete the crystallization, cool at room temperature, wash with deionized water until neutral, the product is suction filtered, at 100 The product was obtained after drying in air.
附图1为合成的产品的X射线衍射图(XRD)，经X射线衍射分析其结构为MAZ沸石分子筛。附图2为合成的样品的扫描电镜照片(SEM)，通过扫描电镜照片可以看出所合成的产品呈现纳米棒状形貌。Accompanying drawing 1 is the X-ray diffraction pattern (XRD) of the synthesized product, and its structure is MAZ zeolite molecular sieve according to X-ray diffraction analysis. Accompanying drawing 2 is the scanning electron microscope photograph (SEM) of the synthesized sample, and it can be seen from the SEM photograph that the synthesized product presents a nanorod shape.
实施例2:MAZ沸石样品的制备Example 2: Preparation of MAZ Zeolite Samples
首先，将0.94g铝酸钠加入至10.8g水中混合均匀，向其中加入0.53g氢氧化钠，待溶液澄清后，逐滴加入12.0g硅溶胶，继续搅拌，再加入3.5g氯化胆碱后搅拌至均匀凝胶；将反应原料加入聚四氟乙烯不锈钢反应釜中，在150℃下晶化1天即完成晶化，室温冷却，用去离子水洗涤至中性，产物抽滤、在100℃空气中干燥后得到产品。First, add 0.94g of sodium aluminate to 10.8g of water and mix well, add 0.53g of sodium hydroxide to it, and after the solution is clarified, add 12.0g of silica sol dropwise, continue stirring, and then add 3.5g of choline chloride. Stir until the gel is uniform; add the reaction raw materials to the PTFE stainless steel reaction kettle, crystallize at 150 ° C for 1 day to complete the crystallization, cool at room temperature, wash with deionized water until neutral, the product is suction filtered, at 100 The product was obtained after drying in air.
实施例3:MAZ沸石样品的制备Example 3: Preparation of MAZ Zeolite Samples
首先，将0.94g铝酸钠加入至3.8g水中混合均匀，向其中加入0.53g氢氧化钠，待溶液澄清后，逐滴加入4.8g硅溶胶，继续搅拌，再加入3.5g氯化胆碱后搅拌至均匀凝胶；将反应原料加入聚四氟乙烯不锈钢反应釜中，在150℃下晶化1天即完成晶化，室温冷却，用去离子水洗涤至中性，产物抽滤、在100℃空气中干燥后得到产品。First, add 0.94g of sodium aluminate to 3.8g of water and mix well, add 0.53g of sodium hydroxide to it, and after the solution is clarified, add 4.8g of silica sol dropwise, continue stirring, and then add 3.5g of choline chloride. Stir until the gel is uniform; add the reaction raw materials to the PTFE stainless steel reaction kettle, crystallize at 150 ° C for 1 day to complete the crystallization, cool at room temperature, wash with deionized water until neutral, the product is suction filtered, at 100 The product was obtained after drying in air.
实施例4:低碱条件下MAZ沸石样品的制备Example 4: Preparation of MAZ zeolite samples under low alkali conditions
首先，将0.94g铝酸钠加入至6.8g水中混合均匀，向其中加入0.40g氢氧化钠，待溶液澄清后，逐滴加入8.4g硅溶胶，继续搅拌，再加入3.5g氯化胆碱后搅拌至均匀凝胶；将反应原料加入聚四氟乙烯不锈钢反应釜中，在150℃下晶化1天即完成晶化，室温冷却，用去离子水洗涤至中性，产物抽滤、在100℃空气中干燥后得到产品。First, add 0.94g of sodium aluminate to 6.8g of water and mix well, add 0.40g of sodium hydroxide to it, and after the solution is clarified, add 8.4g of silica sol dropwise, continue stirring, and then add 3.5g of choline chloride. Stir until the gel is uniform; add the reaction raw materials to the PTFE stainless steel reaction kettle, crystallize at 150 ° C for 1 day to complete the crystallization, cool at room temperature, wash with deionized water until neutral, the product is suction filtered, at 100 The product was obtained after drying in air.
实施例5:高碱条件下MAZ沸石样品的制备Embodiment 5: the preparation of MAZ zeolite sample under highly alkaline condition
首先，将0.94g铝酸钠加入至6.8g水中混合均匀，向其中加入0.65g氢氧化钠，待溶液澄清后，逐滴加入8.4g硅溶胶，继续搅拌，再加入3.5g氯化胆碱后搅拌至均匀凝胶；将反应原料加入聚四氟乙烯不锈钢反应釜中，在150℃下晶化1天即完成晶化，室温冷却，用去离子水洗涤至中性，产物抽滤、在100℃空气中干燥后得到产品。First, add 0.94g of sodium aluminate to 6.8g of water and mix well, add 0.65g of sodium hydroxide to it, and after the solution is clarified, add 8.4g of silica sol dropwise, continue stirring, and then add 3.5g of choline chloride. Stir until the gel is uniform; add the reaction raw materials to the PTFE stainless steel reaction kettle, crystallize at 150 ° C for 1 day to complete the crystallization, cool at room temperature, wash with deionized water until neutral, the product is suction filtered, at 100 The product was obtained after drying in air.
实施例6:MAZ沸石样品的制备Example 6: Preparation of MAZ Zeolite Samples
首先，将0.94g铝酸钠加入至6.8g水中混合均匀，向其中加入0.53g氢氧化钠，待溶液澄清后，逐滴加入8.4g硅溶胶，继续搅拌，再加入2.5g氯化胆碱后搅拌至均匀凝胶；将反应原料加入聚四氟乙烯不锈钢反应釜中，在150℃下晶化1天即完成晶化，室温冷却，用去离子水洗涤至中性，产物抽滤、在100℃空气中干燥后得到产品。First, add 0.94g of sodium aluminate to 6.8g of water and mix well, add 0.53g of sodium hydroxide to it, and after the solution is clarified, add 8.4g of silica sol dropwise, continue stirring, and then add 2.5g of choline chloride. Stir until the gel is uniform; add the reaction raw materials to the PTFE stainless steel reaction kettle, crystallize at 150 ° C for 1 day to complete the crystallization, cool at room temperature, wash with deionized water until neutral, the product is suction filtered, at 100 The product was obtained after drying in air.
实施例7:MAZ沸石样品的制备Example 7: Preparation of MAZ Zeolite Samples
首先，将0.94g铝酸钠加入至6.8g水中混合均匀，向其中加入0.53g氢氧化钠，待溶液澄清后，逐滴加入8.4g硅溶胶，继续搅拌，再加入5.5g氯化胆碱后搅拌至均匀凝胶；将反应原料加入聚四氟乙烯不锈钢反应釜中，在150℃下晶化1天即完成晶化，室温冷却，用去离子水洗涤至中性，产物抽滤、在100℃空气中干燥后得到产品。First, 0.94g of sodium aluminate was added to 6.8g of water and mixed evenly, and 0.53g of sodium hydroxide was added to it. After the solution was clarified, 8.4g of silica sol was added dropwise, stirring was continued, and 5.5g of choline chloride was added. Stir until the gel is uniform; add the reaction raw materials to the PTFE stainless steel reaction kettle, crystallize at 150 ° C for 1 day to complete the crystallization, cool at room temperature, wash with deionized water until neutral, the product is suction filtered, at 100 The product was obtained after drying in air.
实施例8:低温条件下MAZ沸石样品的制备Example 8: Preparation of MAZ zeolite samples under low temperature conditions
首先，将0.94g铝酸钠加入至6.8g水中混合均匀，向其中加入0.53g氢氧化钠，待溶液澄清后，逐滴加入8.4g硅溶胶，继续搅拌，再加入3.5g氯化胆碱后搅拌至均匀凝胶；将反应原料加入聚四氟乙烯不锈钢反应釜中，在100℃下晶化2.5天即完成晶化，室温冷却，用去离子水洗涤至中性，产物抽滤、在100℃空气中干燥后得到产品。First, 0.94g of sodium aluminate was added to 6.8g of water and mixed evenly, and 0.53g of sodium hydroxide was added to it. After the solution was clarified, 8.4g of silica sol was added dropwise, stirring was continued, and 3.5g of choline chloride was added. Stir until homogeneous gel; add the reaction raw materials into the PTFE stainless steel reaction kettle, crystallize at 100 ° C for 2.5 days to complete the crystallization, cool at room temperature, wash with deionized water until neutral, the product is suction filtered, at 100 The product was obtained after drying in air.
实施例9:高温条件下MAZ沸石样品的制备Example 9: Preparation of MAZ zeolite samples under high temperature conditions
首先，将0.94g铝酸钠加入至6.8g水中混合均匀，向其中加入0.53g氢氧化钠，待溶液澄清后，逐滴加入8.4g硅溶胶，继续搅拌，再加入3.5g氯化胆碱后搅拌至均匀凝胶；将反应原料加入聚四氟乙烯不锈钢反应釜中，在180℃下晶化0.5天即完成晶化，室温冷却，用去离子水洗涤至中性，产物抽滤、在100℃空气中干燥后得到产品。First, 0.94g of sodium aluminate was added to 6.8g of water and mixed evenly, and 0.53g of sodium hydroxide was added to it. After the solution was clarified, 8.4g of silica sol was added dropwise, stirring was continued, and 3.5g of choline chloride was added. Stir until the gel is uniform; add the reaction raw materials into the PTFE stainless steel reaction kettle, crystallize at 180 ° C for 0.5 days to complete the crystallization, cool at room temperature, wash with deionized water until neutral, the product is suction filtered, at 100 The product was obtained after drying in air.
注：a初始凝胶中的摩尔配比。Notes: a Molar ratio in the initial gel.
以上所述，仅是本发明的几种实施案例而已，并非对本发明做任何形式上的限制，虽然本发明已以较佳实施案例揭示如上，然而并非用以限定本发明，任何熟悉本专业的技术人员，在不脱离本发明技术方案范围内，当可利用上述揭示的结构及技术内容做出些许的更动或修饰为等同变化的等效实施案例。但是凡是未脱离本发明技术方案的内容，依据本发明的技术实质对以上实施案例所作的任何简单修改、等同变化与修饰，均仍属本发明技术方案范围内。The above is only a few examples of implementation of the present invention, and does not limit the present invention in any form. Although the present invention has been disclosed above with preferred implementation examples, it is not intended to limit the present invention. Those skilled in the art can make some changes or modifications by using the structures and technical contents disclosed above, without departing from the scope of the technical solutions of the present invention, into equivalent implementation cases of equivalent changes. However, any simple modifications, equivalent changes and modifications made to the above embodiments according to the technical essence of the present invention without departing from the content of the technical solutions of the present invention still fall within the scope of the technical solutions of the present invention.
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| CN116081637A (en) * | 2023-01-30 | 2023-05-09 | 南京工业大学 | A kind of MAZ zeolite and its preparation method and application |
| CN118341478A (en) * | 2024-04-24 | 2024-07-16 | 南京工业大学 | Application of MAZ zeolite in catalyzing benzene oxidation |
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