Preparation of embedded micro-mesoporous composite molecular sieve-based sulfur-tolerant methanation catalyst
A composite molecular sieve, sulfur-resistant methanation technology, applied in molecular sieve catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems to be improved, low hydrothermal stability, etc. Cost-effective, simple and easy to prepare
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[0026] A method for preparing an embedded microporous-mesoporous composite molecular sieve sulfur-resistant methanation catalyst, the steps of which are:
[0027] (1) prepare M salt solution;
[0028] (2) Disperse the ZSM-5 microporous molecular sieve in the NaOH solution, add the template agent CTAB, stir vigorously, drop the silicon source TEOS at the same time, add the prepared M salt solution dropwise, stir vigorously for a certain period of time, and transfer to water Crystallization in a thermal reactor;
[0029] (3) The raw solution after crystallization is cooled to room temperature, filtered with suction, washed until neutral, dried in vacuum and roasted to obtain a catalyst, wherein the M loading in the catalyst is 1-20 wt%.
[0030] It is worth noting that the M salt is nickel sulfate, nickel chloride, nickel nitrate, nickel acetate, ammonium molybdate, sodium molybdate, potassium molybdate, manganese sulfate, manganese nitrate, manganese carbonate; The solvent us...
Embodiment 1
[0034] Example 1: A method for preparing an embedded microporous-mesoporous composite molecular sieve sulfur-resistant methanation catalyst. The steps are as follows: Weigh 3.2g of nickel nitrate hexahydrate and dissolve it in 20ml of deionized water to prepare an aqueous solution of nickel nitrate. Disperse 3.3g of ZSM-5 molecular sieve in NaOH solution, heat the solution to 40°C, add a certain amount of template agent (hexadecyltrimethylammonium bromide) under vigorous stirring, mix nickel nitrate aqueous solution and silicon source (orthosilicon ethyl acetate) was slowly added dropwise to the solution, the pH value of the solution was adjusted to 11, and the molar ratio of each substance in the solution was: 1.0ZSM-5: 0.12Ni: 0.12CTAB: 1.0TEOS: 0.2NaOH: 100H 2 O. The mixed solution was vigorously stirred and aged for 2 hours, then moved to a hydrothermal reaction kettle, crystallized at 100°C for 72 hours, cooled rapidly to room temperature, filtered, washed until neutral, ...
Embodiment 2
[0035] Example 2: A method for preparing an embedded microporous-mesoporous composite molecular sieve sulfur-resistant methanation catalyst, the steps of which are: weigh 1.3g of ammonium molybdate and dissolve it in 20ml of deionized water to prepare an ammonium molybdate aqueous solution. Disperse 3.3g of ZSM-5 molecular sieve in NaOH solution, heat the solution to 40°C, add a certain amount of templating agent (hexadecyltrimethylammonium bromide) under vigorous stirring, mix ammonium molybdate aqueous solution and silicon source (normal Ethyl silicate) was slowly added dropwise to the solution, the pH value of the solution was adjusted to 11, and the molar ratio of each substance in the solution was: 1.0ZSM-5: 0.07Mo: 0.12CTAB: 1.0TEOS: 0.2NaOH: 100H 2 O. The mixed solution was vigorously stirred and aged for 2 hours, then moved to a hydrothermal reaction kettle, crystallized at 100°C for 72 hours, cooled rapidly to room temperature, filtered, washed until neutral, dried ov...
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