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Method for temperature-programmed synthesis of nanometer ZSM-5 molecular sieve used for methanol to propylene

A ZSM-5, temperature-programmed technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of prolonged synthesis time, excessively low crystallization temperature, etc. effect of chemical cycle, particle size reduction, and good catalytic performance

Inactive Publication Date: 2017-03-01
JIANGSU TIANNUO NEW MATERIAL TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, too low crystallization temperature prolongs the required synthesis time

Method used

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  • Method for temperature-programmed synthesis of nanometer ZSM-5 molecular sieve used for methanol to propylene
  • Method for temperature-programmed synthesis of nanometer ZSM-5 molecular sieve used for methanol to propylene
  • Method for temperature-programmed synthesis of nanometer ZSM-5 molecular sieve used for methanol to propylene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 7.04g of NaOH to 60.2g of distilled water, stir until a clear solution, add 1.3g of sodium metaaluminate into the above solution and stir until completely dissolved. Under magnetic stirring, slowly add 150g of silica sol dropwise to the above mixed solution to form aluminosilicate gel A; weigh a certain amount of tetrapropylammonium hydroxide, and add tetrapropylammonium hydroxide and aluminosilicate SiO2 in the salt gel The mass ratio is 0.25, the above-mentioned tetrapropyl ammonium hydroxide is added into the deionized water of 30.8g to obtain mixed solution B, under stirring condition, solution B is slowly added in A gel to make mixing, finally Transfer the mixture into a polytetrafluoroethylene-lined stainless steel crystallization kettle, raise the temperature from room temperature to 120°C at a rate of 5°C / hour, and then crystallize at 120°C for 20 hours; the product is filtered, washed, and dried at 85°C After 14 hours, calcination at 550°C for 10 hours, the...

Embodiment 2

[0029] Add 7.04g of NaOH to 60.2g of distilled water, stir until a clear solution, add 1.3g of sodium metaaluminate into the above solution and stir until completely dissolved. Under magnetic stirring, slowly add 150g of silica sol dropwise to the above mixed solution to form aluminosilicate gel A; weigh a certain amount of tetrapropylammonium hydroxide, and add tetrapropylammonium hydroxide and aluminosilicate SiO2 in the salt gel The mass ratio is 0.25, the above-mentioned tetrapropyl ammonium hydroxide is added into the deionized water of 30.8g to obtain mixed solution B, under stirring condition, solution B is slowly added in A gel to make mixing, finally Transfer the mixture into a polytetrafluoroethylene-lined stainless steel crystallization kettle, raise the temperature from room temperature to 120°C at a rate of 10°C / hour, and then crystallize at 120°C for 20 hours; the product is filtered, washed, and dried at 85°C After 14 hours, calcination at 550° C. for 10 hours, ...

Embodiment 3

[0031] Add 7.04g of NaOH to 60.2g of distilled water, stir until a clear solution, add 1.3g of sodium metaaluminate into the above solution and stir until completely dissolved. Under magnetic stirring, slowly add 150g of silica sol dropwise to the above mixed solution to form aluminosilicate gel A; weigh a certain amount of tetrapropylammonium hydroxide, and add tetrapropylammonium hydroxide and aluminosilicate SiO2 in the salt gel The mass ratio is 0.25, the above-mentioned tetrapropyl ammonium hydroxide is added into the deionized water of 30.8g to obtain mixed solution B, under stirring condition, solution B is slowly added in A gel to make mixing, finally Transfer the mixture into a polytetrafluoroethylene-lined stainless steel crystallization kettle, raise the temperature from room temperature to 150°C at a rate of 5°C / hour, and then crystallize at 150°C for 12 hours; the product is filtered, washed, and dried at 85°C After 14 hours, calcination at 550°C for 10 hours, the...

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Abstract

The invention discloses a method for temperature-programmed synthesis of a nanometer ZSM-5 molecular sieve used for methanol to propylene, belonging to the field of synthetic methods for molecular sieves. The method provided by the invention comprises the following steps: subjecting a silicon source, an aluminum source, an alkali source, deionized water and a template agent to uniform mixing under stirring, then adding a seed crystal, transferring the uniformly-mixed mixture into a crystallization kettle, carrying out crystallization for a period of time by adopting a temperature-programmed method, and successively carrying out washing, drying and calcination so as to obtain the nanometer ZSM-5 molecular sieve which has good dispersibility, is used for methanol to propylene and shows good catalytic performance in an MTP reaction. The method provided by the invention can effectively shorten the time of synthesizing the nanometer ZSM-5 molecular sieve with good dispersibility; due to adoption of the temperature-programmed method, the nucleation activation energy of a molecular sieve is reduced; the nucleation rate is increased; the particle size of a sample is reduced; meanwhile, the crystallization process of the molecular sieve is accelerated; the crystallization cycle is shortened; and the crystallinity of the synthesized molecular sieve is high.

Description

technical field [0001] The invention relates to the technical field of molecular sieve synthesis methods, in particular to a synthesis method of nanometer ZSM-5 molecular sieves for temperature-programmed synthesis of methanol to propylene. Background technique [0002] Due to the wide range of cheap raw material sources and high propylene yield, the methanol-to-propylene (MTP) process is considered to be an important pathway for propylene production in the post-oil and gas era, and has received increasing attention from academia and industry. Among the many factors affecting the characteristics and efficiency of the MTP process, the catalyst plays a key role. [0003] After Mobil Petroleum Company of the United States announced the invention of ZSM-5 zeolite molecular sieve in USP3702886 in 1972, due to its high silicon-aluminum ratio, unique three-dimensional cross-channel structure, excellent hydrothermal stability and anti-coking deactivation performance , ZSM-5 molecul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40
Inventor 胡思窦涛张卿郭兆民宋洁邢法猛余倩尹琪
Owner JIANGSU TIANNUO NEW MATERIAL TECH
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