One-step synthesis method for B-EU-1/ZSM-5 composite molecular sieve

A technology of B-EU-1 and ZSM-5, which is applied in molecular sieve catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of high synthesis cost and long synthesis cycle, and achieve stable selectivity and low synthesis cost. Reduce, reduce the effect of the compositing step

Active Publication Date: 2015-04-01
TAIYUAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the synthesis cycle of the catalys

Method used

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  • One-step synthesis method for B-EU-1/ZSM-5 composite molecular sieve
  • One-step synthesis method for B-EU-1/ZSM-5 composite molecular sieve
  • One-step synthesis method for B-EU-1/ZSM-5 composite molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0023] Example 1

[0024] Weigh 0.5g tetrapropylammonium bromide and 3g hexapotassium diammonium bromide into 10ml 10mol / L NaOH solution to fully dissolve, add 1g aluminum sulfate octahydrate, 2g boric acid, stir well, add 30ml 5.465mol / L L silica sol, stir for 40 minutes, after it is in a gel state, add it to a reactor with PTFE lining, let it stand for 2 days at 200℃ for crystallization, take it out, cool, wash, filter, dry, 500℃ Lower roasting to obtain sodium type composite molecular sieve.

[0025] The sodium composite molecular sieve was ion exchanged with 0.1mol / L ammonium nitrate solution at 90℃ for 2h, washed with deionized water, and then ion exchanged with 0.1mol / L ammonium nitrate solution at 90℃ for 2h, washed with deionized water, filtered, Dry in an oven at 100°C and place it in a muffle furnace at 500°C for 4 hours to obtain a hydrogen-type composite molecular sieve.

[0026] A continuous flow fixed-bed reactor (inner diameter 10mm, length 30cm) was used to evaluate...

Example Embodiment

[0032] Example 2

[0033] Take 1g aluminum isopropoxide and 2g boric acid into 10ml 10mol / L NaOH solution, add 30ml 5.465mol / L silica sol dropwise after clarification, stir well, take 0.5g tetrapropylammonium bromide and 2g hexapotassium diammonium bromide Add the above solution and stir for 40 minutes. After the solution is in a gel state, add it to the reaction kettle, crystallize at 170°C for 3 days, cool, wash, filter, dry, and calcinate at 500°C to obtain a sodium-type composite molecular sieve.

[0034] The sodium type composite molecular sieve was ion exchanged with 0.1mol / L ammonium nitrate solution at 90℃ for 2h, washed with deionized water, and then ion exchanged with 0.1mol / L ammonium nitrate solution at 90℃ for 2h, washed with deionized water, filtered, Dry in an oven at 100°C and place it in a muffle furnace at 500°C for 4 hours to obtain a hydrogen-type composite molecular sieve.

[0035] A continuous flow fixed bed reactor (inner diameter 10mm, length 30cm) was used t...

Example Embodiment

[0037] Example 3

[0038] Add 1g NaAlO to 10ml 10mol / L NaOH solution 2 , Add 20ml 4.36mol / L water glass dropwise, stir evenly, add 2g diboron trioxide, 0.5g tetrapropylammonium bromide and 2.5g hexapotassium diammonium bromide at one time, stir for 40min, wait until the solution is gel state Then it was added to the reaction kettle, crystallized at 150°C for 3 days, cooled, washed, filtered, dried, and calcined at 500°C to obtain a sodium-type composite molecular sieve.

[0039] The sodium type composite molecular sieve was ion exchanged with 0.1mol / L ammonium nitrate solution at 90℃ for 2h, washed with deionized water, and then ion exchanged with 0.1mol / L ammonium nitrate solution at 90℃ for 2h, washed with deionized water, filtered, Dry in an oven at 100°C and place it in a muffle furnace at 500°C for 4 hours to obtain a hydrogen-type composite molecular sieve.

[0040] A continuous flow fixed bed reactor (inner diameter 10mm, length 30cm) was used to evaluate the methanol aromati...

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Abstract

The invention discloses a one-step synthesis method for a B-EU-1/ZSM-5 composite molecular sieve. The one-step synthesis method comprises the following steps: adding sodium hydroxide, a silicon source, an aluminum source, a boron-containing compound and a template agent into water at a molar ratio of Na2O:SiO2: Al2O3:B2O3: a template agent:H2O being 1.5 to (0.1-7) to (0.001-0.2) to (0.001-0.3) to (0.01-2.25) to (1-10), and uniformly stirring to obtain mixed gel; crystallizing the mixed gel at a constant temperature of 130-200 DEG C, roasting at 350-650 DEG C to remove the template agent, performing ion exchange by an acid solution, washing and keeping for 4 hours at 350-650 DEG C to obtain a B-EU-1/ZSM-5 hydrogen composite molecular sieve, wherein the template agent consists of tetrapropylammonium bromide and hexamethonium bromide by mixing. The one-step synthesis method disclosed by the invention can be used for quickly and simply synthesizing a composite molecular sieve which simultaneously contains a EUO structure and an MFI structure, and is doped with a nonmetal element B, wherein the composite molecular sieve is used as a catalyst for preparing dimethylbenzene by methanol aromatization.

Description

technical field [0001] The invention relates to a method for preparing a composite molecular sieve catalyst, in particular to a method for preparing a B-EU-1 / ZSM-5 composite molecular sieve. The composite molecular sieve catalyst prepared by the method of the invention is used for direct conversion of methanol to produce xylene. Background technique [0002] Aromatics are the basic raw materials of the petrochemical industry and play an important role in my country's modern national economy. Among the total of about 8 million known organic compounds, aromatic compounds account for about 30%, among which BTX aromatics (benzene, toluene, xylene) are called primary basic organic raw materials. Industrial aromatics mainly come from petroleum processing and coal processing industries. With the development of ethylene industry and oil refining industry in recent years, the output of BTX aromatics produced by petroleum has increased rapidly, and the proportion of aromatics produce...

Claims

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Application Information

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IPC IPC(8): B01J29/80C07C15/08C07C1/20
CPCY02P20/52
Inventor 杨冬花李建华王新波钟丽萍郭超吕爱凝李晓峰窦涛
Owner TAIYUAN UNIV OF TECH
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