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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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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the synthesis cycle of the catalyst is longer and the synthesis cost is higher

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

Embodiment 1

[0024] Weigh 0.5g of tetrapropylammonium bromide and 3g of hexapotassium bisammonium bromide, add it to 10ml of 10mol / L NaOH solution, fully dissolve, add 1g of aluminum sulfate octadecahydrate, 2g of boric acid, stir well, add dropwise 30ml of 5.465mol / L L silica sol, stirred for 40 minutes, and after it was in gel state, put it into a reaction kettle with a polytetrafluoroethylene liner, stood it at 200°C for 2 days, took it out to cool, washed, filtered, and dried at 500°C Calcining at the bottom to obtain sodium compound molecular sieve.

[0025] The sodium-type composite molecular sieve was ion-exchanged with 0.1mol / L ammonium nitrate solution at 90°C for 2h, washed with deionized water, then ion-exchanged with 0.1mol / L ammonium nitrate solution at 90°C for 2h, washed with deionized water, and filtered. Dry it 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-be...

Embodiment 2

[0033] Add 1g of aluminum isopropoxide and 2g of boric acid into 10ml of 10mol / L NaOH solution, add dropwise 30ml of 5.465mol / L silica sol after clarification, stir evenly, take 0.5g of tetrapropylammonium bromide and 2g of hexapotassium bromide diammonium Add it into the above solution, stir for 40 minutes, add the reaction kettle after the solution is in a gel state, crystallize at 170°C for 3 days, cool, wash, suction filter, dry, and roast 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°C for 2h, washed with deionized water, then ion-exchanged with 0.1mol / L ammonium nitrate solution at 90°C for 2h, washed with deionized water, and filtered. Dry it 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 10 mm, length 3...

Embodiment 3

[0038] Add 1g NaAlO to 10ml 10mol / L NaOH solution 2 , add 20ml of 4.36mol / L water glass dropwise, stir evenly, add 2g of diboron trioxide, 0.5g of tetrapropylammonium bromide and 2.5g of hexapotassium bisammonium bromide at one time, stir for 40min, until the solution is in a gel state Afterwards, it was added to a reaction kettle, crystallized at 150°C for 3 days, cooled, washed, filtered with suction, dried, and roasted 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°C for 2h, washed with deionized water, then ion-exchanged with 0.1mol / L ammonium nitrate solution at 90°C for 2h, washed with deionized water, and filtered. Dry it 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 10 mm, length 30 cm) was used to eva...

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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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