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A preparation method of phosphorus oxide modified microporous molecular sieve shape-selective catalyst

A technology of microporous molecular sieves and phosphorus oxides, applied in the direction of molecular sieve catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of high cost, cumbersome preparation operations, harsh conditions, etc., and achieve low cost and high catalyst Effects of improving activity and shape-selective performance

Inactive Publication Date: 2016-08-03
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved in the present invention is to provide a simple and low-cost synthetic method for the preparation of a shape-selective catalyst in the process of synthesizing p-xylene and p-diethylbenzene from the disproportionation of toluene and ethylbenzene. , Preparation method of shape-selective catalyst with high shape-selective performance

Method used

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  • A preparation method of phosphorus oxide modified microporous molecular sieve shape-selective catalyst

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Embodiment 1

[0016] Add hypophosphoric acid into anhydrous methanol, wherein the mass ratio of hypophosphoric acid to methanol is 1:5, stir until completely dissolved; then add microporous molecular sieve ZSM-5 to the above solution, wherein hypophosphoric acid and microporous molecular sieve The mass ratio was 1:20, stirred evenly, and stood at room temperature for 12 hours; evaporated to dryness in a water bath, then dried in an oven at 120°C for 6 hours, then transferred to a muffle furnace, and dried in an air atmosphere at 10°C The temperature was raised to 600°C at a rate of 1 / min, and kept at this temperature for 4 hours, and then lowered to room temperature to obtain the desired phosphorus oxide-modified microporous molecular sieve shape-selective catalyst, denoted as Cat1.

Embodiment 2

[0018] Add pyrophosphoric acid into anhydrous methanol, wherein the mass ratio of pyrophosphoric acid to methanol is 1:7, and stir until completely dissolved; then add microporous molecular sieve ZSM-5 to the above solution, wherein the mass ratio of pyrophosphoric acid to microporous molecular sieve 1:6, stirred evenly, and stood at room temperature for 12 hours; evaporated the obtained material to dryness in a water bath, then put it in a 120°C oven to dry for 6 hours, and then transferred it to a muffle furnace. The temperature was raised to 600° C. and kept at this temperature for 4 hours, and then lowered to room temperature to obtain the desired phosphorus oxide-modified microporous molecular sieve shape-selective catalyst, denoted as Cat2.

Embodiment 3

[0020] Add pyrophosphorous acid into anhydrous methanol, wherein the mass ratio of pyrophosphorous acid to methanol is 1:10, stir until completely dissolved; then add microporous molecular sieve ZSM-5 to the above solution, wherein pyrophosphorous acid and microporous molecular sieve The mass ratio is 1:6, stirred evenly, and allowed to stand at room temperature for 12 hours; evaporated to dryness in a water bath, then dried in an oven at 120°C for 6 hours, then transferred to a muffle furnace, and heated in an air atmosphere at 10°C The temperature was raised to 600°C at a rate of 1 / min, and kept at this temperature for 4 hours, and then lowered to room temperature to obtain the desired phosphorus oxide-modified microporous molecular sieve shape-selective catalyst, denoted as Cat3.

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Abstract

The invention relates to a method for preparing a phosphorus oxide modified microporous molecular sieve shape-selective catalyst. by the method, a microporous molecular sieve ZSM-5 or MCM-22 is used as a matrix, pyrophosphorous acid, hypophosphoric acid, iso-hypophosphoric acid, pyrophosphoric acid, triphosphoric acid or peroxydiphosphoric acid is used as the precursor of a phosphorus oxide, and the phosphorus oxide is loaded on the outer surface of the microporous molecular sieve in an impregnation and temperature programmed calcination method, wherein the mass ratio of the phosphorus oxide to the microporous molecular sieve is (1:6) to (1:20). The obtained shape-selective catalyst provided by the invention has good shape-selection catalytic performance on toluene disproportionation and ethylbenzene disproportionation processes, and the preparation method of the catalyst is simple.

Description

technical field [0001] The invention relates to the field of preparation of solid inorganic composite materials, in particular to a preparation method of a phosphorus oxide modified microporous molecular sieve shape-selective catalyst used in the disproportionation process of toluene and ethylbenzene. Background technique [0002] Toluene disproportionation and ethylbenzene disproportionation are the main industrial production processes for the synthesis of p-xylene and p-diethylbenzene, both of which are typical shape-selective catalytic processes. Microporous molecular sieves such as ZSM-5 and MCM-22 are commonly used shape-selective catalysts for the disproportionation of toluene or ethylbenzene. However, since there are a large number of acid sites on the outer surface of these microporous molecular sieves, the p-xylene generated in the pores of the molecular sieve during the disproportionation of toluene can easily undergo isomerization reaction on the acidic sites on t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/40B01J29/70C07C6/12C07C15/08C07C15/02
CPCY02P20/52
Inventor 薛冰朱星兴柳娜李永昕许杰
Owner CHANGZHOU UNIV
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