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A kind of preparation method of methanol dehydration production dimethyl ether catalyst

A methanol dehydration and catalyst technology, which is applied in the direction of ether preparation, dehydration of hydroxyl-containing compounds to prepare ether, chemical instruments and methods, etc., can solve the problems of selectivity and activity decline, many by-products, low initial temperature, etc., and achieve high activity And anti-coke performance, improve the overall performance, improve the effect of stability

Active Publication Date: 2017-01-25
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the catalyst used for methanol dehydration is generally Al 2 o 3 Or molecular sieves, among which the commonly used molecular sieves include aluminum phosphate, HZSM-5, HY, SAPO, etc., and they all have their own shortcomings: for example, although alumina has high stability, the reaction temperature is high, and the requirements for reaction equipment are very high, resulting in cost High; molecular sieve catalysts have strong acidity and low initial temperature, but they also have the disadvantages of many by-products, easy carbon deposition, and easy deactivation
The above-mentioned catalysts have high catalytic activity and selectivity in the reaction, and the optimal load of silicotungstic acid is 10wt%~16wt%. Under normal pressure, when used to treat pure methanol raw materials, its selectivity is high, but Its low-temperature activity is not good, and when it is used as a methanol raw material containing water, its stability is not good, and the selectivity and activity also decrease.

Method used

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  • A kind of preparation method of methanol dehydration production dimethyl ether catalyst
  • A kind of preparation method of methanol dehydration production dimethyl ether catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0033] (1) Catalyst preparation:

[0034] Weigh 145.8g of cetyltrimethylammonium bromide and 205g of citric acid to form a mixed solution, add 302mL tetraethyl orthosilicate to the mixed solution, stir for 2 h, and then stir at 70°C until coagulation Gel, the gel was aged at room temperature for 12 h, dried at 100 °C for 8 h, and then heat-treated at 200 °C for 2 h, the resulting solid was added to an aqueous solution containing 25.6 g of citric acid, stirred at 70 °C until the solution was evaporated to dryness, The obtained material was immersed in ammonium carbonate solution for 10 minutes, filtered and dried at 60°C, then added to a mixed aqueous solution containing 13.3g of lanthanum nitrate and 15.6g of phosphotungstic acid, stirred at 70°C until the solution was evaporated to dryness, and then The obtained solid was dried at 110°C for 8.0 h, and then calcined at 500°C for 3.0 h to obtain (NH 4 ) 0.5 h 2.5 PW 12 o 40 -La 2 o 3 / SiO 2 Catalyst, where La 2 o 3 Th...

Embodiment 2

[0040] Weigh 200g of cetyltrimethylammonium bromide and 105.7g of citric acid to make a mixed solution, add 250mL tetraethyl orthosilicate into the mixed solution, stir for 2 h, and then stir at 70°C until coagulation Gel, the gel was aged at room temperature for 12 h, dried at 100 °C for 8 h, and then heat-treated at 200 °C for 2 h, the resulting solid was added to an aqueous solution containing 42.3 g of citric acid, stirred at 70 °C until the solution was evaporated to dryness, The obtained material was immersed in ammonium carbonate solution for 10 minutes, filtered and dried at 60°C, then added to a mixed aqueous solution containing 37.2g of lanthanum nitrate and 20.8g of phosphotungstic acid, stirred at 70°C until the solution was evaporated to dryness, and then The obtained solid was dried at 110 °C for 8.0 h, and then calcined at 450 °C for 3.0 h to obtain (NH 4 ) 0.7 h 2.3 PW 12 o 40 -La 2 o 3 / SiO 2 Catalyst, where La 2 o 3 The content is 14wt%, (NH 4 ) 0....

Embodiment 3

[0043] Weigh 316g of cetyltrimethylammonium bromide and 62.4g of citric acid to form a mixed solution, add 246mL tetraethyl orthosilicate into the mixed solution, stir for 2 h, and then stir at 70°C until coagulation Gel, the gel was aged at room temperature for 12 h, dried at 100 °C for 8 h, and then heat-treated at 200 °C for 2 h, the resulting solid was added to an aqueous solution containing 62.4 g of citric acid, stirred at 70 °C until the solution was evaporated to dryness, The obtained material was immersed in ammonium carbonate solution for 10 minutes, filtered and dried at 60°C, then added to a mixed aqueous solution containing 26.6g of lanthanum nitrate and 25.9g of phosphotungstic acid, stirred at 70°C until the solution was evaporated to dryness, and then The obtained solid was dried at 110°C for 8.0 h, and then calcined at 520°C for 3.0 h to obtain (NH 4 ) 0.2 h 2.8 PW 12 o 40 -La 2 o 3 / SiO 2 Catalyst, where La 2 o 3 The content is 10wt%, (NH 4 ) 0.2 h...

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Abstract

The invention discloses a preparation method of a catalyst used for producing dimethyl ether through methanol dehydration. According to the invention, silicone gel-forming is carried out under the existence of a templating agent; processes such as heat treatment, organic acid impregnation, ammonium or ammonia gas treatment and the like are carried out; and an auxiliary agent and heteropolyacid are loaded. Therefore, the auxiliary agent and heteropolyacid are uniformly distributed on the outer surface of a carrier, and catalyst overall performance is improved. Therefore, the catalyst has relatively high activity and coking resistance as well as high selectivity, and catalyst stability is also improved.

Description

technical field [0001] The invention relates to a preparation method of a catalyst for methanol dehydration to produce dimethyl ether, in particular to a preparation method of a loaded heteropolyacid ammonium salt catalyst used for methanol dehydration to produce dimethyl ether. Background technique [0002] Dimethyl ether (Dimethy Ether, abbreviated as DME) is a colorless, non-toxic gas at normal temperature and pressure, which can be compressed into a liquid. Dimethyl ether is an important organic chemical raw material and chemical intermediate, which can be used in aerosols, refrigerants, alkylating agents, pharmaceuticals, cosmetics, fuels and other industries. [0003] Dimethyl ether was first produced by rectification of by-products in high-pressure methanol production, and soon developed into two processes of methanol dehydration and direct synthesis of synthesis gas. The liquid-phase method of methanol dehydration to produce dimethyl ether, the reaction is carried o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/26C07C41/09C07C43/04
Inventor 金浩孙素华朱慧红刘杰杨光
Owner CHINA PETROLEUM & CHEM CORP
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