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Metallic catalyst for synthesizing dimethoxym ethane and methyl formate and production method thereof and use

A technology of metal catalyst and methyl formate, which is applied in the direction of metal/metal oxide/metal hydroxide catalyst, carboxylate preparation, molecular sieve catalyst, etc., can solve the problem of low production capacity of methyl formate, harsh reaction conditions and pollution and other problems, to achieve the effect of uniform distribution of active components, good stability and simple process flow

Inactive Publication Date: 2008-12-24
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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AI Technical Summary

Problems solved by technology

The production capacity of methyl formate produced by the direct synthesis method of syngas is low and the reaction conditions are harsh
The methanol vapor phase dehydrogenation method is mainly carried out on copper-based catalysts, but because copper is easy to aggregate, causing phase change and deactivation, the stability of the catalyst is mainly improved by adding chromium trioxide, etc., and metal chromium is an environmentally harmful polluting elements

Method used

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  • Metallic catalyst for synthesizing dimethoxym ethane and methyl formate and production method thereof and use

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 5mlTiCl under nitrogen protection atmosphere 4 , 3.1gNH 4 VO 3 and 0.12g (NH 4 ) 2 WO 4 In 26ml concentrated HNO 3 , stir to make it completely dissolve, add 23g urea and 14gMCM-41, and then rapidly roast at 500°C for 10min under air atmosphere to get V 2 o 5 -TiO 2 The content is 30wt% (V 2 o 5 / TiO 2 The mass ratio is 40 / 60), WO 3 The content is 0.5wt%, MCM-41 content is 69.5wt% of WO 3 -V 2 o 5 -TiO 2 / MCM-41 catalyst.

[0022] Catalyst at 10vol% O 2 / Ar atmosphere is activated at 400°C for 1.5h, and lowered to a reaction temperature of 130°C, then methanol is preheated to 120°C by a preheater and then gasified and mixed with oxygen-containing gas to form a raw material gas. The volume ratio composition of the raw material gas is CH 3 OH / O 2 / Ar=10.0 / 9.0 / 81.0, the space velocity of the raw material gas in the reaction gas is 11300ml / g cat .h, the reaction is carried out under the condition of working pressure of 0.1MPa. After the reaction produ...

Embodiment 2

[0024] Add 5mlTiCl under nitrogen protection atmosphere 4 and 0.70gNH 4 VO 3 In 11.33ml concentrated HNO 3 After stirring to dissolve completely, add 68g of citric acid, and then quickly roast at 450°C for 15min under air atmosphere to get V 2 o 5 / TiO 2 Catalyst with a mass ratio of 20 / 80.

[0025] The catalyst is activated at 350°C for 2.0 hours in an air atmosphere, and then lowered to a reaction temperature of 125°C, then methanol is preheated to 110°C by a preheater and gasified, and then mixed with oxygen-containing gas to form a raw material gas. The volume ratio of the raw material gas is as follows: CH 3 OH / air=5.2 / 94.8, the space velocity of raw material gas in reaction gas is 8100ml / g cat .h, the reaction is carried out under the condition of working pressure of 0.1MPa. After the reaction product is cooled and separated, the oxygen-containing reaction gas and the product with low boiling point are separated for recovery and purification, and the product with ...

Embodiment 3

[0027] Add 10ml TiCl under nitrogen protection atmosphere 4 , 4.01gNH 4 VO 3 and 0.41gCu(NO 3 ) 2 In 50ml concentrated HNO 3 In, stir to make it dissolve completely, then add 100g citric acid and 7.0g ZrO 2zirconium sol, and then rapidly calcined at 550 ° C for 8 min in an air atmosphere to obtain V 2 o 5 -TiO 2 The content is 60wt% (V 2 o 5 / TiO 2 Mass ratio is 30 / 70), CuO content is 1.0wt%, ZrO 2 39 wt% CuOV 2 o 5 -TiO 2 / ZrO 2 catalyst.

[0028] Activate the catalyst at 500°C for 1.0h in the air atmosphere, and lower it to the reaction temperature of 155°C, then methanol is preheated to 140°C by the preheater and gasified, then mixed with oxygen-containing gas to form the raw material gas, the volume ratio composition of the raw material gas is CH 3 OH / air=3.0 / 97.0, the space velocity of the raw material gas in the reaction gas is 2000ml / g cat .h, the reaction is carried out under the condition of working pressure of 0.3MPa. After the reaction product is c...

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Abstract

The present invention relates to a metal catalyst synthesizing methylal and methyl formate. In weight percentage of the metal catalyst, the content of vanadium is calculated by the weight of V2O5; the content of titanium is calculated by the weight of TiO2; the weight proportion of the V2O5 and the TiO2 in the catalyst is 5 to 70 to 30 to 95; the V2O5 and the TiO2 take 20 percent to 100 percent of the catalyst in weight percentage; the content of accessory ingredient is calculated by the content of the oxide of the accessory ingredient and takes 0wt percent to 2.0wt percent of the catalyst in weight percentage; support takes 0wt percent to 78wt percent of catalyst in weight percentage. The catalyst has the advantages of high methanol conversion rate, the high selectivity of the methylal and the methyl formate, the good stability of the catalyst and long life.

Description

technical field [0001] The invention belongs to an ultra-fine multi-metal catalyst used for synthesizing methylal and methyl formate in one-step method of oxidation of methanol, as well as its preparation method and application process. technical background [0002] Methylal, also known as dimethoxymethane (DMM), is a high value-added green downstream product of methanol, widely used in cosmetics, pharmaceuticals, automobiles, rubber and other fields; as a fuel additive, DMM can effectively improve the performance of diesel fuel in engines. The combustion state in the air can improve the thermal efficiency and reduce the emission of pollutants. At present, the DMM synthesis method is mainly based on methanol as a raw material through a two-step synthesis method, that is, methanol is first oxidized to formaldehyde, and then formaldehyde and methanol are further condensed to form methylal. The technical process of two-step synthesis of methylal is relatively mature, but its p...

Claims

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Application Information

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IPC IPC(8): B01J29/78B01J23/22B01J21/06B01J23/847B01J27/053C07C41/50C07C43/30C07C67/40C07C69/06
Inventor 孙予罕郭荷芹李德宝李文怀
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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