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Catalyst for producing methylal by one-step oxidation of methanol and its preparation method and application

A catalyst and methylal technology, which is applied in the field of one-step methanol oxidation to methylal catalyst and its preparation, can solve the problems of lower reaction economy, increased selectivity of carbon monoxide and carbon dioxide, and no DMM, etc., and achieve a good degree of dispersion , good stability

Active Publication Date: 2019-12-24
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the one-step oxidation of methanol to methylal is a thermodynamically unfavorable reaction, when the reaction temperature is high, the methanol conversion rate increases, but the selectivity of methylal (DMM) drops sharply, while the selectivity of formaldehyde and methyl formate When the temperature rises further, methanol will undergo deep oxidation, which will greatly increase the selectivity of carbon monoxide and carbon dioxide in the product, seriously reducing the economical efficiency of the reaction.
At present, the preparation of vanadium-titanium catalysts for the oxidation of methanol to methylal is the biggest difficulty in preparing catalysts with high performance at low temperatures and improving the selectivity of DMM as much as possible. However, so far, there is no DMM selectivity that can reach 100%. to report

Method used

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  • Catalyst for producing methylal by one-step oxidation of methanol and its preparation method and application
  • Catalyst for producing methylal by one-step oxidation of methanol and its preparation method and application
  • Catalyst for producing methylal by one-step oxidation of methanol and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Dissolve 4.0g vanadyl sulfate and 17.4g titanium sulfate in a three-necked flask filled with 300ml deionized water, and dissolve under stirring to obtain solution A; dissolve 15g cetyltrimethylammonium bromide (CTAB) in 500ml Heat and stir in deionized water for 30 minutes to obtain solution B; drop mixed solution A into solution B at a speed of 80 r / min to obtain mixed solution C containing preliminary precipitation. 40ml of ammonia water (25%) was dissolved in 360ml of deionized water to prepare an ammonia solution. Place C under an ice-water bath and stir vigorously, and drip an ammonia solution into the mixture C at a speed of 80 r / min until pH = 9.0, and obtain a slurry containing two-step precipitation, which is yellow-brown. Continue to stir for 0.5h, then leave it to age for 2h, wash it twice with 100ml of water, and filter with suction to get a tan filter cake, dry the filter cake at 110°C for 2h to get solid D, and roast solid D at 400°C After 6h, the catalys...

Embodiment 2

[0054] Dissolve 4.0g of vanadyl sulfate and 17.4g of titanium sulfate in a three-necked flask filled with 300ml of deionized water, and dissolve under stirring to obtain solution A; dissolve 25g of CTAB in 500ml of deionized water, heat and stir for 30min to obtain solution B; Mixed solution A was dropped into solution B at a speed of 80 r / min to obtain mixed solution C containing preliminary precipitation. 40ml of ammonia water (25%) was dissolved in 360ml of deionized water to prepare an ammonia solution. Place C under an ice-water bath and stir vigorously, and drip an ammonia solution into the mixture C at a speed of 80 r / min until pH = 9.0, and obtain a slurry containing two-step precipitation, which is yellow-brown. Continue to stir for 0.5h, then leave it to age for 2h, wash it twice with 100ml of water, and filter with suction to get a tan filter cake, dry the filter cake at 110°C for 2h to get solid D, and roast solid D at 400°C After 6h, the catalyst for the selectiv...

Embodiment 3

[0060] Dissolve 4.0g of vanadyl sulfate and 17.4g of titanium sulfate in a three-necked flask filled with 300ml of deionized water, and dissolve under stirring to obtain solution A; dissolve 35g of CTAB in 500ml of deionized water, heat and stir for 30min to obtain solution B; Mixed solution A was dropped into solution B at a speed of 80 r / min to obtain mixed solution C containing preliminary precipitation. 40ml of ammonia water (25%) was dissolved in 360ml of deionized water to prepare an ammonia solution. Place C under an ice-water bath and stir vigorously, and drip an ammonia solution into the mixture C at a speed of 80 r / min until pH = 9.0, and obtain a slurry containing two-step precipitation, which is yellow-brown. Continue to stir for 0.5h, then leave it to age for 2h, wash it twice with 100ml of water, and filter with suction to get a tan filter cake, dry the filter cake at 110°C for 2h to get solid D, and roast solid D at 400°C After 6h, the catalyst for the selectiv...

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Abstract

The invention discloses a catalyst for preparing methylal by means of one-step oxidation of methanol, and a preparation method and application of the catalyst. On the basis of taking the total quality of raw material components of the catalyst as a reference, the catalyst is prepared from the following raw material components by mass percent: 5-30% of a vanadium source, 30-60% of a titanium source and 20-62% of a surface active agent, wherein the vanadium source is vanadium oxide, and the titanium source is titanium oxide. The particle form of the catalyst is nano particles; the catalyst is good in degree of dispersion and stability, and has the advantages of being low in reaction temperature, easy to repeat and high in methylal selectivity.

Description

technical field [0001] The invention relates to the field of catalysts, in particular to a catalyst for preparing methylal by one-step oxidation of methanol prepared by a stepwise precipitation method, and a preparation method and application thereof. Background technique [0002] Methylal, also known as dimethoxymethane, is a high value-added downstream green chemical product of methanol, widely used in cosmetics, pharmaceuticals, automobiles, rubber and other fields; as a solvent, methylal has strong solubility and non-toxicity It can replace benzene, toluene, xylene, acetone and other solvents, and can be used as an additive in paints and varnishes, glues and adhesives, inks and various aerosol products, especially in the field of water-based wood coatings. Become one of the best choices for solvent replacement of water-based paints. At the same time, methylal is also an important chemical raw material for the preparation of high-purity formaldehyde; more importantly, me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/22C07C43/30C07C41/50
CPCB01J23/002B01J23/22C07C41/50C07C43/30
Inventor 司马蕊吴平刘子玉曾高峰张瑞芳刘国娟孙予罕
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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