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Catalyst for oxidizing and synthesizing dimethoxymethane by methyl alcohol as well as preparation method and application thereof

A technology for the oxidation of dimethoxymethane and methanol, which is applied in the direction of metal/metal oxide/metal hydroxide catalysts, preparation of organic compounds, physical/chemical process catalysts, etc., and can solve the problem of methylal selectivity of methanol conversion rate Problems that need to be improved, such as limiting the large-scale production and application of DMM, and the complicated DMM process, can achieve the effects of stable structure, long life and simple process flow

Active Publication Date: 2014-07-23
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional two-step method to prepare DMM is complex and costly, which limits the large-scale production and application of DMM.
In recent years, the research on the one-step synthesis of DMM by methanol oxidation has attracted great attention. The catalysts for the synthesis of dimethoxymethane by the one-step oxidation of methanol have been reported: U.S. Patent US6403841, using SbRe 2 o 6 Catalyst; Chinese patent CN101327444B, V prepared by combustion method 2 o 5 / TiO 2 Add catalyst as promoter, but catalyst preparation, activity, stability, conversion rate to methanol and selectivity to methylal need to be improved

Method used

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  • Catalyst for oxidizing and synthesizing dimethoxymethane by methyl alcohol as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Catalyst preparation: Add 3.89g ammonium metavanadate, 8.36mL titanium tetrachloride, 15.86g zirconium oxychloride, 5.86mL malonic acid to 200mL, 12mol / L concentrated hydrochloric acid and 200mL deionized aqueous solution, heat and stir to dissolve, Obtain a transparent solution; the above solution was rapidly heated at 120°C in the air for 40min, then dried at 120°C for 24h, and then the product was roasted at 450°C for 12h to obtain a vanadium oxide content of 20%, a titanium oxide content of 40%, and a zirconium oxide content of 40%. Catalyst with a content of 40% is named 20VTi 0.40 Zr 0.40 .

[0024] Catalyst application: the catalyst in 7vol%O 2 / Ar atmosphere at 80ml.min -1 Activation at 400°C for 4 hours at a flow rate, then lowered to 80°C, the methanol liquid is preheated to 100°C by a preheater and vaporized to form a raw material gas with a mixed gas containing oxygen. The volume ratio of the raw material gas is N 2 :O 2 :CH 3 OH=84.15:9.35:6.50, the r...

Embodiment 2

[0026] Catalyst preparation: Add 4.68g sodium metavanadate, 6.69mL titanium sulfate, 12.24g cerium nitrate, 3.96mL oxalic acid to 200mL, 16mol / L concentrated nitric acid and 200mL deionized aqueous solution, heat and stir to dissolve to obtain a transparent solution; the above solution After rapidly heating at 100°C in the air for 30 minutes, drying at 130°C for 36 hours, and then roasting the product at 400°C for 13 hours, to obtain a product with a vanadium oxide content of 28%, a titanium oxide content of 37%, and a cerium oxide content of 35%. Catalyst, named 28VTi 0.37 Ce 0.35 .

[0027] Catalyst application: the catalyst in 10vol%O 2 / Ar atmosphere 70ml.min -1 Activation at 350°C for 10 hours at a flow rate, and then lowered to 100°C, the methanol liquid is preheated to 110°C by a preheater and vaporized to form a raw material gas with a mixed gas containing oxygen. The volume ratio composition of the raw gas is N 2 :O 2 :CH 3 OH=82.8:9.2:8.0, the raw material gas ...

Embodiment 3

[0029] Catalyst preparation: Add 5.41g potassium metavanadate, 6.69mL titanium isopropoxide, 22.31g aluminum nitrate, 14.55g citric acid to 250mL, 16mol / L concentrated nitric acid and 250mL deionized aqueous solution, heat and stir to dissolve to obtain a transparent solution After the above-mentioned solution was rapidly heated at 120° C. for 30 minutes in the air, it was dried at 120° C. for 15 hours, and then the resulting product was roasted at 400° C. for 12 hours to obtain a vanadium oxide content of 21%, a titanium oxide content of 47%, and an aluminum oxide content of 32% catalyst, named 21VTi 0.47 Al 0.32 .

[0030] Catalyst application: put the catalyst in 12vol%O 2 / Ar atmosphere 80ml.min -1 Activation at 400°C for 5 hours at a flow rate, and then lowered to 100°C, the methanol liquid is preheated to 120°C by a preheater and vaporized to form a raw material gas with a mixed gas containing oxygen. The volume ratio composition of the raw gas is N 2 :O 2 :CH 3 OH...

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Abstract

The invention discloses a catalyst for oxidizing and synthesizing dimethoxymethane by methyl alcohol. The catalyst for oxidizing and synthesizing dimethoxymethane by methyl alcohol consists of vanadium oxide serving as a main catalytic active component, titanic oxide serving as an auxiliary catalytic active component and auxiliary metallic oxide with the composition in mass percentage: 6-60wt% of V2O5, 40-95wt% of TiO2 and 0-55wt% of auxiliary metallic oxide. The catalyst for oxidizing and synthesizing dimethoxymethane by methyl alcohol, which is provided by the invention, has the advantages of simple method, mild reaction condition, good stability, easiness in reproducibility, and high dimethoxymethane selectivity and methyl alcohol conversion rate.

Description

technical field [0001] The invention belongs to a catalyst for synthesizing dimethoxymethane, a preparation method and application thereof, in particular to a composite carrier nano-multimetal catalyst for synthesizing dimethoxymethane by direct oxidation of methanol and its preparation method and application. Background technique [0002] Dimethoxymethane, also known as methylal, the English name is dimethoxymethane (DMM) or methylal, and the structural formula is CH 3 O-CH 2 -OCH 3 . Dimethoxymethane is a high value-added downstream product of methanol. It is colorless, non-toxic and environmentally friendly. It has good decontamination ability and volatility. It is a green chemical product widely concerned by the world. At present, dimethoxymethane is widely used in cosmetics, pharmaceuticals, automobiles, rubber and other fields, and dimethoxymethane has a relatively high oxygen content and cetane number, adding 5% to 10% to diesel Dimethoxymethane can improve diese...

Claims

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Application Information

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IPC IPC(8): B01J23/22B01J23/28C07C43/30C07C41/50
Inventor 房克功范志宏孙予罕
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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