Catalyst for methanol oxidation to methylal by one step, preparing method and applications thereof

A technology of oxidation synthesis and catalyst, which is applied in the preparation of organic compounds, physical/chemical process catalysts, molecular sieve catalysts, etc., can solve the problems of high price and limited practical application of catalysts, and achieve high selectivity, long life and good stability Effect

Inactive Publication Date: 2008-07-23
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the catalyst formulations described in U.S. Patent No. 6403841 and Chinese Patent CN1911503A introduce relatively expensive rhenium elements. Because the high-valent oxides of rhenium are easy to volatilize at high temperatures, the catalyst is deactivated, etc., which limits the actual use of this type of catalyst. application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 0.25 g of phosphomolybdic acid and 2.5 g of SBA-16 molecular sieve were carefully ground and mixed, and then calcined at 350° C. for 5 hours to obtain a catalyst with a content of phosphomolybdic acid of 7.48 wt % and a content of SBA-15 of 92.52 wt %.

[0028] Catalyst in 10vol% O 2 / Ar atmosphere at 350°C for 4 hours, lowered to 180°C, and then introduced methanol vapor preheated at 140°C with Ar and O 2 The mixed gas, the raw gas composition is CH 3 OH / O 2 / Ar=6.3 / 9.4 / 84.3, the reaction pressure is normal pressure, and the reaction gas space velocity is 4000ml / g cat .h, the reactivity of the catalyst is shown in Table 1.

Embodiment 2

[0030] Grind and mix 0.13g of phosphomolybdic acid and 2.5g of MCM-41 molecular sieve carefully, and roast at 550°C for 5h to obtain a catalyst with a content of phosphomolybdic acid of 4.03wt% and an MCM-41 content of 95.97wt%.

[0031] Catalyst in 10vol% O 2 / Ar 550°C for 1h, lower to 180°C, feed methanol steam and air preheated at 140°C, the raw gas composition is CH 3 OH / O 2 / Ar=6.3 / 9.4 / 84.3, the reaction pressure is normal pressure, and the reaction gas space velocity is 4000ml / g cat .h, the reactivity of the catalyst is shown in Table 1.

Embodiment 3

[0033] Dissolve 3.3g of phosphotungstic acid in deionized water, add 5.0g of HZSM-5 molecular sieve (Si / Al=60), impregnate at 50°C to form a viscous precursor, dry at 70°C for 24h, and then bake in air (300°C , 7h), the content of phosphotungstic acid was 36.46wt%, and the content of HZSM-5 was 63.54wt%.

[0034] Treat the catalyst at 300°C for 5 hours in an air atmosphere, lower it to 170°C, feed methanol steam and air preheated at 140°C, and the composition of the raw gas is CH 3 OH / O 2 / N 2 =10.0 / 18.0 / 72.0, the reaction pressure is normal pressure, and the reaction gas space velocity is 2000ml / g cat .h, the reactivity of the catalyst is shown in Table 1.

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Abstract

A methanol catalyst for the selective oxidation of methylal is composed of heteropoly acid and molecular sieve carrier, wherein, the heteropoly acid takes 3-45% of the catalyst by weight percentage, the metal content takes 0-5% of the catalyst by metal single mass, and remaining is silicon modular sieve. For the preparation of the catalyst, a mechanical mixing method, an immersion method, an in-situ synthesis method, and a surface grafting method are applied. The invention can realize the preparation of methylal by oxidation method in one step, shorten process flow and reduce production cost. Meanwhile, the catalyst is obviously characterized by high selectivity of methylal, good stability and long service life.

Description

technical field [0001] The invention belongs to a solid catalyst for synthesizing methylal by one-step oxidation of methanol, a preparation method and application thereof. technical background [0002] Methylal, also known as dimethoxymethane, is a green methanol downstream product with high added value, widely used in cosmetics, pharmaceuticals, automobiles, rubber and other fields. Its outstanding decontamination ability and volatility make it a new generation of environmentally friendly solvents recommended by the National Environmental Protection Agency; as a cleaning agent, methylal can replace chlorinated solvents and reduce the emission of volatile pollutants; at the same time, methylal It is an important raw material for the preparation of high-concentration formaldehyde (83.3%). In addition, because methylal has a high oxygen content and cetane number, it can effectively improve the combustion status of diesel in the engine, improve thermal efficiency, and reduce p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/03B01J27/19C07C43/303C07C41/50
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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