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Method for preparing dimethoxymethane by adopting supported niobium oxide catalyst

A catalyst and niobium oxide technology, which is applied in the field of catalysis, can solve the problems of low operating temperature of strong acid cation exchange resin catalyst, complicated preparation process of composite solid super acid catalyst, and corrosion of equipment, etc.

Inactive Publication Date: 2011-04-06
CHINA NAT OFFSHORE OIL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved in the present invention is to overcome the previous reports, in the process of preparing methylal, the liquid acid catalyst used corrodes equipment and pollutes the environment, the use temperature of the strong acid cation exchange resin catalyst is low, and the preparation of conventional composite solid superacid catalyst The shortcomings of complex process and easy loss provide a method for preparing methylal by the reaction of methanol and formaldehyde catalyzed by loaded niobium oxide

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] At 50°C, 7.1g of niobic acid, which had been washed three times with distilled water and dried at 120°C, was dissolved in 200mL of oxalic acid solution with a mass concentration of 20%, to obtain a 0.20mol / L niobium oxalate solution, and then 320g of niobium oxalate was added. Activated alumina balls of φ1.6~2.0mm are impregnated with equal volume while hot. Stand at room temperature for 24 hours, dry at 120° C. for 24 hours, and bake at 550° C. for 5 hours in an air atmosphere to obtain catalyst A with a niobium oxide loading of 1.6%.

Embodiment 2

[0025] At 50°C, 9.3g of niobic acid, which had been washed three times with distilled water and dried at 120°C, was dissolved in 200mL of oxalic acid solution with a mass concentration of 20%, to obtain a 0.26mol / L niobium oxalate solution, and then 320g of niobium oxalate was added. Activated alumina balls of φ1.6~2.0mm are impregnated with equal volume while hot. Stand at room temperature for 24 hours, dry at 120° C. for 24 hours, and bake at 550° C. for 5 hours in an air atmosphere to obtain catalyst B with a niobium oxide loading of 2.1%.

Embodiment 3

[0027] At 50°C, 3.1g of niobic acid, which was washed three times with distilled water and dried at 120°C, was dissolved in 200mL of oxalic acid solution with a mass concentration of 20%, to obtain a 0.09mol / L niobium oxalate solution, and then 320g of niobium oxalate was added. Activated alumina balls of φ1.6~2.0mm are impregnated with equal volume while hot. Stand at room temperature for 24 hours, dry at 120° C. for 24 hours, and bake at 550° C. for 5 hours in an air atmosphere to obtain catalyst C with a niobium oxide loading of 0.7%.

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Abstract

The invention discloses a method for preparing polyformaldehyde dimethyl ether by adopting a supported niobium oxide catalyst, which is characterized by comprising the following steps of: a) performing catalytic reaction to prepare the polyformaldehyde dimethyl ether, wherein a molar ratio of the dimethoxymethane to trioxymethylene is 0.5 to 5; supported niobium oxide is taken as a catalyst and accounts for 0.1 to 5 percent based on the total mass of reactants; the reaction temperature is between 100 and 200 DEG C; the time is between 10 minutes and 48 hours; and the reaction pressure is between 0.1 and 10MPa; b) performing rectification separation, namely separating a low-boiling point component dimethoxymethane DMM, polydiformaldehyde dimethyl ether DMM2 and the unreacted trioxymethylene, and separating polyformaldehyde diformaldehyde DMM3-8, wherein a kettle bottom is provided with high-polymerization degree polyformaldehyde dimethyl ether DMMn, and n is more than 8; and c) adding a small amount of fresh trioxymethylene into the dimethoxymethane, the diformaldehyde dimethyl ether DMM2 and the unreacted trioxymethylene which are separated in the step b and continuously reacting to prepare the polyformaldehyde diformaldehyde DMM3-8, which is suitable to be used as a diesel fuel-blended component so as to improve the utilization rate of the raw materials.

Description

Technical field: [0001] The invention relates to the technical field of catalysis, and is a method for preparing methylal by using a supported niobium oxide catalyst; specifically, it is a method for preparing methylal from methanol and formaldehyde in the presence of a supported niobium oxide catalyst. Background of the invention: [0002] Methylal is an important downstream product of formaldehyde, and its production methods and application technologies are constantly being developed and improved. Especially in today's increasingly tense petroleum resources, methylal, as one of the important derivatives of coal chemical industry, has been widely used in methanol-based fuels, diesel additives, fuel cells and liquid fuels in addition to being used as a solvent. It has attracted widespread attention at home and abroad. [0003] Initially, the laboratory prepared methylal by heating formaldehyde and methanol in the presence of concentrated sulfuric acid and other liquid acids...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/20C07C43/30C07C41/56
Inventor 孙彦民李晓云于海斌苗静曾贤君李世鹏
Owner CHINA NAT OFFSHORE OIL CORP
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