Method of producing anhydrous formaldehyde through oxygen-free dehydrogenation

An anhydrous formaldehyde and dehydrogenation technology, which is used in the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of organic compounds, etc. problems, to achieve the effect of good catalyst stability, improved selectivity and purity, and large active surface area

Active Publication Date: 2016-07-06
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The significance of the present invention is to overcome the shortcomings of the catalysts currently used in the preparation of anhydrous formaldehyde, such as: the distribution of copper particles in the copper-based catalyst is uneven, the particles are large, the active surface are

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Weigh 5g of ZSM-5 and add it to 30mL of 0.5mol / L ammonium fluorosilicate aqueous solution, stir at 80°C for 6h, filter and wash, repeat this process 3 times, and dry at 100°C for 10h to obtain the dealuminated molecular sieve carrier . Weigh 1.9g of copper nitrate trihydrate, 2.3g of zinc nitrate hexahydrate and the ZSM-5 molecular sieve after the dealumination were added to 250mL of water, stirred at 80°C for 30min, and prepared 1mol / L sodium carbonate solution to adjust the pH of the above system to 8 , continue to stir for 30 minutes, filter while hot, wash with 1 L of hot water at 80°C until neutral, and dry it in an oven at 80°C overnight. Calcined at 550°C for 4 hours in air to obtain the copper-based catalyst. Weigh 2 g of the catalyst to form a tablet, sieve to 14-25 mesh, and fill it into a quartz tube reactor. At 600°C, methanol was pre-reduced to activate the copper-based catalyst for 1 hour. Under normal pressure, nitrogen gas was used as the carrier gas, ...

Embodiment 2

[0018] Weigh 5g of NaY molecular sieve and add it to 30mL of 0.5mol / L ammonium fluorosilicate aqueous solution, stir at 100°C for 6h, filter and wash, repeat this process 3 times, and dry at 100°C for 10h to obtain the dealuminated molecular sieve carrier . Weigh 0.8g of chromium nitrate nonahydrate, 1.9g of copper nitrate trihydrate, 2.3g of zinc nitrate hexahydrate, and the NaY-type molecular sieve after dealumination, add them to 250mL of water, stir at 80°C for 30min, and prepare a 1mol / L sodium carbonate solution Adjust the pH of the above system to 8, continue to stir for 30 minutes, filter while hot, wash with 1L of 80°C hot water until neutral, and dry it in an oven at 120°C overnight. Calcined at 650°C for 4 hours in air to obtain the copper-based catalyst. Weigh 2 g of the catalyst to form a tablet, sieve to 14-25 mesh, and fill it into a quartz tube reactor. At 600°C, methanol was pre-reduced to activate the copper-based catalyst for 1 h. Under normal pressure, ni...

Embodiment 3

[0020]Weigh 5g of HY molecular sieve and add it to 30mL of 0.5mol / L sodium fluorosilicate aqueous solution, stir at 80°C for 6h, filter and wash, repeat this process 3 times, and dry at 100°C for 10h to obtain the dealuminated molecular sieve carrier. Weigh 1.9g of copper nitrate trihydrate, 2.3g of zinc nitrate hexahydrate and the above-mentioned dealuminated HY molecular sieve into 250mL of water, stir at 80°C for 30min, prepare a 1mol / L potassium carbonate solution to adjust the pH of the above system to 8, continue Stir for 30 minutes, filter while hot, wash with 1L of 80°C hot water until neutral, and dry it in an oven at 150°C overnight. Calcined at 600°C for 4 hours in air to obtain the copper-based catalyst. Weigh 2 g of the catalyst to form a tablet, sieve to 14-25 mesh, and fill it into a quartz tube reactor. At 600°C, methanol was pre-reduced to activate the copper-based catalyst for 1 hour. Under normal pressure, nitrogen gas was used as the carrier gas, and 40 vo...

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PUM

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Abstract

The invention relates to a method of producing anhydrous formaldehyde through oxygen-free dehydrogenation. A copper based catalyst is employed in the method and is arranged in a quartz reaction tube, wherein the quartz reaction tube is placed in a fixed bed reactor. Before reaction, at a certain temperature, the copper based catalyst is pre-reduced with methanol or hydrogen. Under normal pressure, the methanol is fed through a constant-flux pump with inert gas as a carrier gas to carry out a reaction at 400-700 DEG C, wherein the methanol is subjected to oxygen-free dehydrogenation to obtain formaldehyde. The copper based catalyst includes, by mass, 1-20 parts of copper, 100 parts of a dealuminated molecular sieve carrier, and 0-20 parts of a co-catalyst. Chromatography detection proves that methanol conversion is 45-99% and methanol selectivity is 30-95%. The catalyst is a copper based catalyst supported on chemically-dealuminated molecular sieve. The catalyst integrates both high specific surface area of the carrier molecular sieve and high activity of the copper based catalyst, and has high catalytic activity and thermal stability, less generation of side products and simple preparation process.

Description

technical field [0001] The invention belongs to the field of preparing anhydrous formaldehyde, in particular to a method for preparing anhydrous formaldehyde through anaerobic dehydrogenation. Background technique [0002] Formaldehyde is an important organic chemical raw material, which can be used to produce thermosetting resins such as phenolic resin and melamine resin, as well as various chemical products such as urotropine and 1,4-butanediol. Formaldehyde is also a synthetic dye, pesticide, fine and An important raw material for specialty chemicals. [0003] At present, methanol oxidation is generally used in industry to prepare formaldehyde. The produced formaldehyde contains a large amount of water, and the vapor pressure of formaldehyde aqueous solution is low, and formaldehyde and water can easily form an azeotrope. Therefore, formaldehyde is separated and purified. Very difficult, resulting in large energy consumption and high cost. In recent years, there is an i...

Claims

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Application Information

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IPC IPC(8): C07C47/04C07C45/00B01J29/46B01J29/14B01J29/85B01J35/10
Inventor 王峰王业红徐杰李利花张健张志鑫张晓辰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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