Preparation method of pyridine-3-formaldehyde

A technology of formaldehyde and pyridine, which is applied in the field of preparation of pyridine-3-carbaldehyde, can solve the problem of low yield of pyridine-3-carbaldehyde, achieve strong industrial application value, simple preparation process, high reaction conversion rate and selectivity Effect

Inactive Publication Date: 2012-08-08
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The 3-picoline is vaporized and mixed with oxygen and water vapor, and directly oxidized to pyridine-3-carbaldehyde through a fixed-bed reactor equipped with a catalyst (Chemistry Letters, 2001, 8: 754-755), using the following method Chromium, aluminum, and vanadium are oxides of active components as catalysts, but the yield of pyridine-3-carbaldehyde obtained by this method is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Dissolve 8.0g of ammonium molybdate, 14.4g of bismuth nitrate, 1.6g of ferric nitrate, 4g of sodium nitrate and 16.0g of oxalic acid in 450ml of water, heat to 70°C, add 96g of titanium dioxide, stir and mix evenly, evaporate the water under reduced pressure, and put The obtained solid was ground, added an appropriate amount of water and extruded into strips, baked at 120°C for 2 hours, and then calcined at 600°C for 8 hours to obtain a black strip catalyst, which was folded into 3-4mm for use.

[0012] Pack the black strip catalyst prepared in the previous step into a fixed-bed reactor, keep the temperature of the fixed-bed reactor at 390°C, feed oxygen and water into the fixed-bed reactor, the flow rate of oxygen is 250mL / min, and the flow rate of water is 250mL / min. Flow rate is 0.2mL / min, and after 1 hour, continue to feed oxygen and mass concentration in the fixed bed reactor and be the aqueous solution of 20% 3-picoline, the aqueous solution flow rate of 3-picoline...

Embodiment 2

[0014] Dissolve 8.0g of ammonium molybdate, 8.8g of bismuth nitrate, 2.0g of cobalt nitrate, 2.4g of sodium hydroxide and 12.0g of citric acid in 450ml of water, heat to 60°C, add 84g of titanium dioxide, stir and mix well, evaporate to dryness under reduced pressure Finally, grind the obtained solid, add an appropriate amount of water and extrude it into a strip, bake it at 100°C for 3 hours, and then calcinate it at 500°C for 9 hours to obtain a black strip catalyst, which is folded into 3-4mm for use.

[0015] Pack the black strip catalyst prepared in the previous step into a fixed-bed reactor, keep the temperature of the fixed-bed reactor at 350°C, feed oxygen and water into the fixed-bed reactor, the flow rate of oxygen is 200mL / min, and the flow rate of water is 200mL / min. Flow rate is 0.18mL / min, and after 1 hour, continue to feed oxygen and mass concentration in fixed-bed reactor and be the aqueous solution of 10% 3-picoline, the aqueous solution flow rate of 3-picoline...

Embodiment 3

[0017] Dissolve 8.0g of ammonium molybdate, 2.4g of bismuth nitrate, 4.0g of chromium nitrate, 0.8g of potassium nitrate and 8.0g of tartaric acid in 450ml of water, heat to 80°C, add 72g of titanium dioxide, stir and mix evenly, evaporate the water under reduced pressure, Grind the obtained solid, add an appropriate amount of water and extrude it into strips, bake at 80°C for 4 hours, and then calcinate at 400°C for 10 hours to obtain a black strip catalyst, which is folded into 3-4mm for use.

[0018] Pack the black strip catalyst prepared in the previous step into a fixed-bed reactor, keep the temperature of the fixed-bed reactor at 290°C, feed oxygen and water into the fixed-bed reactor, the flow rate of oxygen is 100mL / min, and the flow rate of water is 100mL / min. Flow rate is 0.10mL / min, after 1 hour, continue to feed oxygen and mass concentration in fixed-bed reactor and be the aqueous solution of 5% 3-picoline, the aqueous solution flow rate of 3-picoline is 0.10mL / min,...

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PUM

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Abstract

The invention discloses a preparation method of pyridine-3-formaldehyde. The preparation method mainly comprises the following steps: preparing a supported catalyst by treating ammonium molybdate, bismuth nitrate and a transition metallate as active component precursors and titanium dioxide as a carrier and adjusting by an acid adjusting agent and an organic complexing agent; and carrying out a gas phase catalytic oxidation reaction on 3-methylpyridine, oxygen and water which are used as raw materials in a fixed bed at 290-390DEG C to generate crude pyridine-3-formaldehyde, and extracting, distilling and rectifying the crude pyridine-3-formaldehyde to obtain a product containing above 98% of pyridine-3-formaldehyde. The preparation method of the invention, which has the advantages of simple preparation process, high catalytic reaction activity and selectivity, and low cost, is suitable for industrialized production.

Description

technical field [0001] The invention relates to a preparation method of pyridine-3-carbaldehyde, in particular to a method for preparing pyridine-3-carbaldehyde by catalytically oxidizing 3-picoline in a fixed bed gas phase. Background technique [0002] Pyridine-3-carboxaldehyde is an important fine chemical raw material. In medicine, it is mainly used in the synthesis of anticancer drugs resveratrol derivatives, camelamine derivatives, quinazoline derivatives, antihypertensive drugs imidazole Phenoline derivatives, sinomenine derivatives for the treatment of rheumatic pain and arthritis drugs, flavonoid compounds with various activities and pharmacological effects such as antibacterial, anti-inflammatory, anti-oxidation, anti-allergy, anti-virus, anti-cancer, etc.; in terms of pesticides, it It is mainly used to synthesize new neonicotinoid insecticides and aurone herbicides; in addition, it can also be used to synthesize some important drug intermediates such as chiral ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/48B01J23/887B01J23/31
Inventor 戴立言俞杰王晓钟陈英奇
Owner ZHEJIANG UNIV
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