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A kind of method of producing pyridine compound

A technology of compound and pyridine, which is applied in the field of liquid-phase continuous preparation of pyridine compounds mainly composed of 3-picoline, can solve the problems of easy deactivation of catalysts, and achieve the effects of improving production efficiency, improving utilization rate and saving energy

Active Publication Date: 2011-12-28
浙江爱迪亚营养科技开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

One is recovered from coal coking by-products; the other uses acetaldehyde, formaldehyde and ammonia as raw materials to synthesize 3-picoline by gas phase method, but this method is mixed with a large amount of pyridine, and the catalyst is easily deactivated. Requires frequent regeneration

Method used

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  • A kind of method of producing pyridine compound
  • A kind of method of producing pyridine compound

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Four 2L autoclaves are used to form a reactor according to the process flow chart. Add 500 grams of catalyst to the first three autoclaves, respectively add 1200 grams of 50% ethanol aqueous solution to the four autoclaves, start stirring, and heat up to 228 ° C. Turn on the high-pressure metering pumps of No. 1, No. 2, and No. 3 autoclaves, and inject the pre-prepared raw materials (aqueous solution containing 16.3% urotropine, 32% paraldehyde, and 31% ethanol) into the first three autoclaves respectively. Inside, the control pressure is 4.0Mpa. The flow rates are 400 g / h, 350 g / h, and 300 g / h respectively, and the No. 4 autoclave keeps the liquid level stable. Continuous feed 300 hours, obtain altogether 48.99 kilograms of 3-methylpyridines, 1.06 kilograms of pyridines, 2.25 kilograms of 2,5-lutidines, 2.52 kilograms of 3,5-lutidines, 6.63 kilograms of 3-ethylpyridines, 0.8 kg of 2-methyl-5-ethylpyridine.

Embodiment 2

[0024] Four 2L autoclaves are used to form a reactor according to the process flow chart. Add 500 grams of catalyst to the first three autoclaves, respectively add 1200 grams of 50% ethanol aqueous solution to the four autoclaves, start stirring, and heat up to 232 ° C. Turn on the high-pressure metering pumps of No. 1, No. 2, and No. 3 autoclaves, and inject the pre-prepared raw materials (aqueous solution containing 16.3% urotropine, 32% paraldehyde, and 31% ethanol) into the first three autoclaves respectively. Inside. The flow rate is 500 g / h, 450 g / h, 400 g / h respectively, the control pressure is 4.3Mpa, and the No. 4 autoclave keeps the liquid level stable. Continuous feed 300 hours, obtain altogether 54.54 kilograms of 3-methylpyridines, 1.18 kilograms of pyridines, 2.51 kilograms of 2,5-lutidines, 2.83 kilograms of 3,5-lutidines, 7.38 kilograms of 3-ethylpyridines, 0.89 kg of 2-methyl-5-ethylpyridine.

Embodiment 3

[0026] Four 2L autoclaves are used to form a reactor according to the process flow chart. Add 500 grams of catalyst to the first three autoclaves, respectively add 1200 grams of 50% ethanol aqueous solution to the four autoclaves, start stirring, and heat up to 220 ° C. Turn on the high-pressure metering pumps of No. 1, No. 2, and No. 3 autoclaves, and inject the pre-prepared raw materials (aqueous solution containing 16.3% urotropine, 32% paraldehyde, and 31% ethanol) into the first three autoclaves respectively. Inside. The flow rate is 400 g / h, 350 g / h, 300 g / h respectively, the control pressure is 3.6Mpa, and the No. 4 autoclave keeps the liquid level stable. Continuous feed 300 hours, obtain altogether 41.39 kilograms of 3-methylpyridines, 0.95 kilograms of pyridines, 1.98 kilograms of 2,5-lutidines, 2.12 kilograms of 3,5-lutidines, 6.01 kilograms of 3-ethylpyridines, 0.71 kg of 2-methyl-5-ethylpyridine.

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Abstract

The invention relates to a method for producing a pyridine compound. The method comprises the following steps: respectively placing a 50% ethanol aqueous solution in four reaction kettles, respectively placing a solid catalyst in the first three reaction kettles, and simultaneously heating the four reaction kettles to 220-230 DEG C; respectively putting a raw material prepared in advance to the bottoms of the inner cavities of the first three reaction kettles through pipelines; mixing liquid flowing out of the outlet of the NO.1 reaction kettle with the raw material in the NO.2 reaction kettle and then flowing to the bottom of the inner cavity of the NO.2 reaction kettle together; mixing the liquid flowing out of the outlet of the NO.2 reaction kettle with the raw material in the NO.3 reaction kettle and then flowing to the bottom of the inner cavity of the NO.3 reaction kettle together; and enabling the liquid flowing out of the NO. 3 reaction kettle to flow into the NO.4 reaction kettle through the pipeline; controlling the pressure and liquid level of the NO.4 reaction kettle, and continuously feeding material for 300 hours; and distilling the liquid flowing out of the NO.4 reaction kettle so as to obtain the pyridine compound which mainly contains 3-methylpyridine. The method has the advantages that through continuous liquid phase reaction, production efficiency is greatlyimproved, the utilization of equipment is improved, and the utilization of energy is improved to a large degree.

Description

technical field [0001] The invention relates to a method for continuously preparing pyridine compounds mainly composed of 3-picoline in liquid phase. Background technique [0002] Pyridine compounds are a class of very important chemical intermediates, especially 3-picoline. 3-picoline, also known as β-picoline and 3-picoline, is used as an intermediate for the insecticides imidacloprid and acetamiprid in pesticides, and is used to synthesize the next step intermediate 3-picoline-N- oxide. Mainly used to make vitamin B 6 , nicotinic acid and nicotinamide, nicolamine and cardiotonic agents; it can also be used as solvents, alcohol denaturants, dye intermediates, resin intermediates, rubber vulcanization accelerators, insecticides, waterproofing agents, and film sensitizers agent additives. [0003] There are two methods of production of 3-picoline. One is recovered from coal coking by-products; the other uses acetaldehyde, formaldehyde and ammonia as raw materials to syn...

Claims

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Application Information

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IPC IPC(8): C07D213/16C07D213/10
Inventor 陈启明应国海黄上马傅康炜
Owner 浙江爱迪亚营养科技开发有限公司
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