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Preparation method for 2,4,6-trimethyl pyridine

A kind of technology of collidine, collidine sulfate, applied in the field of chemistry, can solve the problems of rising cost, waste of resources, low industrial value and the like

Active Publication Date: 2012-03-14
上海鼎素精细化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved by the present invention is that the solvent in the existing method is absolute ethanol, but absolute ethanol is not easy to be used repeatedly, thus causing problems such as increased cost, waste of resources, and low industrial value

Method used

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Embodiment Construction

[0018] The present invention is a method for preparing 2,4,6-collidine applied in the field of chemistry, and is a significant improvement based on the shortcomings of existing methods for preparing 2,4,6-collidine. has very important practical significance.

[0019] 1. Selection of raw materials

[0020] The 2,4,6-collidine fraction is extracted by the primary rectification of the pyridine raw material at 167-173° C., wherein the 2,4,6-collidine content is 50-70%.

[0021] 2. Selection of solvent

[0022] 2.1 Selection of solvent types

[0023] The solvent in the existing preparation method is dehydrated alcohol, but dehydrated alcohol is not easy to be used repeatedly. The invention uses 95% industrial ethanol as a solvent for recrystallization, and after the test, it is found that the effect is not much different from the original one, and the cost is lower, it can be used repeatedly, and has industrial value.

[0024] 2.2 Selection of solvent dosage

[0025] The key t...

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Abstract

The invention discloses a preparation method for 2,4,6-trimethyl pyridine. The method comprises the following steps of: adding raw materials of 2,4,6-trimethyl pyridine, an industrial ethanol solvent and concentrated sulfuric acid into a reactor, and reacting with stirring till crystals are formed in the reactor; filtering or performing suction filtering; washing the crystals including a part of impurities at high temperature after filtering; and recrystallizing the crystal lattice of 2,4,6-trimethyl pyridine sulfate including a part of impurities after filtering. The invention has the advantages: according to basic property of a pyridine-series compound, by performing vitriolization, crystallization in ethanol, recrystallization and alkaline hydrolysis and purifying 2,4,6-trimethyl pyridine from a crude 2,4,6-trimethyl pyridine fraction extracted by primary rectification, the concentration of refined 2,4,6-trimethyl pyridine can be increased to 97-98 percent, the recovering rate is not lowered greatly, and the concentration can be increased to over 99 percent in further recrystallization.

Description

technical field [0001] The invention relates to a method for preparing chemical products in the field of chemistry, in particular to a method for preparing 2,4,6-collidine refined by recrystallization. Background technique [0002] As we all know, the key to the purification of 2,4,6-collidine by recrystallization is to select a suitable recrystallization solvent so as to dissolve as many other compounds as possible while precipitating 2,4,6-collidine salt crystallization. Impurities. What used in the existing preparation method is dehydrated alcohol as recrystallization solvent, in the ethanol solution of 2,4,6-collidine, add 98% concentrated sulfuric acid to react with it, generate sulfonate, through After cooling and filtering the crystals, the obtained crystals were recrystallized with 3 times the weight of ethanol. Use ammonia water to decompose to ph=8 at room temperature, and rectify it to obtain 2,4,6-collidine with a purity of more than 95%. [0003] However, the...

Claims

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Application Information

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IPC IPC(8): C07D213/16
Inventor 谢解锋杨泽静周磊磊孙迦宾
Owner 上海鼎素精细化工有限公司
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