Method for manufacturing catalyst used for synthesizing 2-picoline

A technology of picoline and catalyst, which is applied in the field of catalysts for the synthesis of 2-picoline, which can solve the problems of large influence on catalyst activity, fear of heat and easy decomposition, and high activity of crystalline cobaltocene

Active Publication Date: 2008-01-23
HEBI SAIKE CHEM ENG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] 2-picoline is an intermediate in the chemical industry, mainly used in medicine and other industries. The 2-picoline currently used in my country is mainly imported. The key problem in its synthesis is the catalyst dicobaltene used in the synthesis process. Both are crystalline cobaltocenes, and their production process is relatively complicated, and the process conditions are harsh. The final crystallized cobaltocenes need to be realized under high vacuum conditions.
In particular, it should be pointed out that the activity of crystalline cobaltocene is very high, it is afraid of light, heat and easy to decompose, afraid of acid gas, easy to oxidize and sp

Method used

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Embodiment Construction

[0013] The steps of the specific embodiment of the present invention are as follows (parts are parts by weight): a. Add 4.5 to 11.4 parts of tetrahydrofuran and 0.60 to 1.64 parts of sodium amide in the sodium salt kettle, and drop them in at a temperature of 0 to 45 ° C. 1.14-2.27 parts of cyclopentadiene, add cyclopentadiene dropwise and keep reacting at the above temperature for 0.5-3 hours to obtain cyclopentadienyl sodium; b. Add 4.0-13.6 parts of tetrahydrofuran to the synthesis kettle Finally, add 1 part of anhydrous cobalt chloride, stir for 30-40 minutes, then add the prepared cyclopentadienyl sodium, keep the liquid reflux at 60-70°C and continue stirring for 1-2 hours; c. Reflux ends Finally, start to recover the solvent THF, heat to 65-75 ° C, when the liquid flow rate decreases, turn on the vacuum negative pressure distillation to recover the solvent, when there is no liquid in the kettle, stir and add 13-180 parts of acetonitrile continuously, and stir at room tem...

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Abstract

The invention discloses a catalyst with high safety used for synthesizing 2-picoline and the preparation method, the procedures are: add THF and NaNH2 in sodium salt kettle, drip CPD when the temperature is 0 to 45 DEG C. and keep the reaction for 0.5 to 3 hours to produce CPD sodium; add anhydrous CoCl2 in the synthesis kettle after adding tetrahydrophthalic anhydride furan, stir for 30 to 40 minutes then add the prepared CPD sodium, keep the backflow of the liquid at the temperature of 60 to 70 DEG C. and keep stirring reaction for 1 to 2 hours continuously, the reaction of preparing catalyst is finished; after the backflow ending, recycle solvent and increase the temperature to 65 to 75 DEG C., when the liquid flow volume is reduced, open vacuum pressure distill recycle solvent, stir and add acetonitrile continuously when having no liquid in the kettle, after stirring for 1 hours under the room temperature to remove sodium chloride and get the catalyst in mixture state. The invention has simple reaction process, which prevents the strict requirements and complication of the synthesis technique of organic Co catalyst crystal.

Description

Technical field: [0001] The invention relates to a catalyst used in the synthesis of chemical products, in particular to a catalyst used for synthesizing 2-picoline. Background technique: [0002] 2-picoline is an intermediate in the chemical industry, mainly used in medicine and other industries. The 2-picoline currently used in my country is mainly imported. The key problem in its synthesis is the catalyst dicobaltene used in the synthesis process. They are all crystalline cobaltocenes, and their production process is relatively complicated, and the process conditions are harsh. The final crystallization of cobaltocenes needs to be realized under high vacuum conditions. In particular, it should be pointed out that the activity of crystalline cobaltocene is very high, it is afraid of light, heat and easy to decompose, afraid of acid gas, easy to oxidize and spontaneously combustible in the air. It is difficult to guarantee the quality and quality, and it is difficult to ach...

Claims

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Application Information

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IPC IPC(8): B01J31/12C07D213/06
Inventor 秦保伟郜家军
Owner HEBI SAIKE CHEM ENG CO LTD
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