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3,5,6-trichloropyridin-2-ol sodium high-boiling solid waste conversion method

A technology of sodium trichloropyridine and solid waste, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve the problem of inappropriate economy and low conversion rate. Advanced problems, to achieve the effect of small size and low energy

Inactive Publication Date: 2011-01-12
SHANXI KANGDELI FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to this calculation, the amount of catalyst used is almost equal to the content of tetrachloropyridine. This kind of reaction is not suitable from an economic point of view, and the conversion rate of the reaction is not very high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] Embodiment 1, a kind of sodium clopyridinate high boiling solid waste conversion method, the tetraclopyridine high boiler 600Kg containing 75% that obtains in the production of clopyridinate sodium, and the sodium hydroxide that concentration is 30% 1500kg of the solution and their total amount of 4% catalyst hexamethylphosphoric triamide are added together in a 5000L conversion kettle, reacted at 100° for 20 hours, and the reaction solution after the conversion reaction is cooled and crystallized for solid-liquid separation to obtain trichloro Crude sodium pyridyl alcohol. Put the crude product into the refining kettle, add water to raise the temperature to dissolve, and after cooling down for recrystallization, centrifuge the precipitated solid phase and liquid phase, and the filter cake is the wet product of 2,3,5-trichloropyridinol sodium, and then dry it to obtain 2, The finished product of 3,5-triclopyridinate sodium, the separated mother liquor is used as water t...

Embodiment 2

[0009] Embodiment 2, a kind of clopyridinate sodium high boiling solid waste conversion method, the tetraclopyridine high boiler 800Kg containing 70% obtained in the production of clopyridinate sodium, and the sodium hydroxide that concentration is 30% 2000kg of the solution and their total amount of 3% catalyst hexamethylphosphoric triamide are added together in a 5000L conversion kettle, reacted for 15 hours under the condition of 105 °, and the reaction liquid after the conversion reaction is cooled and crystallized for solid-liquid separation to obtain trichloro Crude sodium pyridyl alcohol. Put the crude product into the refining kettle, add water to raise the temperature to dissolve, and after cooling down for recrystallization, centrifuge the precipitated solid phase and liquid phase, and the filter cake is the wet product of 2,3,5-trichloropyridinol sodium, and then dry it to obtain 2, The finished product of 3,5-triclopyridinate sodium, the separated mother liquor is ...

Embodiment 3

[0010] Embodiment 3, a kind of clopyridinate sodium high boiling solid waste conversion method, the tetraclopyridine high boiler containing 80% that obtains in the production of clopyridinate sodium 600Kg, and the sodium hydroxide that concentration is 30% 2000kg of the solution and their total amount of 3% catalyst hexamethylphosphoric triamide are added together in a 5000L conversion kettle, reacted for 20 hours at 110 °, and the reaction solution after the conversion reaction is cooled and crystallized for solid-liquid separation to obtain trichloro Crude sodium pyridyl alcohol. Put the crude product into the refining kettle, add water to raise the temperature to dissolve, and after cooling down for recrystallization, centrifuge the precipitated solid phase and liquid phase, and the filter cake is the wet product of 2,3,5-trichloropyridinol sodium, and then dry it to obtain 2, The finished product of 3,5-triclopyridinate sodium, the separated mother liquor is used as water ...

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PUM

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Abstract

The invention relates to waste treatment technology for production of 3,5,6-trichloropyridin-2-ol sodium, in particular to a 3,5,6-trichloropyridin-2-ol sodium high-boiling solid waste conversion method, and solves the problem of recycling a by-product tetrachloropyridine in the production of the 3,5,6-trichloropyridin-2-ol sodium. The method comprises the following steps of: adding 1 part of high-boiling substance and 1 to 1.3 parts of sodium hydroxide and a catalyst hexamethyl phosphoric triamide which accounts for 3 to 5 percent of the total amount of the high-boiling substance and the sodium hydroxide into a conversion kettle based on pure tetrachloropyridine in the production of the 3,5,6-trichloropyridin-2-ol sodium, performing reaction for 10 to 20 hours at the temperature of between 100 and 110 DEG C, cooling and crystallizing the reaction liquid after the conversion reaction, and performing solid-liquid separation to obtain crude 3,5,6-trichloropyridin-2-ol sodium; and adding the crude product into a refining kettle, adding water, heating for dissolving, cooling and recrystallizing, and performing centrifugal separation of the separated solid phase and liquid phase. The 3,5,6-trichloropyridin-2-ol sodium high-boiling solid waste conversion method has the advantages of over 90 percent of conversion rate of tetrachloropyridine, relatively low catalyst consumption in the reaction for treating the same amount of tetrachloropyridine, small volume of the used reaction vessel and lower energy consumption.

Description

technical field [0001] The invention relates to a waste treatment technology for the production of clopyridinate sodium, in particular to a method for converting clopyridinate sodium into high-boiling solid waste. Background technique [0002] The domestic production of triclopyridinate sodium all adopts the trichloroacetyl chloride process route, the main raw materials are trichloroacetyl chloride, acrylonitrile, cuprous chloride is used as a catalyst, and o-dichlorobenzene is used as a solvent. In the reaction process of closed addition, many by-products can be produced, and the most important by-product is tetrachloropyridine, whose yield accounts for 10% of the final product. [0003] Tetrachloropyridine can be dissolved in o-dichlorobenzene, it is difficult to separate, and only after the solvent is distilled and recovered, a concentrated high boiling liquid can be obtained, which contains about 70% of tetrachloropyridine, 25% of solvent, and 5% of other impurities . ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/63B01J31/02
Inventor 杨东亮
Owner SHANXI KANGDELI FINE CHEM