Fluoroborate exchange crystallization recovery technology for cephalosporin fluorine-containing waste liquid

A fluoroborate, potassium fluoroborate technology, applied in tetrafluoroboric acid, boron halide compounds, ammonium chloride and other directions, can solve the problems of strict emission control, corrosion of equipment, serious problems, etc., to avoid corrosion, easy operation control, The effect of reducing production costs

Inactive Publication Date: 2019-02-19
SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The 3-position sulfur substitution synthesis reaction produces a large amount of fluorine-containing waste liquid, which severely corrodes equipment and strictly controls emissions, and cannot be recycled through normal recovery technologies

Method used

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  • Fluoroborate exchange crystallization recovery technology for cephalosporin fluorine-containing waste liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Add 8L of cephalosporin fluorine-containing waste liquid in the stirred tank, after measuring 5.7mol / L of fluoroborate, stir and add 10% ammonia water to adjust the pH to 7.0, then continue to add 3.4kg potassium chloride in the stirred tank to carry out salt For the exchange reaction, the temperature is 50°C, and the reaction is stirred for 2 hours. During the reaction, crystallization is continuously produced. After the reaction, the solid-liquid separation is carried out through a centrifuge to obtain the remaining waste liquid and solid potassium fluoroborate from which the fluorine-containing compound has been removed. The solid remains in the centrifuge and is washed with water, and washed twice. After centrifugal washing, wet potassium fluoroborate is obtained and then dried in a dryer. The drying time is 8 hours, and the drying temperature is 120°C. Finally, the pure product is collected; after determination of fluorine The recovery rate of potassium borate w...

Embodiment 2

[0029] (1) Add 10L of cephalosporin fluorine-containing waste liquid in the stirred tank, after measuring 8.3mol / L of fluoroborate, stir and add 20% ammonia water to adjust the pH to 14, then continue to add 7.4kg of potassium chloride in the stirred tank for salting For the exchange reaction, the temperature is 100°C, and the reaction is stirred for 2 hours. During the reaction, crystallization is continuously produced. After the reaction, the solid-liquid separation is carried out through a centrifuge to obtain the remaining waste liquid and solid potassium fluoroborate from which the fluorine-containing compound has been removed. The solid remains in the centrifuge and is washed with water, and washed twice. After centrifugal washing, wet potassium fluoroborate is obtained and then dried in a dryer. The drying time is 12 hours, and the drying temperature is 150°C. Finally, the pure product is collected; The recovery rate of potassium borate was 99.1%, and the purity was 99.2...

Embodiment 3

[0032] (1) Add 5L of cephalosporin fluorine-containing waste liquid in the stirred tank, after measuring 2.3mol / L of fluoroborate, stir and add 15% ammonia water to adjust the pH to 10.0, then continue to add 0.94kg potassium chloride solution in the stirred tank to carry out For the salt exchange reaction, the temperature is 80°C, and the reaction is stirred for 3 hours. During the reaction, precipitation occurs continuously; Continue to stay in the centrifuge and add water to wash, wash twice, get wet potassium fluoroborate after centrifugal washing, and then dry it in a dryer, drying time 9h, drying temperature 130°C, and finally collect the pure product; after determination of fluoroboric acid The recovery rate of potassium was 98.9%, and the purity was 99.0%.

[0033] (2) The remaining waste liquid after filtration can enter the rectification kettle to rectify and recover the organic solvent, the pressure is 0.1MPa, the temperature is 45°C, the organic solvent is condense...

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Abstract

The invention discloses a fluoroborate exchange crystallization recovery technology for a cephalosporin fluorine-containing waste liquid. The technology comprises the following steps that (1) the pH of the cephalosporin fluorine-containing waste liquid is adjusted to 7.0-14.0; (2) potassium chloride is added for salt exchange, and potassium fluoroborate is separated out in the form of crystals during a reaction because of low solubility; (3) filtration, washing and drying are conducted to obtain pure potassium fluoroborate; (4) due to the removal of fluorine compounds, the waste liquid can bedirectly distilled to recover an organic solvent so as to avoid corrosion of equipment, and residual liquid is concentrated and crystallized to recover ammonium chloride. According to the technology,fluoroborates are effectively separated, potassium fluoroborate is an important raw material for producing boron trifluoride, the production cost is reduced, and the technology has the advantages of being simple in process operation, low in equipment requirement, high in recovery yield and environmentally friendly, so that the recovery purpose of preventing cephalosporin from producing the fluorine-containing waste liquid is achieved.

Description

technical field [0001] The invention relates to a recovery technology of fluoroborate exchange crystallization of cephalosporin fluorine-containing waste liquid. Background technique [0002] In the cephalosporin synthesis process, most of them need to introduce a mercapto-containing substitution functional group at the 3-position of the mother nucleus. In the process, boron trifluoride complexes are mostly used to participate in the reaction. Boron trifluoride (BF 3 ) aprotic strong acidic complex catalyst system, which effectively increases the catalyst concentration of the reaction system, realizes the complex dissolution of 7-ACA raw materials, enhances the reactivity of the 3-acetoxy group, and is beneficial to the 3- The side chain substitution reaction occurs, which has the advantages of accelerating the reaction process, shortening the reaction time, effectively controlling the formation of by-products, mild and easy-to-control reaction conditions, and high reaction ...

Claims

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Application Information

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IPC IPC(8): C01B35/06C01C1/16
CPCC01B35/066C01C1/164C01P2006/80
Inventor 刘晓彤朱传喜李呈龙
Owner SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK CO LTD
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