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Method and system for recycling borofluoride and solvent from 7-ACT crystallization mother liquor

A technology of 7-ACT and crystallization mother liquor, which is applied in the purification/separation of carboxylic acid nitriles, purification/separation of amino compounds, organic chemistry, etc. It can solve the problems of polluted environment and excessive ammonia nitrogen value, and achieve the improvement of recovery quality and solvent recovery rate The effect of increasing and reducing production costs

Active Publication Date: 2015-11-18
山东安弘制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the device can achieve the purpose of recovering acetonitrile, the fluoroborate remains in the still residue and is discharged, and the water phase is discharged into the environment without being recycled, causing the ammonia nitrogen value in the water body to seriously exceed the standard, polluting the environment

Method used

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  • Method and system for recycling borofluoride and solvent from 7-ACT crystallization mother liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Such as figure 1 As shown, a system for recovering fluoroborate and solvent from 7-ACT crystallization mother liquor, including crystallization mother liquor tank 1, evaporator 2, crystallizer 3, filter 4, condenser 5, extraction tower 6 and rectification Tower 7;

[0035] Described crystallization mother liquor tank 1 is connected with evaporator 2, and described evaporator 2 is connected with condenser 5 and crystallizer 3 respectively, and described condenser 5 is connected with extraction tower 6, and described extraction tower 6 is connected with finishing Distillation tower 7 is connected; Described crystallizer 3 is connected with filter 4;

[0036] The liquid discharge port of the filter 4 is connected with the feed port of the evaporator 2 , and the top discharge port of the rectification tower 7 is connected with the feed port of the extraction tower 6 .

[0037] The condenser 5 described in this embodiment is a graphite condenser, and the filter 4 described...

Embodiment 2

[0039] The method for reclaiming fluoroborate and solvent from the 7-ACT crystallization mother liquor using the system described in Example 1, the steps are as follows:

[0040] Add about 3000L of 7-ACT crystallization mother liquor, add 12kgLiOH to adjust the pH to 6.8, control the temperature at 60°C, and distill under reduced pressure through the evaporator 2 until the amount of steam evaporated is 75% of the total mother liquor, and the steam enters the extraction after passing through the graphite condenser 5 Tower 6. Since the 7-ACT crystallization mother liquor contains both water and organic solvents, the distillation is in an azeotropic state at the beginning, and the steam contains both water and organic solvents; as the distillation proceeds, the water is distilled out separately and can be recycled.

[0041] After distillation, the remaining 7-ACT crystallization mother liquor reaches a certain concentration, then lowers to room temperature, enters the crystallize...

Embodiment 3

[0044] Add 12kg LiOH to about 3000L of 7-ACT crystallization mother liquor to adjust the pH to 7.2, control the temperature at 80°C, and distill under reduced pressure through evaporator 2 until the amount of steam evaporated is 70% of the total mother liquor. The steam enters the extraction tower 6 after passing through the graphite condenser 5 .

[0045]After distillation, the remaining 7-ACT crystallization mother liquor is lowered to room temperature, enters the crystallizer 3, adds 100g ammonium fluoroborate salt as a seed crystal, controls the temperature at 0°C to fully crystallize the ammonium fluoroborate salt, and then pours it into the plate and frame filter 4 After filtering and washing the solids, it is ammonium fluoroborate, the recovery rate is 96.33%, the recovered product has a purity of 99.62% and a content of 98.86%. The filtrate is transferred to the 7-ACT crystallization mother liquor tank through a closed system, and the next batch of rough distillation i...

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Abstract

The invention relates to a method and system for recycling borofluoride and a solvent from 7-ACT crystallization mother liquor. The method comprises the following steps: (1) adjusting the pH of the 7-ACT crystallization mother liquor to be 6.5-8.0, and distilling; (2) after condensing the distilled steam, adding an extraction agent for extraction, carrying out rectification on the extracted organic phase to obtain the solvent and the extraction agent, and recycling an aqueous phase; (3) after the remaining distilled 7-ACT crystallization mother liquor naturally cools, adding seed crystals, separating out solids by crystallization, performing solid-liquid separation, washing the solids to obtain borofluoride, and combining the liquid with the 7-ACT crystallization mother liquor in the step (1) for cyclic utilization. The invention also provides the system for implementing the method. According to the method and the system, the purpose of zero release of the whole technology can be achieved, and the method has the advantages of being easy to operate, high in yield, low in cost, and the like.

Description

technical field [0001] The invention relates to a method for recovering fluoroborate and solvent, in particular to a method for recovering fluoroborate and solvent from 7-ACT crystallization mother liquor. Background technique [0002] Ceftriaxone sodium is a long-acting antibiotic drug among the third-generation cephalosporins. It has bactericidal effects on many Gram-positive bacteria, negative bacteria and anaerobic bacteria, and it is effective on most β-lactamases produced by bacteria Highly stable, thus enhancing its antibacterial effect. At present, ceftriaxone sodium is widely used clinically and is one of the 22 kinds of cephalosporin antibiotic preparations approved by the state for clinical application. [0003] The method of synthesizing ceftriaxone sodium is mostly with 7-ACA (3-acetoxymethyl-5-sulfur-7-amino-8-oxygen-1-azabicyclooct-2-ene-2 ​​carboxylic acid) and TTZ (triazine ring) is used as a raw material to generate 7-ACT (7-amino ceftriaxone) through con...

Claims

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Application Information

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IPC IPC(8): C07C255/03C07C253/34C07C211/62C07C209/86
Inventor 谢鹏冯宪东刘月符淙淙赵丹丹
Owner 山东安弘制药有限公司