Unlock instant, AI-driven research and patent intelligence for your innovation.

A method and system for recovering fluoroborate and solvent from 7‑ACT crystallization mother liquor

A technology of crystallization mother liquor and fluoroborate, which is applied in the purification/separation of carboxylic acid nitriles, purification/separation of amino compounds, organic chemistry, etc., can solve the problems of environmental pollution, excessive ammonia nitrogen value, etc., and achieve the improvement of recovery quality and solvent recovery The effect of improving the efficiency and reducing the production cost

Active Publication Date: 2017-03-15
山东安弘制药有限公司
View PDF1 Cites 0 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A method and system for recovering fluoroborate 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 includes crystallization mother liquor tank 1, evaporator 2, crystallizer 3, filter 4, condenser 5, extraction tower 6 and rectification Tower 7;

[0035] The crystallization mother liquor tank 1 is connected to the evaporator 2, the evaporator 2 is connected to the condenser 5 and the crystallizer 3, the condenser 5 is connected to the extraction tower 6, and the extraction tower 6 is connected to the refiner. The distillation tower 7 is connected; the crystallizer 3 is connected to the filter 4;

[0036] The liquid outlet of the filter 4 is connected to the inlet of the evaporator 2, and the outlet of the top of the rectification tower 7 is connected to the inlet of the extraction tower 6.

[0037] In this embodiment, the condenser 5 is a graphite condenser, and the filter 4 is a plate and frame filter.

Embodiment 2

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

[0040] About 3000L of 7-ACT crystallization mother liquor is added with 12kg LiOH to adjust the pH to 6.8, and the temperature is controlled at 60℃. The steam is distilled under reduced pressure through evaporator 2 until the amount of steam is 75% of the total amount of mother liquor. The steam enters after graphite condenser 5. Extraction tower 6. Since 7-ACT crystallization mother liquor contains water and organic solvent at the same time, it is distilled into azeotropic state at the beginning, and the steam contains water and organic solvent at the same time; 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, and then it is reduced to room temperature, enters the cr...

Embodiment 3

[0044] About 3000L of 7-ACT crystallization mother liquor was added with 12kg LiOH to adjust the pH to 7.2, the temperature was controlled at 80°C, and the steam was distilled under reduced pressure through the evaporator 2 until the amount of steam evaporated was 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, and 100g of ammonium fluoroborate is added as a seed crystal, and the temperature is controlled to 0°C to fully crystallize the ammonium fluoroborate, and then it is poured into the plate and frame filter 4. After filtration and solid washing, it is ammonium fluoroborate, the recovery rate is 96.33%, the purity of the recovered product is 99.62%, and the content is 98.86%. The filtrate is transferred to the 7-ACT crystallization mother liquor tank through a closed sy...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

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 in the third-generation cephalosporins. It has a bactericidal effect on many gram-positive, negative and anaerobic bacteria, and it has a bactericidal effect on most β-lactamases produced by bacteria Highly stable, thereby enhancing its antibacterial effect. At present, ceftriaxone sodium is widely used in clinical practice and is one of the 22 kinds of cephalosporin antibiotic preparations approved by the state for clinical application. [0003] At present, the method of synthesizing ceftriaxone sodium is mostly 7-ACA (3-acetoxymethyl-5-thio-7-amino-8-oxo-1-azabicyclooct-2-ene-2 ​​carboxylic acid) and TTZ (triazine ring) is used as a raw material to produce 7-ACT (7-aminoceftriazine) by condensat...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/03C07C253/34C07C211/62C07C209/86
Inventor 赵卫良谢鹏冯宪东周臣生刘月符淙淙
Owner 山东安弘制药有限公司