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

Comprehensive recovery method of effective components in N-haloacetyl-7-ACA crystallization mother liquor

A technology of -7-ACA and haloacetyl, which is applied in the field of comprehensive recovery of active ingredients in N-haloacetyl-7-ACA crystallization mother liquor, can solve problems such as waste, large COD, and increased processing costs, and reduce environmental pollution. Pollution, the effect of improving economic benefits

Active Publication Date: 2022-02-01
SHANXI WEIQIDA PHARMA IND
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the N-haloacetyl-7-ACA crystallization mother liquor is directly discharged to the environmental protection treatment link without recycling, it will not only cause huge waste, but also generate huge COD, which increases the treatment cost

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
  • Comprehensive recovery method of effective components in N-haloacetyl-7-ACA crystallization mother liquor
  • Comprehensive recovery method of effective components in N-haloacetyl-7-ACA crystallization mother liquor
  • Comprehensive recovery method of effective components in N-haloacetyl-7-ACA crystallization mother liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Recovery of N-bromoacetyl-7-ACA

[0037] Get N-bromoacetyl-7-ACA crystallization mother liquor, wherein N-bromoacetyl-7-ACA concentration is 2.2g / L, triethylamine salt concentration is 12.1g / L (in triethylamine), pH is 1.5, The temperature is 23°C, it is cooled to 4.0°C, and 30% sodium hydroxide solution is added to adjust the pH to 2.5; then the macroporous adsorption resin column bed is passed through the macroporous adsorption resin at a flow rate of 3BV / h (the macroporous adsorption resin model is XAD16N, and the loading capacity is 1L, The ratio of height to diameter is 9), and the amount of loading on the column is 20L in total, and 20L of the adsorption residue (triethylamine concentration 12g / L) is collected at the same time; then, use 0.12mol / L sodium bicarbonate solution to desorb and adsorb on the After desorption of N-bromoacetyl-7-ACA on the resin, 1.1L of desorption liquid was collected after desorption, and the concentration of N-bromoacetyl-7-ACA was...

Embodiment 2

[0041] (1) Recovery of N-bromoacetyl-7-ACA

[0042] Get N-bromoacetyl-7-ACA crystallization mother liquor, wherein N-bromoacetyl-7-ACA concentration is 3g / L, triethylamine salt concentration is 15g / L (in triethylamine), pH is 1.5, temperature 23 ℃, it is cooled to 4.0 ℃, and 30% sodium hydroxide solution is added to adjust the pH to 2.5; Ratio is 9), the amount of loading on the column is 20L in total, and 20L (triethylamine concentration 15g / L) of the residual liquid of adsorption is collected simultaneously; N-bromoacetyl-7-ACA, 1.6L of desorption solution was collected after desorption, and the concentration of N-bromoacetyl-7-ACA was 36g / L; the temperature of the desorption solution was raised to 20°C, and 6M hydrochloric acid was added to adjust the pH of the system to 1.5, N-bromoacetyl-7-ACA was crystallized, centrifuged, washed and dried to obtain 52 g of N-bromoacetyl-7-ACA solid, with a purity of 99% and a yield of 86.7%.

[0043] (2) recovery of triethylamine

[...

Embodiment 3

[0046] (1) Recovery of N-chloroacetyl-7-ACA

[0047] Get N-chloroacetyl-7-ACA crystallization mother liquor, wherein N-chloroacetyl-7-ACA concentration is 10.7g / L, triethylamine salt concentration is 91.5g / L (in triethylamine), pH is 1.0, The temperature is 5°C, its temperature is controlled at 4.0°C, and 30% sodium hydroxide solution is added to adjust the pH to 3.0; then pass through a macroporous adsorption resin column bed at a flow rate of 0.5BV / h (the macroporous adsorption resin model is LX-1180, The loading capacity is 1L, the height-to-diameter ratio is 15), and the column volume is 3L in total. After the adsorption is completed, wash the column with 0.5BV of purified water, and collect 3.5L of the adsorption residue (triethylamine concentration: 78.1g / L); then, use 0.20 The mol / L sodium bicarbonate solution desorbs the N-chloroacetyl-7-ACA adsorbed on the resin at a flow rate of 0.5BV / h. After the desorption is completed, 0.6L of the desorption solution is collected,...

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 belongs to the technical field of pharmacy, and relates to a comprehensive recovery method of effective components in N-haloacetyl-7-ACA crystallization mother liquor, which comprises the following steps of: specifically adsorbing N-haloacetyl-7-ACA in the mother liquor by adopting non-polar macroporous adsorption resin under the condition that the pH value is 2-4, and desorbing and crystallizing to obtain a qualified N-haloacetyl-7-ACA finished product; adjusting the pH value of the triethylamine salt in the adsorption residual liquid to 12-14, converting into triethylamine, and obtaining a qualified triethylamine product through liquid separation and rectification. The comprehensive recovery method provided by the invention provides an environment-friendly and economical treatment method for the product waste liquid in the production process of the N-haloacetyl-7-ACA, and has obvious effects on reducing environmental pollution and improving economic benefits.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and relates to a method for comprehensively recovering active ingredients in N-haloacetyl-7-aminocephalosporanic acid (hereinafter referred to as: N-haloacetyl-7-ACA) crystallization mother liquor, more specifically , involving comprehensive recovery of N-haloacetyl-7-ACA and triethylamine from N-haloacetyl-7-ACA crystallization mother liquor in the preparation of N-haloacetyl-7-ACA during the preparation of cefathiamidine method, the N-haloacetyl-7-ACA can be N-chloroacetyl-7-ACA or N-bromoacetyl-7-ACA. Background technique [0002] Cefathiamidine, also known as cephalosporin 18, is the first-generation cephalosporin antibacterial agent developed by my country. It exerts antibacterial effects by inhibiting the synthesis of bacterial cell walls, and is effective against Staphylococcus aureus, Streptococcus viridans, and Pneumococcus. It has a strong effect and has a unique antibacterial activity...

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
IPC IPC(8): C07D501/12C07D501/28C07C209/86C07C211/05
CPCC07D501/12C07D501/28C07C209/86C07C211/05
Inventor 刘宏飞白延峰白飞冯涛李伟
Owner SHANXI WEIQIDA PHARMA IND