A method for reclaiming diethyl oxalate and methyl acetate from triazine ring cyclization mother liquor with polyol as carrier

A technology of diethyl oxalate and methyl acetate, applied in chemical instruments and methods, preparation of carboxylic acid esters, preparation of organic compounds, etc., can solve problems such as unseen treatment reports

Active Publication Date: 2019-02-15
SHANDONG HUIHAI PHARMA & CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no relevant specific treatment report in the current literature

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 2500kg of triazine ring ring-closing mother liquor and 125kg of glycerol to the reaction kettle, start stirring, then add 300kg of industrial hydrochloric acid (content 30%), acidify and esterify at 50-60°C for 1 hour, and cool down to 30°C after the esterification is complete. ~40°C, filter with plate and frame to obtain a mixed solution of sodium chloride solid and water, methyl acetate, methanol, ethanol, polyol and oxalic acid; rinse the sodium chloride solid with 100kg of methanol, and dry it to obtain 212kg of solid sodium chloride; The eluent is mixed in the mixed solution of water, methyl acetate, methanol, ethanol, polyol and oxalic acid; 2205kg of water, methyl acetate, methanol and ethanol are removed from the solvent recovery tower to recover the solvent and recycled to the triazine ring for one step; the remaining materials, polyol and oxalic acid, are esterified by adding 230kg of ethanol and 230kg of phenyl, at -0.08~-0.1MPa 205 kg of diethyl oxalate ...

Embodiment 2

[0028] Add 2500kg of triazine ring ring closure mother liquor and 125kg of ethylene glycol into the reaction kettle, start stirring, then add 300kg of industrial hydrochloric acid (content 30%), carry out acidification and esterification at 50-60°C for 2 hours, and cool down to 30~40℃, plate and frame filter to obtain the mixed solution of sodium chloride solid and water, methyl acetate, methanol, ethanol, polyol and oxalic acid; rinse the sodium chloride solid with 100kg of methanol, and dry it to obtain 215kg of solid sodium chloride ; The eluent is mixed in the mixed solution of water, methyl acetate, methanol, ethanol, polyol and oxalic acid; 2215kg of water, methyl acetate, methanol and ethanol are removed, and the solvent is recovered from the solvent recovery tower to be recycled to the triazine ring for one step; the remaining material polyol and oxalic acid are esterified by adding 460kg of ethanol and 460kg of phenyl to -0.08~-0.1 Diethyl oxalate 200kg was collected ...

Embodiment 3

[0030] Add 2500kg of triazine ring ring-closing mother liquor, 250kg of neopentyl glycol and glycerol to the reaction kettle, start stirring, then add 300kg of industrial hydrochloric acid (content 30%), carry out acidification and esterification at 50-60°C for 2 hours, esterification After completion, cool down to 30-40°C, filter the plate and frame to obtain a mixed solution of sodium chloride solid and water, methyl acetate, methanol, ethanol, polyol and oxalic acid; rinse the sodium chloride solid with 100kg of methanol, and dry it to obtain a solid Sodium chloride 205kg; the eluent is mixed in the mixed solution of water, methyl acetate, methanol, ethanol, polyol and oxalic acid; the mixed solution of water, methyl acetate, methanol, ethanol, polyol and oxalic acid is distilled to 110~ At 120°C, distill 2220kg of water, methyl acetate, methanol and ethanol, remove the solvent recovery tower to recover the solvent and reuse it for the triazine ring synthesis step; add 230kg...

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PUM

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Abstract

The invention relates to a method for recovering diethyl oxalate and methyl acetate from triazine ring cyclization mother liquid by taking polyhydric alcohol as a carrier. The comprehensive treatment of the triazine ring cyclization mother liquid is realized by adding high-boiling-point polyhydric alcohol as the carrier, acidizing and esterifying the triazine ring cyclization mother liquid, desalting, recovering methanol, ethanol and methyl acetate through distillation, recovering diethyl oxalate through esterification and recycling the polyhydric alcohol. The methanol, the ethanol, sodium acetate and sodium oxalate in the triazine ring cyclization mother liquid are completely recovered, the recovered methanol, ethanol, methyl acetate and diethyl oxalate can be completely reused for the triazine ring cyclization step, and only one solid material, namely sodium chloride, is generated.

Description

technical field [0001] The invention belongs to the field of mother liquor treatment, and in particular relates to a method for recovering diethyl oxalate and methyl acetate from a triazine ring cyclization mother liquor by using polyhydric alcohol as a carrier. Background technique [0002] Triazine ring is a pharmaceutical intermediate, and ceftriaxone sodium synthesized from it, also known as ceftriaxone, is a broad-spectrum, long-acting third-generation cephalosporin antibiotic for injection. It is mainly used for infections caused by sensitive bacteria, such as respiratory infections (especially pneumonia), ear, nose and throat infections, urinary system infections, sepsis, meningitis, prevention of surgical infections, bone and joint infections, skin and soft tissue infections, For reproductive system infections (including gonorrhea), the general curative effect is satisfactory, and it can also be used for trauma infections and abdominal infections. [0003] In the tr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C67/54C07C69/36C07C69/14C07C51/02C07C51/44C07C55/06C01D3/04
CPCC01D3/04C07C51/02C07C51/44C07C67/08C07C67/54C07C69/36C07C69/14C07C55/06
Inventor 卢言建于西波李保铃张世凤
Owner SHANDONG HUIHAI PHARMA & CHEM
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