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Method for recovering oxalic acid in triazine ring cyclization mother liquor slag with tin chloride as catalyst

A technology of tin chloride and triazine ring, which is applied in the field of recovery of chemical intermediate products, can solve the problems of low yield, high production cost, and substandard acidity, and achieve the effect of high reaction yield and low cost

Active Publication Date: 2018-05-08
SHANDONG HUIHAI PHARMA & CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to overcome the ubiquitous problems in the prior art, such as material danger, low yield, high production cost, substandard acidity, etc., and provide a kind of catalyst recovery of oxalic acid in the slag of triazine ring cyclization mother liquor with tin chloride Methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 330g of 35% hydrogen chloride ethanol solution to a 1L autoclave, and obtain 150g of sodium oxalate and 0.75g of tin chloride after adding treatment, heat up to reflux, keep warm for 3h, after the reaction is complete, drop to room temperature, and transfer the material to a Add 124.5ml of benzene to a 1000ml four-neck bottle of stirring and water separation facilities, heat up and reflux to separate water until the anhydrous phase of the water separator is separated, heat up to distill benzene out, and collect the remaining material under reduced pressure at 92-106°C to obtain 161.7 g diethyl oxalate, purity 99.55%, yield 99.02%; sodium chloride 131.3g, content 98.83% can be taken out.

Embodiment 2

[0025] Add 360g of 30% hydrogen chloride ethanol solution to a 1L autoclave, and obtain 150g of sodium oxalate and 0.5g of tin chloride after adding and processing, heat up to reflux, keep warm for 2h, after the reaction is complete, drop to room temperature, and transfer the material to a Add 150ml of benzene to the 1000ml four-neck bottle of the water separation facility of the mixer, heat up and reflux to separate the water, until the anhydrous phase of the water separator is separated, heat up to evaporate the benzene, and collect the remaining material under reduced pressure at 92-106°C to obtain 160.6g of oxalic acid Diethyl ester, purity 99.62%, yield 98.26%, sodium chloride 132.4g, content 98.92% can be taken out.

Embodiment 3

[0027] Add 300g of 36% hydrogen chloride ethanol solution to a 1L autoclave, and after the addition process, 150g of sodium oxalate and 0.015g of tin chloride are obtained, and the temperature is raised to reflux, and the temperature is kept for 3 hours. After the reaction is completed, it is lowered to room temperature. Add 140ml of benzene to the 1000ml four-necked bottle of the water separation facility, raise the temperature and reflux to divide the water until no water comes out of the water separator, then raise the temperature to evaporate the benzene, and collect the fraction at 92-106°C under reduced pressure to obtain 161.9g of diethyl oxalate , 99.42% purity, 99.06% yield, 131.6g sodium chloride, 98.73% content can be taken out.

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PUM

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Abstract

The invention relates to a method for recycling oxalic acid from triazine ring cyclization mother liquor dreg with tin chloride as a catalyst. The method comprises the steps of treating the triazine ring cyclization mother liquor solid dreg with water according to a conventional method, obtaining sodium oxalate, adding the sodium oxalate and the catalyst to a hydrogen chloride ethanol solution, and raising the temperature and conducting backflow for 2-3 hours in a closed environment; after a reaction is ended, lowering the temperature to the room temperature, conducting filtration, and obtaining solid sodium chloride and an ethanol oxalate solution; leaching the solid sodium chloride with ethyl alcohol, and applying leacheate to preparation of the hydrogen chloride ethanol solution in a mingled mode; adding a dehydrating agent to the ethanol oxalate solution, conducting temperature raising, backflow and water diversion till no aqueous phase is separated out, evaporating the dehydrating agent out, conducting reduced pressure distillation and collection on remaining materials within the range from minus 0.08 MPa to minus 0.1 MPa, conducting fraction at the temperature of 92-106 DEG C, and obtaining diethyl oxalate. The hydrogen chloride ethanol solution prepared through the method is low in cost, the tin chloride serves as the catalyst, and the yield of the oxalic acid reaction is high and reaches 99%. Only one type of by-products is generated, namely sodium chloride, no other waste materials are generated in the reaction process, and safety and environmental friendliness are achieved.

Description

technical field [0001] The invention belongs to the field of recovery of chemical intermediate products, and in particular relates to a method for recovering oxalic acid in triazine ring cyclization mother liquid slag by using tin chloride as a catalyst. Background technique [0002] Triazine ring is a pharmaceutical intermediate, and ceftriaxone synthesized from it is a broad-spectrum, long-acting third-generation cephalosporin antibiotic for injection. [0003] In the triazine ring cyclization mother liquor, the main components are methanol, ethanol, and a large amount of organic salts. After the methanol and ethanol solvents are recovered through distillation and other processes, a large amount of organic salts become solid waste. The main components of solid waste are sodium acetate, sodium oxalate, etc., and a small amount of solvents such as methanol, water, etc. remain. At present, there is no suitable way to treat or recycle this kind of solid waste. It can only be ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/36C07C67/08
CPCC07C51/02C07C67/08C07C69/36C07C55/06
Inventor 李保铃孙成斌王乐强郭刚姜福元
Owner SHANDONG HUIHAI PHARMA & CHEM