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A kind of method of processing triazine ring sodium salt mother liquor slag

A technology of triazine ring sodium and triazine ring, applied in the field of chemical synthesis waste treatment, can solve the problems of complex process, unprocessable triazine ring sodium salt slag, unstable properties and the like, and achieves high reaction temperature, good appearance and color, Simple process effect

Active Publication Date: 2020-10-16
SHANDONG HUIHAI PHARMA & CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The slag mainly contains sodium oxalate and sodium acetate and a small amount of sodium sulfate, sodium triazine ring salt, sodium carbonate, and the mother liquor of triazine ring sodium salt after alkalization. , the processing cost is too high; in order to reduce production costs and increase profits, the company has independently developed and processed the mother liquor slag of triazine ring sodium salt, and successively used the methods of patent CN 105330545 B and CN 106349068 A to solve the problem that the current triazine ring sodium salt slag cannot be processed , Difficult environmental issues
[0003] Catalyst tin tetrachloride must be used in the method of patent CN 105330545 B to process mother liquor slag, the boiling point of tin tetrachloride is low, the boiling point is not easy to recover between methanol and diethyl oxalate, the property is unstable, easy to decompose, and The post-treatment of the catalyst is not mentioned in the technical plan, which is a safety hazard of this process; and in this reaction, the reaction products are oxalic acid and diethyl oxalate, and the reaction process is not easy to hollow and control
[0004] CN 106349068 A and other methods for treating triazine ring sodium salt slag have complex processes. We have verified through small experiments that under the reaction conditions provided by the patent, the sodium salt cannot be converted with high efficiency, and the content of sodium chloride generated is low, only 75- 80%, the smell is strong, the sodium chloride obtained after applying ethylene glycol and other solvents is earthy yellow, and it is not easy to deal with later

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A method for processing triazine ring sodium salt mother liquor slag, comprising the following steps:

[0016] Put the wet product triazine ring sodium salt mother liquor slag into a four-necked bottle, add polyethylene glycol and hydrochloric acid, the weight of polyethylene glycol is 4 times of the weight of the sodium salt mother liquor slag, and the weight of hydrochloric acid is the weight of the sodium salt mother liquor slag 0.8 times of that, heat up to 140°C for 4 hours, after the heat preservation, carry out distillation, distill to the liquid temperature of 160°C, keep heat for 1.5h, then cool down to below 60°C and suction filter to obtain white sodium chloride crystals, apply the filtrate mechanically, chlorinate The sodium content is 99.21%.

Embodiment 2

[0018] A method for processing triazine ring sodium salt mother liquor slag, comprising the following steps:

[0019] Put the wet product triazine ring sodium salt mother liquor slag into a four-necked bottle, add polyethylene glycol and hydrochloric acid, the weight of polyethylene glycol is 3 times of the weight of the sodium salt mother liquor slag, and the weight of hydrochloric acid is the weight of the sodium salt mother liquor slag 1 times the temperature, heat up to 130°C for 2 hours, after the heat preservation, carry out distillation, distill to the liquid temperature of 160°C, keep heat for 2 hours, then cool down to below 60°C and filter with suction to obtain white sodium chloride crystals, the filtrate is used mechanically, sodium chloride The content is 98.89%.

Embodiment 3

[0021] A method for processing triazine ring sodium salt mother liquor slag, comprising the following steps:

[0022] Put the wet product triazine ring sodium salt mother liquor slag into a four-necked bottle, add polyethylene glycol and hydrochloric acid, the weight of polyethylene glycol is 5 times of the weight of the sodium salt mother liquor slag, and the weight of hydrochloric acid is the weight of the sodium salt mother liquor slag 0.5 times of the temperature, raise the temperature to 120°C and keep it for 5 hours. After the heat preservation, carry out distillation. After distilling to a liquid temperature of 160°C, keep it for 1 hour, then lower the temperature to below 60°C and filter with suction to obtain white sodium chloride crystals. The filtrate can be applied mechanically. The content is 98.93%.

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PUM

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Abstract

The invention relates to a method for treating triazine ring sodium salt mother solution dreg. The method comprises the steps of putting wet triazine ring sodium salt mother solution dreg into a four-mouth bottle, adding polyethylene glycol and hydrochloric acid, heating to 120-140 DEG C, maintaining the temperature for 2-6 hours, distilling until the temperature of the liquid is 160 DEG C, maintaining the temperature for 0.5-2 hours, cooling, carrying out suction filtration so as to obtain white sodium chloride crystal, and using filtrate indiscriminately. Polyethylene glycol is taken as a solvent and is non-toxic, low in odor, high in boiling point, easy to separate, recycle and indiscriminately use and low in loss; the reaction temperature is high, the procedure is simple, the sodium chloride content is high after reaction and is over 98.5%, and sodium chloride has good appearance and color and is a white crystal; and by virtue of high-boiling-energy circular indiscriminate use, only one product, namely sodium chloride is produced, so that the treatment is easy.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis waste treatment, in particular to a method for treating mother liquor slag of triazine ring sodium salt. Background technique [0002] At present, the company produces triazine ring products, which are intermediates of pharmaceutical cephalosporins. During the production process, the mother liquor of triazine ring sodium salt is processed to obtain triazine ring slag. The slag mainly contains sodium oxalate and sodium acetate and a small amount of sodium sulfate, sodium triazine ring salt, sodium carbonate, and the mother liquor of triazine ring sodium salt after alkalization. , the processing cost is too high; in order to reduce production costs and increase profits, the company has independently developed and processed the mother liquor slag of triazine ring sodium salt, and successively used the methods of patent CN 105330545 B and CN 106349068 A to solve the problem that the current...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01D3/08
CPCC01D3/08C01P2006/80
Inventor 黄明路朱传伟姜福元李保铃孙成斌殷福东
Owner SHANDONG HUIHAI PHARMA & CHEM