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Recovery method of dmf and inorganic salt in ceftazidime side chain ester wastewater

A ceftazidime and recovery method technology, applied in the field of waste water treatment and recovery, can solve the problems of harsh use conditions, low efficiency, high recovery cost, etc., and achieve the effects of high recovery rate, simple process, and shortened recovery time

Active Publication Date: 2020-09-04
YIYUAN XINQUAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In view of the simple domestic DMF recovery device, high energy consumption and expensive recovery cost, recycling is of little significance to some enterprises
In the process of recycling inorganic salts, the use of traditional process equipment for recycling is easy to block the pipeline and there are problems of difficult recovery and low efficiency. Therefore, finding a method for efficient recovery of DMF and inorganic salts will reduce enterprise costs and relieve environmental pressure.
[0004] According to relevant literature reports, Xu Jiewen and others used activated carbon adsorption method when studying low-content DMF wastewater. This method is only suitable for the recovery of low-concentration DMF; Xu Mingxian and others used supercritical water oxidation to treat DMF wastewater and removed a large amount of CODcr. Improves the biodegradability of wastewater. This method is more suitable for treating high-concentration organic wastewater that is difficult to biodegrade, but the conditions are harsh and it is difficult to use it on a large scale.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 1000mL of etherified wastewater, add 2000mL of chloroform for extraction, extract three times in total, the extraction time is 10min, and the standing time is 10min, and the chloroform phase and the water phase are combined for later use.

[0022] The combined chloroform phases were distilled under reduced pressure, and a small amount of CaCO was placed at the bottom of the distillation flask 3 , the pressure is not lower than -0.08MPa, the temperature range is 35 ± 25 ° C, until there is no liquid in the distillate phase, the collected distillate chloroform continues to be used as an extraction agent, and the remaining organic phase in the bottom flask is DMF ( About 131mL), the recovery rate is 87.3%, the purity is 99.2%, and the water content is 0.07%; the combined water phase is added to the scraper evaporator, the vacuum distillation pressure is -0.08MPa, and the jacket temperature is not lower than 75°C , until all the water is evaporated, the salt in the bot...

Embodiment 2

[0024] Take 1000mL of etherified wastewater, add 2500mL of chloroform for extraction, and extract four times in total. The extraction time is 15 minutes, and the resting time is 10 minutes. The chloroform phase and the water phase are combined for later use.

[0025] The combined chloroform phases were distilled under reduced pressure, and a small amount of CaCO was placed at the bottom of the distillation flask 3 , the pressure is not lower than -0.08MPa, the temperature range is 35 ± 25 ° C, until there is no liquid in the distillate phase, the collected distillate chloroform continues to be used as an extraction agent, and the remaining organic phase in the bottom flask is DMF ( About 132mL), the recovery rate is 88%, the purity is 99.5%, and the water content is 0.06%; the combined aqueous phase is added to the scraped evaporator, the vacuum distillation pressure is -0.08MPa, and the jacket temperature is not lower than 75°C , until all the water is evaporated, the salt in...

Embodiment 3

[0027] Take 1000mL of etherified wastewater, add 3000mL of chloroform for extraction, extract five times in total, the extraction time is 15min, and the standing time is 10min, and the chloroform phase and the water phase are combined for later use.

[0028] The combined chloroform phases were distilled under reduced pressure, and a small amount of CaCO was placed at the bottom of the distillation flask 3 , the pressure is not lower than -0.08MPa, the temperature range is 35 ± 25 ° C, until there is no liquid in the distillate phase, the collected distillate chloroform continues to be used as an extraction agent, and the remaining organic phase in the bottom flask is DMF ( about 134mL), the recovery rate was 89.3%, the purity was 99.1%, and the moisture content was 0.09%; the combined aqueous phase was added to a scraped evaporator, the vacuum distillation pressure was -0.08MPa, and the jacket temperature was not lower than 75°C , until all the water is evaporated, the salt in...

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Abstract

The invention relates to a method for recovering DMF and inorganic salts from ceftazidime side chain ester wastewater, and belongs to the technical field of wastewater treatment and recovery. The method for recovering DMF and inorganic salts from ceftazidime side chain ester wastewater comprises the following steps: extracting the ceftazidime side chain ester wastewater to obtain a water phase andan organic phase, recovering the water phase by a scraper evaporator to remove water, collecting the inorganic salts, and introducing HBr gas to the inorganic salts to completely convert excess K2CO3into KBr; and carrying out reduced pressure rectification on the organic phase to obtain DMF and an extractant which can be repeatedly used. The method for recovering DMF and inorganic salts from theceftazidime side chain ester wastewater has the advantages of simplicity and convenience in operation, improvement of the recovery rate of the solvent and the inorganic salts, reduction of the cost of enterprises, and reduction of the pollution to the environment.

Description

technical field [0001] The invention relates to a method for recovering DMF and inorganic salts in ceftazidime side chain ester waste water, belonging to the technical field of waste water treatment and recovery. Background technique [0002] Ceftazidime side-chain esters are important intermediates in the synthesis of ceftazime active esters, and their quality and cost have an important impact on raw materials. Using DMF as solvent during the synthesis of ceftazidime side chain ester, K 2 CO 3 As an acid-binding agent, wastewater contains a certain amount of DMF and inorganic salts (KBr and excess K 2 CO 3 ), if the wastewater is directly discharged, it will cause serious environmental pollution and economic losses. [0003] DMF wastewater is highly toxic and needs to be treated before being discharged. At present, the methods for recovering DMF mainly include: chemical method (alkalinization method), biochemical method, physicochemical method (adsorption, rectificatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C02F9/10C07C231/24C07C233/03C01D3/10C02F103/36
CPCC01D3/10C02F1/04C02F1/26C02F9/00C02F2103/36C02F2301/08C07C231/24C07C233/03
Inventor 张艳红张立明
Owner YIYUAN XINQUAN CHEM