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Method for recovering tetramethyl guanidine

A technology of tetramethylguanidine and extraction solvent, which is applied in the field of recovery of tetramethylguanidine, can solve the problems of increased environmental burden and waste, and achieve the effect of improving recovery rate and weakening the occurrence of hydrolysis reaction

Inactive Publication Date: 2004-11-17
吉林省石油化工设计研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This not only increases the burden on the environment, but also causes waste

Method used

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  • Method for recovering tetramethyl guanidine
  • Method for recovering tetramethyl guanidine

Examples

Experimental program
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Effect test

Embodiment 1

[0027] 1) Concentrate in a 2000ml four-necked flask, add 1200 grams of tetramethylguanidine-containing wastewater produced at the time of synthesizing cephera, neutralize it with sodium hydroxide or hydrochloric acid aqueous solution to a pH of 6-7, and distill under reduced pressure to remove it. Of the water to produce solid salt.

[0028] 2) Reduce the solid salt, transfer it to a 1000ml four-necked flask, add 400ml of toluene, add a water separator and a dropping funnel, stir quickly, add dropwise 45ml of 30% sodium hydroxide aqueous solution at 20°C, The dripping is completed within 2 hours. After the reaction is completed, heat and increase the temperature to azeotropically dehydrate until there is no more water out of the water separator. Remove the water separator, install a fractionating column, heat and fractionate under normal pressure, recover most of the toluene solvent, and continue to reuse. The remaining product was further distilled under reduced pressure at 130°C...

Embodiment 2

[0031] 1) Concentrate in a 2000ml four-necked flask, add 1200 grams of tetramethylguanidine-containing wastewater produced at the time of synthesis of cephera, neutralize it with sodium hydroxide or hydrochloric acid to a pH of 6-7, and distill under reduced pressure to remove the content Moisture makes solid salt.

[0032] 2) Reduce the solid salt and smash it into a 1000ml four-necked flask, add 450ml of toluene, add a water separator and a dropping funnel, stir quickly, add dropwise 45ml of 30% potassium hydroxide aqueous solution at 30℃, below As in Example 1, the total recovery rate of tetramethylguanidine is 55.8%.

Embodiment 3

[0034] 1) Concentrate in a 2000ml four-necked flask, add 1200 grams of tetramethylguanidine-containing wastewater produced at the time of synthesis of cephera, neutralize it with sodium hydroxide or hydrochloric acid to a pH value of 6-7, and distill under reduced pressure to remove the content 1000 grams of water.

[0035] 2), reduction Move the concentrate to a 1000ml four-necked bottle, add 400ml of toluene, add a water separator and a dropping funnel, heat to increase temperature, azeotropic dehydration, until there is no more water out of the water separator. The temperature was lowered, and 45 ml of a 30% sodium hydroxide aqueous solution was added dropwise at 40°C, and the addition was completed within 2 hours. The following steps are the same as in Example 1, and the total recovery rate of tetramethylguanidine is 54.6%.

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Abstract

The invention provides a process for recovering tetramethylguanidine which comprises, using wastewater produced in the process of cephalosporin antibiotics synthesis as raw material, proceeding the three procedures of condensation, reduction and separation, with the action or water non-dissoluble organic extraction solvent, reacting caustic alkali with the tetramethylguanidine in the waste water, producing free tetramethylguanidine, and the high purity tetramethylguanidine can be obtained further crude steaming separation and vacuum rectification.

Description

Technical field [0001] The invention relates to a method for recovering tetramethylguanidine. In particular, it relates to a method for recovering 1,1,3,3-tetramethylguanidine, which is a carboxyl protective agent as a pharmaceutical synthesis auxiliary, that is, a method for recovering tetramethylguanidine from waste water produced in the process of preparing cephalosporin antibiotics. Background technique [0002] Tetramethylguanidine is an important organic synthesis intermediate. It is expensive and can be used as a catalyst for polyurethane foam. It is also used for levelling of nylon (nylon), wool and other proteins. It is used for cephalosporin in the pharmaceutical industry. Synthesis of a series of antibiotics. [0003] In the process of synthesizing cephalosporin antibiotics, 1,1,3,3-tetramethylguanidine is widely used as a carboxyl protective agent, and the amount is large. In the late stage of antibiotic synthesis, it is necessary to acidify the reaction product to re...

Claims

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Application Information

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IPC IPC(8): C07C277/08C07C279/04
Inventor 李东阳杨文库苗春山王欣然魏巍王松林
Owner 吉林省石油化工设计研究院
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