Method for recovering sodium theophylline mother liquid

A technology for recycling and processing tea sodium, which is applied in organic chemistry and other fields, can solve problems such as low efficiency, decreased ability to absorb tea sodium, and reduced efficiency of analyzing tea sodium, and achieve the effect of improving quantity and quality

Active Publication Date: 2013-08-14
CSPC INNOVATION PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In actual production, the efficiency of the existing process for recovering tea sodium is not high, which is mainly due to the fact that the mother liquor of tea sodium contains more impurities, so that after repeated use of the macroporous adsorption resin, on the one hand, its ability to absorb tea sodium decreases. On the other hand, the efficiency of analyzing tea sodium is also significantly reduced, and the COD value of the raffinate discharged after analysis is also large, which requires additional regeneration of the macroporous adsorption resin, and the frequent regeneration of the resin leads to a shortened service life of the resin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] a) Use concentrated sulfuric acid with a concentration of 92% to neutralize the tea sodium mother liquor with a content of 0.75%, adjust the pH value to 5.5, and obtain the tea sodium mother liquor neutralized by acid, and then pass 500ml of the tea sodium mother liquor neutralized by acid Column volume is the strong base negative 204 macroporous adsorption resin column of 60ml, obtains the macroporous adsorption resin that is adsorbed with tea sodium, collects the raffinate that flows out by macroporous adsorption resin column simultaneously;

[0016] b) Mix 2ml of methanol, 18ml of lauric acid diethanolamide surfactant, and 180ml of water to make a resin regeneration solution;

[0017] c) Under the ultrasonic field of 20KHz, let the resin regeneration solution pass through the macroporous adsorption resin column to decompose the tea sodium, and obtain the analysis solution dissolved in tea sodium;

[0018] d) Concentrate and centrifuge the obtained analytical solution...

Embodiment 2

[0023] a) Use concentrated sulfuric acid with a concentration of 92% to neutralize the tea sodium mother liquor with a content of 0.50%, adjust the pH value to 6.0, and obtain the tea sodium mother liquor neutralized by acid, and then pass 500ml of the tea sodium mother liquor neutralized by acid Column volume is the strong base negative 207 macroporous adsorption resin column of 60ml, obtains the macroporous adsorbent resin that is adsorbed with tea sodium, collects the raffinate that flows out by macroporous adsorbent resin simultaneously;

[0024] b) Mix 95ml of isopropanol, 95ml of tert-butanol, 18ml of Tween 60 surfactant and 2ml of water to make a resin regeneration solution;

[0025] c) Under the ultrasonic field of 60KHz, let the resin regeneration solution pass through the macroporous adsorption resin column, so as to analyze the tea sodium, and obtain the analysis solution dissolved in tea sodium;

[0026] d) Concentrate and centrifuge the obtained analytical solutio...

Embodiment 3

[0031] a) Use concentrated sulfuric acid with a concentration of 92% to neutralize the tea sodium mother liquor with a content of 0.80%, adjust the pH value to 6.5, and obtain the tea sodium mother liquor neutralized by acid, and then pass 500ml of the tea sodium mother liquor neutralized by acid Column volume is the strong base negative 297 macroporous adsorption resin column of 60ml, obtains the macroporous adsorbent resin that is adsorbed with tea sodium, collects the raffinate that flows out by macroporous adsorbent resin simultaneously;

[0032] b) Mix 20ml of acetone, 20ml of ethanol, 60ml of alkanolamide surfactant and 100ml of water to make a resin regeneration solution;

[0033] c) Under the ultrasonic field of 30KHz, let the resin regeneration solution pass through the macroporous adsorption resin column to decompose the tea sodium, and obtain the analysis solution dissolved in tea sodium;

[0034] d) Concentrate and centrifuge the obtained analytical solution to obt...

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PUM

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Abstract

The invention discloses a method for recovering sodium theophylline mother liquid. The method comprises the following steps of: neutralizing the sodium theophylline mother liquid by using concentrated sulfuric acid, and enabling the neutralized sodium theophylline mother liquid to pass through macroporous adsorption resin so as to obtain sodium theophylline adsorbed macroporous adsorption resin; preparing a resin regeneration solution from 1-95% of organic solvent, 4-30% of surfactant and 1-95% of water; and in ultrasonic wave fields, desorbing the sodium theophylline adsorbed macroporous adsorption resin by using the resin regeneration solution so as to obtain sodium theophylline desorbed liquid, and then, concentrating and centrifuging so as to obtain solid sodium theophylline. By adopting the method disclosed by the invention to recover the sodium theophylline mother liquid, the macroporous adsorption resin still has relatively-high adsorption ratio and desorption ratio after repeated use, the sodium theophylline adsorption ratio is increased to about 90% from original 60-70%, the desorption ratio is increased to about 95% from about 85%, the COD (Chemical Oxygen Demand) of the discharged residual liquid is decreased to about 10,000 mg / L from original average 13,000 mg / L, and the number and quality of the recovered sodium theophylline are greatly increased.

Description

technical field [0001] The invention relates to a treatment method for a chemical mother liquor, in particular to a recycling and treatment method for a tea sodium mother liquor. Background technique [0002] Theophylline sodium salt is referred to as tea sodium for short, and its chemical name is 1,3-dimethylxanthine sodium salt. The tea sodium solid material is obtained by centrifugation after synthesis, nitrosation, reduction, formylation, and ring closure reactions. At the same time, the mother liquor produced during the centrifugation process contains 0.5%-0.8% tea sodium. If it is not treated, it will lose hundreds of dollars per year. tons of tea sodium, so the current industry mostly adopts macroporous adsorption resin for recovery. The process is generally as follows: neutralize the tea sodium mother liquor with acid → absorb the tea sodium in the mother liquor through the macroporous adsorption resin → analyze the tea sodium on the macroporous adsorption resin wit...

Claims

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Application Information

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IPC IPC(8): C07D473/08
Inventor 刘健张浩赵旭姚彩霞黄玉睿孙志伟
Owner CSPC INNOVATION PHARMA
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