Recovering and separation method for iodine in cefepime waste liquid

A recovery method and waste liquid technology, applied in the direction of iodine, iodine/hydrogen iodide, etc., can solve the problems of difficult iodine recovery, imminent recovery of iodine, waste of iodine, etc., and achieve the effects of less entrained impurities, cost saving, and simple process route

Active Publication Date: 2019-04-16
SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK CO LTD +2
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AI Technical Summary

Problems solved by technology

[0003] At present, most of the production of cephalosporins in my country does not recover iodine from the waste liquid. The iodide ion in the waste liquid of cefepime comes from trimethylsiliodinane, and the industrial production of cefepime 3-substituted intermediate requires excessive trimethyl Only iodosilane can complete the iodine reaction, and then the iodide ion in the compound undergoes an ion exchange reaction with an anion, so that the iodine in all the trimethylsiliodones used in the reaction exists in the form of iodide ions in the cephalosporin waste liquid However, because the hydroiodic acid produced by the reaction exists in the solution, it combines with cephalosporins to form hydroiodide, which makes the recovery of iodine difficult.
Since iodine is a precious metal, this phenomenon causes the waste of iodine, so the recovery of iodine is imminent

Method used

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  • Recovering and separation method for iodine in cefepime waste liquid

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Experimental program
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Effect test

Embodiment 1

[0026] Add 3L of cefepime waste liquid into the stirred reactor, the lye is 20% sodium hydroxide, adjust the pH=12 to separate the lye, stir and heat to hydrolyze, the heating temperature is 90℃, after separating the organic phase, add 36% Adjust pH to 0.5 with hydrochloric acid, continue to heat and hydrolyze for 3h, recover the water phase, cool, pass into the oxidation extraction tower, 25.8g sodium nitrite for oxidation reaction for 10min, then spray methylene chloride on the top of the tower, extract until the purple color disappears in the water phase , The organic phase flows into the vacuum distillation kettle, the pressure is 0.15MPa, the temperature is 12°C, and most of the extractant dichloromethane is evaporated for recycling. The remaining components continue to be sealed and heated to 30°C under vacuum, and the temperature rises by 1°C every 10 minutes. The elemental iodine is sublimated, and then the distillation kettle is cooled down, and the iodine is sublimed t...

Embodiment 2

[0028] Add 4L cefepime waste liquid into the stirred reactor, the lye is 20% potassium hydroxide, adjust the pH=13 to separate the lye, stir and heat to hydrolyze, the heating temperature is 120℃, after separating the organic phase, add 36% Adjust pH=2 with hydrochloric acid, continue to heat and hydrolyze for 3h, recover the water phase, cool, pass into the oxidation extraction tower, 90g sodium nitrite for oxidation reaction for 20min, then spray ether at the top of the tower, extract until the purple color disappears in the water phase and the organic phase Flow into the vacuum distillation kettle, the pressure is 0.08MPa, the temperature is 18°C, most of the extractant ether is distilled out for recycling, and the remaining components continue to be sealed and heated to 30°C under vacuum, and the iodine elemental substance is sublimated every 15 minutes. The distillation kettle is cooled down and the iodine is sublimed to obtain a pure product with a recovery rate of 98.7% a...

Embodiment 3

[0030] Add 1L of cefepime waste liquid into the stirred reactor, the lye is 30% sodium hydroxide, adjust the pH=13 to separate the lye, stir and heat to hydrolyze, the heating temperature is 120℃, after separating the organic phase, add 36% Adjust pH to 1.5 with hydrochloric acid, continue to heat and hydrolyze for 2h, recover the water phase, cool, pass into the oxidation extraction tower, 20g sodium nitrite for oxidation reaction for 30min, then spray methylene chloride on the top of the tower, extract until the purple color disappears in the water phase. The organic phase flows into the vacuum distillation kettle, the pressure is 0.1MPa, the temperature is 15°C, and most of the extractant dichloromethane is evaporated for recycling. The remaining components continue to be sealed and heated to 30°C under vacuum, and 1°C rises every 15 minutes. The simple substance is sublimated, and then the distillation kettle is cooled and the temperature is lowered to obtain a pure product ...

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Abstract

The invention discloses a recovering and separation method for iodine in cephalosporin medicine waste liquid. The method comprises the following steps that alkali is added into the cephalosporin medicine waste liquid, methyl alcohol, acetone and alkali liquid are extracted and separated, the alkali liquid is circularly heated and hydrolyzed, and after filtering, the alkali liquid is conveyed intoan acidizing groove for acidification; organic matter which cannot be dissolved in water is removed through standing and layering, then a water-phase oxidation reaction tower oxidizes I- into IO3-, the alkali liquid is introduced in a reduction kettle, and the IO3- is reduced into I2; simple substance iodine is separated out, after filtering and recovering, crude iodine is obtained, and heating, sublimation and condensation continue to obtain the simple substance iodine. According to the method, precious metal iodine in the waste liquid is recovered, through alkali addition for hydrolyzing andacidizing, iodine exists in the waste liquid in a free state, and the organic matter which cannot be dissolved in water is separated out. According to the method, it is not necessary to strictly control the dosage of an oxidizing agent, the operation is simple and safe, the rate of recovering iodine reaches 98.5% or above, and the method is suitable for process scale-up production.

Description

Technical field [0001] The invention relates to a method for recovering and separating iodine in cefepime waste liquid. Background technique [0002] Cefepime, a new generation of cephalosporins, is mainly used for urinary tract infections, skin infections, abdominal infections, gynecological infections and sepsis caused by sensitive bacteria infections. Cefepime is the fourth-generation cephalosporin and the third Compared with other generations, its antibacterial effect has been further developed, with balanced antibacterial properties and good antibacterial activity against negative bacilli. These characteristics make it a more widely accepted antibacterial drug in clinical medicine in the future. [0003] At present, most of the production of cephalosporins in China does not recover iodine in the waste liquid. The iodine ion in the cefepime waste liquid is derived from trimethylsiliodane. The production of cefepime 3-substituted intermediates in industry requires excessive trim...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B7/14
CPCC01B7/14
Inventor 刘明霞李强张以鹏
Owner SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK CO LTD
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