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Method for recycling DL-lysine hydrochloride from aspirin-DL-lysine mother liquor

A technology of lysine hydrochloride and lysine-pirin, which is applied in the field of recovery of DL-lysine hydrochloride from lysine-pirin mother liquor, can solve the problems of difficulty, difficult waste liquid treatment, waste, etc. Achieve the effect of avoiding waste, saving energy and cost, high economic benefit and social benefit

Active Publication Date: 2011-05-18
蚌埠丰原涂山制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, it is a waste to only recover ethanol from the mother liquor and treat it as waste liquid, because it contains many useful substances after all; at the same time, the concentration of the above-mentioned tower bottom liquid is relatively large, and the COD is as high as 225,000. If it is directly discharged as waste liquid, it will pollute the environment, but Difficult to process and expensive
Therefore, the treatment of this waste liquid is a difficult problem.

Method used

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  • Method for recycling DL-lysine hydrochloride from aspirin-DL-lysine mother liquor
  • Method for recycling DL-lysine hydrochloride from aspirin-DL-lysine mother liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Acid separation and precipitation

[0031] Take the lysine-pirin mother liquor, recover ethanol with a distillation tower, take 1000ml of the bottom liquid, stir, add 30ml of hydrochloric acid, adjust the pH to 3, heat to 90°C, keep for 30 minutes, cool to 20°C, filter to obtain the filtrate.

[0032] (2) concentrated

[0033] The filtrate was put into a still, and concentrated in vacuum at 70°C until the concentration of DL-lysine hydrochloride was 60%.

[0034] (3) Precipitation

[0035] Measure the concentrated solution, add 1 times the amount of glacial acetic acid dropwise, slowly cool down to 10°C, keep warm for 3 hours, shake off, wash once with a small amount of glacial acetic acid or absolute ethanol to obtain DL-lysine hydrochloride.

[0036] (4) Content determination

[0037] Using the perchloric acid method, the content of DL-lysine hydrochloride was measured to be 97.5%.

[0038] The COD value of the lysine-pirin mother liquor after treatment is 66,...

Embodiment 2

[0040] (1) Acid separation and precipitation

[0041] Take the lysine-pirin mother liquor, recover ethanol with a distillation tower, take 1000ml of the bottom liquid, stir, add 50ml of hydrochloric acid, adjust the pH to 2, heat to 80°C, keep for 25 minutes, cool to 18°C, filter to obtain the filtrate.

[0042] (2) concentrated

[0043] The filtrate was put into a distillation pot and concentrated in vacuum at 75°C until the concentration of DL-lysine hydrochloride was 65%.

[0044] (3) Precipitation

[0045] Measure the concentrated solution, add 1.5 times the amount of glacial acetic acid dropwise, slowly cool down to 8°C, keep warm for 3 hours, shake off, wash once with a small amount of glacial acetic acid or absolute ethanol to obtain DL-lysine hydrochloride.

[0046] (4) Content determination

[0047] Using the perchloric acid method, the content of DL-lysine hydrochloride was measured to be 99.1%.

[0048] The COD value of the lysine-pirin mother liquor after treat...

Embodiment 3

[0050] (1) Acid separation and precipitation

[0051] Take the lysine-pirin mother liquor, recover ethanol with a distillation tower, take 1000ml of the bottom liquid, stir, add 70ml of hydrochloric acid, adjust the pH to 1.5, heat to 80°C, keep for 20 minutes, cool to 15°C, filter to obtain the filtrate.

[0052] (2) concentrated

[0053] The filtrate was put into a still, and concentrated in vacuum at 80°C until the concentration of DL-lysine hydrochloride was 70%.

[0054] (3) Precipitation

[0055] Measure the concentrated solution, add 1 times the amount of absolute ethanol dropwise, slowly cool down to 5°C, keep warm for 4 hours, shake off, wash once with an appropriate amount of glacial acetic acid or absolute ethanol to obtain DL-lysine hydrochloride.

[0056] (4) Content determination

[0057] Using the perchloric acid method, the content of DL-lysine hydrochloride was measured to be 98.6%.

[0058] The COD value of the lysine-pirin mother liquor after treatment is ...

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Abstract

The invention relates to a method for recycling DL-lysine hydrochloride from aspirin-DL-lysine mother liquor, comprising the steps of: evaporating out ethanol, adding hydrochloric acid for separation and precipitation, concentrating filtrate and separating out crystals. The method disclosed by the invention has the advantages of simplicity and high product purity, and the recycled DL-lysine hydrochloride can be used as an intermediate for further synthesis of aspirin-DL-lysine, therefore, the production cost is greatly saved and reduced, the difficulty in waste water treatment and environmental pollution are simultaneously reduced, and the economic and social benefits are improved.

Description

technical field [0001] The invention relates to a method for recovering DL-lysine hydrochloride, in particular to a method for recovering DL-lysine hydrochloride from lysine-pirin mother liquor. Background technique [0002] Lysine, also known as aspirin lysine salt or lysine acetylsalicylic acid, is a double salt of aspirin and lysine. Its production process is to drop DL-lysine solution into aspirin ethanol solution to precipitate Ampirin. [0003] Since lysine is easily hydrolyzed, the composition of its mother liquor is relatively complex, mainly containing ethanol, water, lysine, lysine salicylate, acetic acid and other impurities, so the mother liquor cannot be used to apply or recover lysine Pirin. The processing method of this mother liquor is to reclaim ethanol with distillation tower at present, and the residual tower bottom liquid (brown aqueous solution) is treated as waste liquid. [0004] However, it is a waste to only recover ethanol from the mother liquor ...

Claims

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Application Information

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IPC IPC(8): C07C229/26C07C227/18
Inventor 谢延汪洪湖
Owner 蚌埠丰原涂山制药有限公司
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