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Method for recovering phenylbutazone from phenylbutazone refined product mother solution waste residues

A technology of phenylbutazone and mother liquor, which is applied in the field of medicine and chemical industry, can solve the problems of old oil residue, easy decomposition of phenylbutazone, destruction of phenylbutazone, etc., and achieves improved productivity, obvious economic and environmental benefits, and reduced production costs. Effect

Inactive Publication Date: 2016-05-25
JINGHUA PHARMA GRP NANTONG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the production process, the mother liquor of butyl pine fine-quality products contains 8-12% of the product, but butyl pine is easy to decompose when heated at high temperature, and the process of recovering ethanol by steam heating and evaporating to dryness destroys butyl pine and turns it into old oil The residue cannot be further recovered, so it is necessary to study the recovery method to recover the residual phenylbutazone in the mother liquor

Method used

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  • Method for recovering phenylbutazone from phenylbutazone refined product mother solution waste residues

Examples

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Effect test

Embodiment 1

[0023] Such as figure 1 Shown, the method for reclaiming butyl pine from butyl pine fine-art mother liquor waste residue of the present invention may further comprise the steps:

[0024] (1) Take the 8wt% phenylbutazone fine mother liquor and place it in the recycling tank, heat and reduce pressure in a water bath to recover ethanol, control the temperature of the water bath below 40°C, and keep the vacuum at -0.098MPa. The concentrated hydraulic pressure after recovering ethanol is put into cold crystallization In the pot, cool to 5°C to crystallize, and then centrifuge to obtain the recovered product of phenylbutazone and the secondary mother liquor, and the secondary mother liquor is used for further recovery of phenylbutazone;

[0025] (2) Adjust the pH of the secondary mother liquor obtained in step (1) to above 12 with NaOH with a mass concentration of 5%, and then heat and reduce pressure in a water bath to recover ethanol. The concentrated solution is diluted with wat...

Embodiment 2

[0028] Such as figure 1 Shown, the method for reclaiming butyl pine from butyl pine fine-art mother liquor waste residue of the present invention may further comprise the steps:

[0029] (1) Take 2wt% phenylbutazone fine-quality mother liquor and put it in the recovery tank, heat and reduce pressure in a water bath to recover ethanol, control the temperature of the water bath below 40°C, and keep the vacuum at -0.09MPa. The concentrated hydraulic pressure after recovering ethanol is put into cold crystallization In the pot, cool to 0°C to crystallize, and then centrifuge to obtain the recovered product of phenylbutazone and the secondary mother liquor, where the secondary mother liquor is used for further recovery of phenylbutazone;

[0030] (2) Adjust the pH of the secondary mother liquor obtained in step (1) to above 12 with NaOH with a mass concentration of 5%, and recover ethanol by heating in a water bath under reduced pressure. The temperature of the water bath is below ...

Embodiment 3

[0033] Such as figure 1 Shown, the method for reclaiming butyl pine from butyl pine fine-art mother liquor waste residue of the present invention may further comprise the steps:

[0034] (1) Take 10wt% phenylbutazone fine-quality mother liquor and put it in the recovery tank, heat and reduce pressure in a water bath to recover ethanol, control the temperature of the water bath below 40°C, and keep the vacuum at -0.094MPa, and the concentrated hydraulic pressure after recovering ethanol is put into cold crystallization In the pot, cool to 3°C to crystallize, and then centrifuge to obtain the recycled phenylbutazone and the secondary mother liquor, where the secondary mother liquor is used for further recovery of phenylbutazone;

[0035] (2) Adjust the pH of the secondary mother liquor obtained in step (1) to above 12 with NaOH with a mass concentration of 5%, and then heat and reduce pressure in a water bath to recover ethanol. The concentrated solution is diluted with water, ...

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Abstract

The invention relates to a method for recovering phenylbutazone from phenylbutazone refined product mother solution waste residues. The method comprises the following steps: (1) heating a phenylbutazone mother solution under reduced pressure to recover ethanol, cooling to crystallize, and centrifugating to obtain a phenylbutazone recovery product and a secondary mother solution; (2) regulating the pH value of the phenylbutazone secondary mother solution obtained in the step (1) with dilute alkali to 12 or above, heating under reduced pressure to recover ethanol, and neutralizing with glacial acetic acid until phenylbutazone crystals precipitate, thereby obtaining the phenylbutazone recovery product; and (3) carrying out alkali fusion acid precipitation on the phenylbutazone recovery product obtained in the step (1) and step (2) to obtain a phenylbutazone crude product for further refinement. The method can recover the ethanol without destroying the residual phenylbutazone in the mother solution and further recycle the phenylbutazone, thereby enhancing the product yield and lowering the production cost.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and in particular relates to a method for recovering phenylbutazone from the waste residue of the fine-quality mother liquor of phenylbutazone. Background technique [0002] The effect of phenylbutazone is similar to that of aminopyrine, and it is effective for rheumatic pain and gout. It is mainly used to treat rheumatoid arthritis and gout. For non-rheumatic patients, the analgesic effect seems to be stronger than that of aspirin. Because rheumatic pain and other diseases are easy to relapse, it is often necessary to use phenylbutazone or interact with other drugs in combination. In addition, phenylbutazone can also be used to treat acute lymphangitis of filariasis (flowing fire), and the indications are preferably for patients with early filariasis without obvious secondary infection. [0003] At present, the preparation method of phenylbutazone is roughly as follows: f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D231/34
CPCC07D231/34
Inventor 严宾吴玉祥袁拥军
Owner JINGHUA PHARMA GRP NANTONG
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