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Extraction method of methyl isobutyl ketone and sodium p-toluenesulfonate

A technology of methyl isobutyl ketone and sodium p-toluenesulfonate, applied in chemical instruments and methods, separation/purification of carbonyl compounds, preparation of organic compounds, etc., can solve the problems of high processing difficulty, low product content and high cost , to achieve the effect of good product quality, simple operation and low cost

Active Publication Date: 2020-03-27
河北威远药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After simple activated carbon decolorization and water recrystallization, it is still difficult to remove the strong odor, and because it contains crystal water, the product content is very low, about 78-93%, and the commercial value is limited
In addition, the above two extraction methods are difficult to use together, and the concentration of organic matter in tiamulin wastewater is very high, and the COD of wastewater is too high, resulting in difficult treatment and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 1L of tiamulin production wastewater and distill it under normal pressure. After the temperature of the wastewater rises above 98°C, stop the distillation to obtain 137mL of the distilled water and organic phase mixture; after cooling down to below 30°C, separate the liquids , remove the water layer, use biodegradation technology for degradation treatment, separate the organic phase to 68mL, add 3.5g of quicklime to the separated organic phase, raise the temperature to 50-55°C, stir for 0.5-1.0 hours, and then under 0.08MPa Distill under reduced pressure to obtain 63 mL of high-purity methyl isobutyl ketone.

[0024] Concentrate the waste water mother liquor remaining from the initial atmospheric distillation to 0.7-0.75L under reduced pressure at 0.085MPa, cool down to 25-30°C, and filter. The weight of the filter cake is 122g. The obtained filter cake is further extracted with sodium p-toluenesulfonate. The COD value of the treated wastewater is 45900mg / L, and th...

Embodiment 2

[0026] Take 2L of tiamulin production waste water and carry out distillation under normal pressure. The distillation temperature is 85-98°C. After the waste water temperature rises above 98°C, stop the distillation to obtain 262mL of the distilled water and organic phase mixture ; After the temperature was lowered to below 30°C, the liquid was separated, and the water layer was separated to obtain 133 mL of the organic phase. Add 7.0 g of quicklime to the separated organic phase, raise the temperature to 50-55° C., stir for 0.5-1.0 hours, and then distill under reduced pressure at 0.08 MPa to obtain 122 mL of high-purity methyl isobutyl ketone.

[0027] Concentrate the waste water mother liquor remaining from the initial atmospheric distillation to 1.4-1.5L under reduced pressure at 0.085MPa, cool down to 25-30°C, and filter. The weight of the filter cake is 251g. The obtained filter cake was further extracted with sodium p-toluenesulfonate, and the COD value of the treated wa...

Embodiment 3

[0029] Take 5L of tiamulin production wastewater and distill it under normal pressure. The distillation temperature is 85-98°C. After the temperature of the wastewater rises above 98°C, stop the distillation to obtain 692mL of the distilled water and organic phase mixture ; After cooling down to below 30°C, separate the liquid and remove the water layer to obtain 344mL of the organic phase; add 17.5g of quicklime to the separated organic phase, raise the temperature to 50-55°C, stir for 0.5-1.0 hours, and then under 0.08MPa Distill under reduced pressure to obtain 321 mL of high-purity methyl isobutyl ketone.

[0030] Concentrate the waste water mother liquor remaining from the initial atmospheric distillation to 3.5L-3.75L under reduced pressure at 0.085MPa, cool down to 25-30°C, and filter. The weight of the filter cake is 608g. The obtained filter cake was further extracted with sodium p-toluenesulfonate, and the COD value of the treated wastewater was 46128mg / L, and the we...

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Abstract

The invention relates to an extraction method of methyl isobutyl ketone and sodium p-toluenesulfonate. The extraction method comprises the following steps: carrying out atmospheric distillation on high-concentration tiamulin wastewater to distill out a mixed solution of an organic phase and water; cooling, carrying out liquid separation on the mixed solution, removing the water layer to obtain anorganic phase, adding calcium oxide into the organic phase, removing water and carrying out reduced pressure distillation to obtain high-purity methyl isobutyl ketone; carrying out vacuum concentration, cooling, separating out crystals and filtering on the residual wastewater mother liquor after distilling and separating out the organic phase and water mixed liquor; adding a solvent into the filter cake, heating and carrying out reflux water diversion; and after water separation, cooling, filtering and drying the filter cake to obtain high-purity sodium p-toluenesulfonate. The extraction method is simple, the extracted methyl isobutyl ketone and sodium p-toluenesulfonate are high in purity and the COD value of wastewater is greatly reduced.

Description

technical field [0001] The invention relates to a method for extracting and purifying methyl isobutyl ketone and sodium p-toluenesulfonate from tiamulin wastewater, belonging to the technical field of wastewater treatment. Background technique [0002] Tiamulin is fermented by the higher fungus Basidiomycetes Pleurotus mutilus to obtain pleuromutilin, and then chemically synthesized to obtain hydrogenated fumarate. It is a diterpene antibiotic for livestock and poultry. The synthesis process of tiamulin is a one-step sulfonation reaction, that is, the sulfonation reaction of pleuromutilin and p-toluenesulfonyl chloride to obtain an intermediate, which is then acylated with ethanethiol to generate the product tiamulin. After the reaction of this step is completed, solids containing a large amount of sodium p-toluenesulfonate will be separated out after cooling down. After centrifugation, the reaction solution must be separated to separate the water layer and washed before pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/82C07C49/04C07C303/44C07C309/30
CPCC07C45/82C07C303/44C07C49/04C07C309/30
Inventor 赵盼聂丰秋贾善考
Owner 河北威远药业有限公司
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