Method for using carvone production wastewater for recycling acetone oxime

A technology for producing waste water and acetone oxime, which is applied in oxime preparation, organic chemistry, etc., can solve the problems of difficult biochemical degradation, acetone oxime energy consumption, large equipment investment, complex components, etc., and achieve the effect of strong extraction capacity

Active Publication Date: 2009-07-08
HUAIAN WAN BANG SPICE IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The general treatment method is to directly use biochemical methods, but the disadvantage is that the components in the wastewater are very complex and contain a large amount of acetone oxime, and acetone oxime has a great inhibitory effect on the growth of most of the bacteria treated by biochemical treatment, so it is difficult to Biochemical degradation, acetone oxime must be recovered before biochemical treatment, the traditional distillatio

Method used

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  • Method for using carvone production wastewater for recycling acetone oxime

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Put 165 grams of 120-150°C / 2mmHg back fraction during rectification in the production process of carvone and 600 grams of waste water with a mass concentration of 19.5% acetone oxime into a 1000ml three-necked flask, heat up to 45°C, stir for 37min, and cool to room temperature. Transfer to a 1000ml separating funnel, let it stand for stratification, determine that the water phase contains 1.3% acetone oxime, and transfer it to the sewage station for treatment; the organic phase is rectified under reduced pressure, collect 105 grams of fractions at 80-85°C / 300mmHg, and analyze the acetone oxime by chromatography The content is 99.2%; 105 grams of acetone oxime fractions are dissolved in 70 grams of water, and a large amount of crystals are precipitated when the temperature is slowly lowered to 5°C. The crystallization solution is centrifuged, the mother liquor is recycled, and the solids are vacuum-dried to obtain 100 grams of acetone oxime product, which is analyzed by G...

Embodiment 2

[0019] Put 160 grams of 120-150°C / 2mmHg rear fraction during rectification in the production process of carvone and 550 grams of waste water with a mass concentration of 18.3% acetone oxime into a 1000ml three-necked flask, heat up to 50°C, stir for 45min, and cool to room temperature. Transfer to a 1000ml separatory funnel, let it stand for stratification, determine that the water phase contains 1.1% acetone oxime, and transfer it to the sewage station for treatment; the organic phase is rectified under reduced pressure, collect 90 grams of fractions at 80-85°C / 300mmHg, and analyze the acetone oxime by chromatography The content is 99.3%; 90 grams of acetone oxime fractions are dissolved in 60 grams of water, and the temperature is slowly cooled to 4° C. A large amount of crystals are precipitated. The crystallization solution is centrifuged, the mother liquor is recycled, and the solids are vacuum-dried to obtain 86 grams of acetone oxime product, which is analyzed by GC The ...

Embodiment 3

[0021] Put 175 grams of 120-150°C / 2mmHg back fraction and 655 grams of waste water with a mass concentration of 17.5% acetone oxime into a 1000ml three-neck flask during the rectification in the production process of carvone, heat up to 40°C, stir for 30min, and cool to room temperature. Transfer to a 1000ml separatory funnel, let it stand for stratification, determine that the water phase contains 1.0% acetone oxime, and transfer it to the sewage station for treatment; the organic phase is rectified under reduced pressure, collect 100 grams of 80-85°C / 300mmHg fraction, and analyze the acetone oxime by chromatography The content is 99.1%; 100 g of acetone oxime fraction is dissolved in 65 g of water, and the temperature is slowly cooled to 3° C., a large amount of crystals are precipitated. The crystallization liquid is centrifuged, the mother liquor is recycled, and the solid is vacuum-dried to obtain 94 g of acetone oxime product, which is analyzed by GC The content is 99.7%....

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Abstract

The invention discloses a method for reclaiming acetone oxime from carvone production wastewater. The method comprises the following steps: firstly, reclaiming of an extractant, namely collecting 120-150 DEG C/2mmHg after-cut under the condition of rectification during carvone production as the extractant, wherein the mass content of the carvone is less than 0.5 percent; secondly, extraction of the wastewater, namely mixing the wastewater containing the acetone oxime and the extractant according to the weight ratio of 3.4-3.8:1, raising the temperature to be between 40 and 50 DEG C, stirring for 30 to 45 minutes, cooling the mixture to the room temperature, performing standing and delamination, re-extracting a water phase until reaching the standards, introducing the water phase into a wastewater purification treatment system, and reclaiming the acetone oxime from an organic phase, wherein the mass content of the acetone oxime in the water phase is less than 1.5 percent; thirdly, rectification, namely performing vacuum rectification on the organic phase, and collecting 80-85 DEG C/300mmHg acetone oxime cut fractions; and fourthly, recrystallization, namely dissolving the acetone oxime cut fractions into water according to the mass ratio of 1.5:1, reducing the temperature to be between 3 and 5 DEG C for crystallization and centrifugal separation, recycling a mother liquor, drying solid under vacuum and obtaining the acetone oxime. The method has simple technique, is convenient to operate and easy in industrial implementation, and changes the prior mode of no products after environment-friendly investment, and has high economic efficiency and social efficiency.

Description

technical field [0001] The invention relates to a method for treating waste water of spice compounds and recovering by-products, in particular to a method for recovering acetone oxime from carvone production waste water. Background technique [0002] Carvone production wastewater is a typical high-concentration organic wastewater, which has the characteristics of high concentration of organic matter, high chroma, difficult biochemical degradation, and complex components. [0003] The general treatment method is to directly use biochemical methods, but the disadvantage is that the components in the wastewater are very complex and contain a large amount of acetone oxime, and acetone oxime has a great inhibitory effect on the growth of most of the bacteria treated by biochemical treatment, so it is difficult to Biochemical degradation, acetone oxime must be recovered before biochemical treatment, the traditional distillation recovery of acetone oxime consumes a lot of energy an...

Claims

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Application Information

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IPC IPC(8): C07C251/38C07C249/14
Inventor 林祥陈文昌陈兆刚许竹青
Owner HUAIAN WAN BANG SPICE IND CO LTD
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