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Method for recovering antioxidant 300 from efficient solvent oil mother liquor

A recovery method and solvent oil technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of slow crystallization of antioxidant 300, accidents, and difficult centrifugation, etc. Reduced risk and short centrifugation time

Inactive Publication Date: 2020-09-15
淄博万科化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The recovery effect of this method is relatively poor, and only about 20% to 30% of antioxidants can be recovered.
At the same time, because the feed liquid after distillation is very viscous at normal temperature, the crystallization of antioxidant 300 is slow, which takes 3-4 days, and it is very difficult to centrifuge, and the centrifugation time is very long, which takes 5-6 hours
In addition, solvent oil is a flammable and explosive dangerous product, and the centrifuge is a high-speed operation equipment, and the possibility of accidents increases during long-term operation

Method used

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  • Method for recovering antioxidant 300 from efficient solvent oil mother liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Distill and concentrate the 200# solvent oil mother liquor containing antioxidant 300 under reduced pressure (-0.08±0.01MPa) at a temperature of 135±5°C, and distill out 200# solvent oil with 30% of the total volume of the mother liquor; put the concentrated solution into recovery Kettle, start stirring (35±5Hz), recover the jacket of the kettle and slowly feed chilled water, stir until the temperature of the concentrated solution is 65±5°C; add n-hexane with 10% volume of the concentrated solution, continue stirring (25±5Hz) to cool down to Stir at -10°C (25±5Hz) for 2 hours; stop stirring, let stand for 12 hours to continue crystallization; then start stirring (50Hz), open the discharge valve of the recovery kettle, put it into a centrifuge for centrifugation (20 minutes), and discharge.

[0027] The obtained antioxidant 300 is white crystal, loose, and its measured melting point is 160.3°C (contains few other by-products). After one purification and weighing, the reco...

Embodiment 2

[0029] Distill and concentrate the 200# solvent oil mother liquor containing antioxidant 300 under reduced pressure (-0.07±0.01MPa) at a temperature of 135±5°C, and distill out 200# solvent oil containing 50% of the total volume of the mother liquor; put the concentrate into recycling Kettle, start stirring (30-40Hz), recover the jacket of the kettle and slowly feed frozen water, stir until the temperature of the concentrated solution is 60±5°C; add n-hexane with 10% volume of the concentrated solution, continue stirring (25±5Hz) to cool down to Stir at -10°C (25±5Hz) for 3h; stop stirring, let stand for 12h to continue crystallization; then start stirring (50Hz), open the discharge valve of the recovery kettle, put it into a centrifuge for centrifugation (20 minutes), and discharge.

[0030] The obtained antioxidant 300 is white crystal, loose, and its measured melting point is 159.9° C. (contains few other by-products). After 2 times of purification and weighing, the recovery...

Embodiment 3

[0032] Distill and concentrate the 200# solvent oil mother liquor containing antioxidant 300 under reduced pressure (-0.07±0.01MPa) at a temperature of 135±5°C, and distill out 200# solvent oil containing 60% of the total volume of the mother liquor; put the concentrated solution into recovery Kettle, start stirring (30-40Hz), recover the jacket of the kettle and slowly feed frozen water, stir until the temperature of the concentrated solution is 70±5°C; add n-hexane with 10% volume of the concentrated solution, continue stirring (25±5Hz) to cool down to Stir at -10°C (25±5Hz) for 2 hours; stop stirring, let stand for 12 hours to continue crystallization; then start stirring (50Hz), open the discharge valve of the recovery kettle, put it into a centrifuge for centrifugation (20 minutes), and discharge.

[0033] The obtained antioxidant 300 is white crystal, loose, and its measured melting point is 159.7°C (contains few other by-products). After one purification and weighing, th...

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Abstract

The invention belongs to the technical field of chemical engineering, and particularly relates to a method for recovering an antioxidant 300 in efficient solvent oil mother liquor. The recovery methodof the antioxidant 300 in the efficient solvent oil mother liquor comprises the following steps of: (1) mother liquor concentration: carrying out reduced pressure distillation and concentration on the mother liquor containing the antioxidant 300 to evaporate No.200 solvent oil of which the volume is 30-60% of the total volume of the mother liquor; (2) cooling of the concentrated solution: introducing chilled water into a jacket of a recovery kettle, putting the concentrated solution with the temperature of 130-140 DEG C into the recovery kettle, and stirring until the temperature of the concentrated solution is 50-80 DEG C; (3) crystallization: adding n-hexane accounting for 10%-20% of the volume of the concentrated solution into the recovery kettle, continuously stirring until the temperature is -10 DEG C to -5 DEG C, and then stirring for 2-3 hours; and (4) standing and centrifuging: stopping stirring, standing, and then centrifuging to obtain the antioxidant 300. The method is short in crystallization time, high in recovery efficiency, low in centrifugal difficulty and high in operation safety.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for recovering antioxidant 300 in high-efficiency solvent oil mother liquor. Background technique [0002] Antioxidant 300 is a thiobisphenol antioxidant with excellent performance. It is a high-efficiency primary antioxidant for rubber, polyolefin, plastic and other products, especially for polyethylene cable and wire materials. The antioxidant effect is particularly outstanding . [0003] The solvent oil used in the refining and purification of antioxidant 300 contains more and more antioxidant by-products during recycling, and at the same time, about 5% to 8% of antioxidant 300 is dissolved, which needs to be recovered when the solvent oil is reused. Part of the antioxidant 300. [0004] The general recovery method now is to distill part of the solvent oil from the solvent oil mother liquor, put the remaining part of the feed liquid into a stor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/28C07C323/20
CPCC07C319/28C07C323/20
Inventor 张胜传崔华松于海宝李雪松
Owner 淄博万科化工有限公司
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