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Method of recovering antioxidant 1024 intermediate

A technology for antioxidants and intermediates, which is applied in the field of recycling antioxidant 1024 intermediates, can solve the problems that antioxidant 1024 has a great influence on product purity, is prone to chemical reactions, and is difficult to recycle and reuse, so as to achieve resource recovery. The effect of reuse, easy separation and extraction, and convenient operation

Active Publication Date: 2019-09-27
JIANGSU JIYI NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] But in the prior art, the productive rate of β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionyl hydrazide is low, and it is not easy to separate, so that the raw material cost is high, the toxicity is difficult to reduce, and the practicability is also greatly reduced; at the same time In the production process, the purity of the antioxidant 1024 product is greatly affected, and the reaction waste liquid of the antioxidant 1024 contains excessive β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionyl hydrazide. There is no recycling process in the preparation process, and the reaction waste liquid contains a large amount of β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionyl hydrazide, which is difficult to recycle and reuse, forming solid-liquid waste. On the one hand, it causes environmental pollution, on the other hand, it causes waste of resources
[0007] At the same time, β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionyl hydrazide is susceptible to secondary pollution, and is prone to chemical reactions when in contact with the outside air, so it is necessary to select a more suitable method for its storage

Method used

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Embodiment 1

[0034] A method for reclaiming antioxidant 1024 intermediates, comprising the following steps:

[0035] S1, pretreatment: Pour 500kg of antioxidant 1024 reaction waste liquid into the reactor, which is fixed with a thermometer, a reflux condenser, a feeder and an inert gas protection device, and is carried out by using a stirring device in the reactor. Mechanical stirring, so that the reaction waste liquid mixed evenly;

[0036] S2. Primary solid-liquid separation: add 62.5kg of anhydrous sodium sulfate into the reactor through the feeder on the reactor, and after fully stirring through the stirring device, cool down until crystals are precipitated, and then continue to cool down to 0°C to wait for crystals After complete precipitation, the reaction waste liquid is transported to a centrifuge for centrifugation to obtain sodium sulfate decahydrate and reaction waste liquid I;

[0037] S3, a vacuum distillation: transfer the reaction waste liquid I obtained in the above steps ...

Embodiment 2

[0043] A method for reclaiming antioxidant 1024 intermediates, comprising the following steps:

[0044] S1, pretreatment: Pour 500kg of antioxidant 1024 reaction waste liquid into the reactor, which is fixed with a thermometer, a reflux condenser, a feeder and an inert gas protection device, and is carried out by using a stirring device in the reactor. Mechanical stirring, so that the reaction waste liquid mixed evenly;

[0045] S2. Primary solid-liquid separation: Add 78.8kg of anhydrous sodium sulfate into the reactor through the feeder on the reactor, and after fully stirring through the stirring device, cool down until crystals are precipitated, and then continue to cool down to 0°C to wait for crystals After complete precipitation, the reaction waste liquid is transported to a centrifuge for centrifugation to obtain sodium sulfate decahydrate and reaction waste liquid I;

[0046] S3, a vacuum distillation: transfer the reaction waste liquid I obtained in the above steps ...

Embodiment 3

[0052] A method for reclaiming antioxidant 1024 intermediates, comprising the following steps:

[0053] S1, pretreatment: Pour 500kg of antioxidant 1024 reaction waste liquid into the reactor, which is fixed with a thermometer, a reflux condenser, a feeder and an inert gas protection device, and is carried out by using a stirring device in the reactor. Mechanical stirring, so that the reaction waste liquid mixed evenly;

[0054] S2. Primary solid-liquid separation: Add 85.3kg of anhydrous sodium sulfate into the reactor through the feeder on the reactor, and after fully stirring through the stirring device, cool down until crystals are precipitated, and then continue to cool down to 0°C to wait for crystals After complete precipitation, the reaction waste liquid is transported to a centrifuge for centrifugation to obtain sodium sulfate decahydrate and reaction waste liquid I;

[0055] S3, a vacuum distillation: transfer the reaction waste liquid I obtained in the above steps ...

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Abstract

The invention discloses a method of recovering an antioxidant 1024 intermediate, and relates to the technical field of organic chemistry. The method includes the following steps: pre-treatment on antioxidant 1024 reaction waste liquid, first solid-liquid separation, first vacuum distillation, secondary solid-liquid separation, secondary vacuum distillation, crystallization, collection and packaging. When the method disclosed by the invention is used to fully recover and utilize by-products in the antioxidant 1024 reaction waste liquid, toxin of products is reduced, the production is energy-conserving and environmentally friendly, and pollution to the environment is avoided. The technique is easy and convenient for operation, separation and extraction, and storage. Secondary pollution is effectively avoided. The antioxidant 1024 intermediate is fully recovered. Resourceful utilization is realized. Raw material cost of the antioxidant 1024 is greatly reduced. Large-scale industrialized production of the antioxidant 1024 is possible.

Description

technical field [0001] The invention relates to the technical field of organic chemical industry, in particular to a method for recovering an antioxidant 1024 intermediate. Background technique [0002] Antioxidant 1024 is a high-efficiency and non-polluting antioxidant with excellent performance. It is soluble in methanol and acetone, slightly soluble in chloroform and ethyl acetate, insoluble in water, and has a dual structure of hindered phenol and hydrazide. Oxidation and metal deactivation functions. As a metal deactivator, it will not produce color stains, it can be used alone or in combination with other general antioxidants, and has excellent synergistic effect. It is suitable for polyethylene, polypropylene, polystyrene, polyamide, polyester, especially suitable for antioxidant of phenolic resin, which can effectively prevent the polymer from autoxidation caused by the presence of transition metal ions (such as catalyst residues). [0003] In the process of prepar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C241/04C07C243/32
CPCC07C241/04C07C243/32
Inventor 郭骄阳赵崇鑫
Owner JIANGSU JIYI NEW MATERIAL CO LTD
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