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Method for preparing adipic acid and C4-6-dibasic acid from cyclohexane oxidation reaction byproduct

An oxidation reaction and cyclohexane technology, applied in chemical instruments and methods, preparation of organic compounds, separation/purification of carboxylic acid compounds, etc., can solve the problem of low added value of recovered products, low recovery rate of by-products, and increased production costs and other issues, to save energy consumption, easy operation, and reduce emissions

Active Publication Date: 2015-01-14
CHONGQING HUAFON CHEM +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The treatment process of this patent not only has high cost and high discharge of three wastes, but also has a low recovery rate of by-products (such as other non-acidic organic by-products generated in the oxidation process of cyclohexane are not recovered), and the product (mixed organic acid ester) is recovered at the same time low added value
[0007] Patent CN1184802A (1998) introduces a kind of method for preparing diacid from similar hexanaphthene oxidation product washing acid water, proposes to adopt the method for catalytic hydrogenation, evaporative concentration, nitric acid oxidation to process washing acid water, and there are obvious deficiencies in the treatment process: (1 ) The catalytic hydrogenation process uses noble metals such as Pd and other catalysts, and the operating pressure is high, which increases the production cost; (2) the existing carbonyl compounds in the original acid wastewater are reduced to alcohol compounds after catalytic hydrogenation, so when using When nitric acid is oxidized, increase the amount of nitric acid
Since the process parameters of cyclohexane oxygen-lean oxidation process and cyclohexane air oxidation process are different, and the oxygen content of oxidant is different, the types and amounts of by-products produced are different. Therefore, the recovery and utilization of by-products produced in cyclohexane air oxidation process , especially to convert it to adipic acid and C 4～6 -Dibasic acid, improving the two-step oxidation of cyclohexane to produce adipic acid and C 4～6 -The method of dibasic acid yield has no patents and literature reports

Method used

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  • Method for preparing adipic acid and C4-6-dibasic acid from cyclohexane oxidation reaction byproduct
  • Method for preparing adipic acid and C4-6-dibasic acid from cyclohexane oxidation reaction byproduct
  • Method for preparing adipic acid and C4-6-dibasic acid from cyclohexane oxidation reaction byproduct

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Embodiment 1

[0040] Embodiment 1 adopts the inventive method to produce adipic acid and C 4～6 -a

[0041] Get 80kg hexanaphthene air oxidation liquid from hexanaphthene air oxidation device, wash with deionized water according to oil / water ratio of 100 in extraction tower, the washing aqueous solution that obtains uses fresh hexanaphthene according to oil / water ratio 3. Carry out backwashing to obtain 1.26 kg of washing aqueous solution altogether, wherein the organic matter content is 20.6% (weight), the washing temperature is 70° C., and the operating pressure is normal pressure. The obtained washing water is evaporated and concentrated under normal pressure, and the distilled light component weight is 60%, and the concentrated solution obtained is divided into 2 parts:

[0042] (1) 1 part was oxidized with nitric acid with a content of 60%, and the reaction temperature was gradiently raised: 55±5°C, 65±5°C, 75±5°C, 85±5°C, the total reaction time was 3h, and the amount of nitric acid w...

Embodiment 2

[0044] Embodiment 2 adopts the inventive method to produce adipic acid and C 4～6 -a

[0045] Get 85kg hexanaphthene air oxidation liquid from hexanaphthene air oxidation device, wash with deionized water according to oil / water ratio of 110 in the extraction tower, the washing aqueous solution that obtains uses fresh hexanaphthene according to oil / water ratio 4. Carry out back washing to obtain 1.28kg of aqueous washing solution altogether, wherein the organic matter content is 21.8% (weight), the washing temperature is 65° C., and the operating pressure is normal pressure. The obtained washing water is subjected to atmospheric pressure evaporation and concentration, and the distilled light component weight is 58%, and the concentrated solution obtained is divided into 2 parts:

[0046](1) 1 part was oxidized with nitric acid with a content of 60%, the reaction temperature was raised by gradient: 60±5°C, 70±5°C, 80±5°C, 90±5°C, the total reaction time was 4h, and the amount of...

Embodiment 3

[0048] Embodiment 3 adopts the inventive method to produce adipic acid and C 4～6 -a

[0049] Get 75kg hexanaphthene air oxidation liquid from hexanaphthene air oxidation device, wash with deionized water according to the oil / water ratio of 95 in the extraction tower, the washing aqueous solution that obtains uses fresh hexanaphthene according to oil / water ratio 4. Perform backwashing to obtain a total of 1.209 kg of aqueous washing solution, wherein the organic matter content is 18.5 wt%, the washing temperature is 65° C., and the operating pressure is normal pressure. The obtained washing water is subjected to atmospheric pressure evaporation and concentration, and the distilled light component weight is 62%, and the concentrated solution obtained is divided into 2 parts:

[0050] (1) 1 part was oxidized with nitric acid with a content of 65%, and the reaction temperature was raised by gradient: 60±5°C, 70±5°C, 80±5°C, 90±5°C, the total reaction time was 4h, and the amount o...

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Abstract

The invention belongs to the technical field of organic synthesis and particularly relates to a method for preparing adipic acid and C4-6-dibasic acid from a cyclohexane oxidation reaction byproduct, aiming at solving the technical problem that the method for preparing adipic acid and C4-6-dibasic acid from the cyclohexane oxidation reaction byproduct can be used for preparing adipic acid and C4-6-dibasic acid by taking the cyclohexane oxidation reaction byproduct as a raw material. The technical scheme is as follows: the method for preparing adipic acid and C4-6-dibasic acid from the cyclohexane oxidation reaction byproduct comprises the following steps of a, separating the byproduct contained in cyclohexane oxidation reaction liquid; b, transforming the byproduct into adipic acid and C4-6-dibasic acid; c, separating and recovering adipic acid and C4-6-dibasic acid. The method disclosed by the invention can be used for separating the byproduct generated in the process of a cyclohexane air oxidation-alkaline saponification decomposition process and successfully transforming into important chemical products, namely adipic acid and C4-6-dibasic acid and achieves the effects of reducing consumption, reducing emission, sufficiently utilizing resources and changing wastes into valuables.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to the preparation of adipic acid and C 4～6 - Dibasic acid method. Background technique [0002] Adipic acid is an important aliphatic dibasic acid, an important chemical raw material and intermediate, mainly used in the manufacture of nylon-66, polyurethane, plasticizers, lubricants, pesticides and adhesives. [0003] C 4～6 -Dibasic acid refers to a mixed dibasic acid composed of succinic acid, glutaric acid and adipic acid, also known as nylon acid, which is also an important chemical raw material and can be used as a raw material for the production of various polyurethane foams; if C 9 ~C 10 Esterification of mixed dibasic acid by primary alcohol can obtain high-quality softener, which can be used in polyvinyl chloride to make it have excellent cold impact resistance; esterification with methanol can obtain mixed dibasic acid dimethyl ester (DBE) as a coa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/27C07C55/14C07C55/02C07C55/12C07C55/10
CPCC07C51/27C07C51/43C07C55/14C07C55/10C07C55/12C07C55/02
Inventor 唐丽华陈恩之张晓娟陈旭沈国良唐劲松姜曦王艳辉赵风轩张羿新贾长英苗迎彬谢毅丁亮亮王兆东
Owner CHONGQING HUAFON CHEM
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