Method and equipment for continuously extracting p-benzoquinone from aniline-oxidized oxidized material

A technology for p-benzoquinone and oxidizing materials, applied in chemical instruments and methods, solvent extraction, separation methods, etc., can solve the problems of reduced yield, high equipment requirements, and easy decomposition of benzoquinone, etc., with simple methods and simple equipment Effect

Active Publication Date: 2014-04-23
湖北普瑞提化工科技有限公司
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] P-benzoquinone is an important intermediate in organic synthesis. The traditional method of extracting p-benzoquinone from the oxidation material oxidized by aniline by high-temperature water vapor is the traditional method for extracting p-benzoquinone, especially the extraction of p-benzoquinone from the oxidation material by high-temperature water vapor has the following obvious deficiencies: 1. High steam temperature (100-120°C), benzoquinone is easy to decompose, increasing material loss and reducing product yield
2. High equipment requirements and large wear and tear
3. The temperature of p-benzoquinone aqueous solution is high, it is easy to coke, and the yield decreases

Method used

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  • Method and equipment for continuously extracting p-benzoquinone from aniline-oxidized oxidized material

Examples

Experimental program
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Effect test

Embodiment 1

[0011] Example 1. Take 500ml of oxidizing material with a benzoquinone content of 5%, put it into a 1000ml separatory funnel, add 250ml of methyl isobutyl ketone, mix evenly for 3 minutes, pour the mixed solution into a filter and filter , to separate the manganese mud from the liquid. Put the filtrate into the separatory funnel and let it stand for 5 minutes, release the lower layer as benzoquinone aqueous solution, repeat the extraction 8 times, add the extraction dose according to 200ml, 150ml, 150ml, 100ml, 100ml, and ensure that the concentration of the extract phase in the first extraction tower reaches 5 %, extracted until the benzoquinone content (mass fraction) in the aqueous solution is lower than 0.03%. The upper layer is p-benzoquinone solution, collected for use. The manganese mud is stirred and washed with 30ml~50ml of solvent each time, and the filtered liquid is used as the extractant of the above filtrate.

[0012] Product yield: p-benzoquinone yield ≥ 98%. ...

Embodiment 2

[0013] Embodiment 2, get benzoquinone content and be 3% oxidation material 1000ml, insert in the 2000ml separatory funnel, then add the butyl acetate of 800ml, mix evenly, time 3 minutes, the mixed solution is poured in filter and filtered, makes manganese The mud is separated from the liquid. Put the filtrate into the separatory funnel and let it stand for 5 minutes, release the lower layer as benzoquinone aqueous solution, repeat the extraction 6 times, add the extraction dose according to 600ml, 400ml, 400ml, 200ml, 200ml, and ensure that the concentration of the extract phase in the first extraction tower reaches 18 %, extracted until the benzoquinone content (mass fraction) in the aqueous solution is lower than 0.03%. The upper layer is p-benzoquinone solution, collected for use. The manganese mud is stirred and washed with 30ml~50ml of solvent each time, and the filtered liquid is used as the extractant of the above filtrate.

[0014] Product yield: p-benzoquinone yiel...

Embodiment 3

[0016] Add 650L of oxidizing material water suspension with a p-benzoquinone content of 4% (mass percentage) into the high-speed continuous mixer, add 280L of sec-butyl acetate, stir and mix for 15 minutes, and the mixed liquid enters the solid-liquid separator , to separate the solid manganese mud from the liquid. The liquid is injected from the upper part of the extraction tower 1, and the extraction phase and the raffinate phase are fully separated as the liquid falls. The extraction phase is poured into countercurrent contact at 5 places, and the p-benzoquinone is extracted from the raffinate phase to obtain a new extract phase. The phase falls and contacts with the extraction phase injected from the bottom 1 / 5 of the extraction tower 3 in countercurrent, and the p-benzoquinone is extracted from the raffinate phase to obtain a new extraction phase. The extraction phase rises and enters the extraction tower 1 after coming out from the top of the extraction tower 2 The lowe...

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Abstract

The invention provides a method for obtaining high-concentration p-benzoquinone from an aniline-oxidized oxidized material by adopting multi-stage circulation continuous extraction. The method comprises the steps of adding a water suspension of the aniline-oxidized oxidized material containing 3-10% of p-benzoquinone into a high-speed continuous mixing machine, adding n-butyl acetate and sec-butyl acetate as well as isomer series, methyl isobutyl ketone and acetic ether according to a volume ratio of the oxidized material to an extracting agent of 10:(4-5), mixing with stirring for 10-15 minutes, delivering a mixed solution containing inorganic salts including a p-benzoquinone solute, the extracting agent, manganese mud, manganese sulfate, ammonium sulfate and the like into a solid-liquid separator to ensure that solid manganese mud is separated from liquid. The liquid enters a multi-stage reverse flow continuous extraction system, and the solid manganese mud enters a solvent recovery system. The technical scheme disclosed by the invention does not need water vapor high-temperature extraction to cause decomposition of benzoquinone, so that the yield of p-benzoquinone is influenced, the yield of the p-benzoquinone can be influenced. The yield of the p-benzoquinone in the invention reaches more than 98%, an extraction reagent is easily available, and the method and equipment are simple.

Description

technical field [0001] The invention relates to a method for continuously extracting p-benzoquinone from an oxidized material oxidized by aniline, which specifically adopts multi-stage circulation continuous extraction to obtain high-concentration p-benzoquinone, and belongs to the field of fine chemical industry. Background technique [0002] P-benzoquinone is an important intermediate in organic synthesis. The traditional method of extracting p-benzoquinone from the oxidation material oxidized by aniline by high-temperature water vapor is the traditional method for extracting p-benzoquinone, especially the extraction of p-benzoquinone from the oxidation material by high-temperature water vapor has the following obvious deficiencies: 1. High steam temperature (100-120°C), benzoquinone is easy to decompose, increasing material loss and reducing product yield. 2. The equipment has high requirements and wears a lot. 3. The temperature of p-benzoquinone aqueous solution is hig...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C50/04C07C46/10B01D11/04
CPCB01D11/0426C07C46/10C07C50/04
Inventor 高士敬
Owner 湖北普瑞提化工科技有限公司
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