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Cycling treatment method for waste acid produced in production of hydroquinone

A hydroquinone and treatment method technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of high equipment requirements, low yield, high cost of raw materials, etc.

Inactive Publication Date: 2012-12-19
JIANGSU YANGNONG CHEM GROUP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The patent US3,862,247 applied by the U.S. Kopper company and the patent US4,270,010 applied by the Swiss Efim Biller company all adopt the high temperature and high pressure hydrolysis process of p-aminophenol to synthesize hydroquinone. The reaction conditions of this method are relatively harsh and the requirements for equipment are high. Raw material cost is relatively high
The patent application number of Yangnong Chemical Group is 200710163599.0 (authorized), which adopts the diazotization hydrolysis process of p-aminophenol, which comprehensively describes the whole process of production of hydroquinone, but it is not good for the enrichment of impurities, There is still room for further research on the influence of equipment and other factors on the application of base acid
[0008] In summary, there are problems such as serious environmental pollution, low yield or relatively harsh reaction conditions in the synthesis process of hydroquinone. Therefore, it is of great significance to develop a hydroquinone synthesis technology with less waste and higher yield great development prospects

Method used

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  • Cycling treatment method for waste acid produced in production of hydroquinone
  • Cycling treatment method for waste acid produced in production of hydroquinone
  • Cycling treatment method for waste acid produced in production of hydroquinone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A waste acid recycling treatment method of hydroquinone, the concrete process steps of the method are described as follows:

[0021] (1) Extraction of hydrolyzate

[0022] After the hydrolysis reaction is completed, the temperature is lowered to 45~60°C, with methyl isobutyl ketone as the continuous phase and the hydrolyzate as the dispersed phase, the methyl isobutyl ketone and 840kg of hydrolyzate are respectively pumped into the high level tank through the metering pump for tower Extraction method, methyl isobutyl ketone is fed from the bottom of the tower, the flow rate is 8L / hr, the flow rate of the hydrolyzed liquid is 60L / hr from the top of the tower, the extraction temperature is controlled at 20~30°C, the extracted water layer is 789kg, and the oil layer is extracted 80kg.

[0023] During the tower extraction process, the feed ratio is adjusted according to the central control situation, and the hydroquinone content in the raffinate water layer is controlled t...

Embodiment 2~4

[0031] With the operation steps and reaction conditions of embodiment 1, just change the adsorbent used in the decolorization and decoking process, the experimental data are shown in Table 1:

[0032] Table 1 Comparison of Experimental Results of Embodiment 1 and 2~4

[0033]

[0034] From the above results, it can be seen that activated carbon as an adsorbent has a better effect on decoking and decolorizing waste acid.

Embodiment 5~11

[0036] With the various operation steps and reaction conditions of embodiment 1, just change the specification of activated carbon used in the decoking and decolorization process, the experimental data are shown in Table 2:

[0037] Table 2 Comparison of Experimental Results of Embodiment 1 and 5-11

[0038]

[0039] When the specific surface area of ​​activated carbon is greater than 1200 m 2 / g. When the particle size is greater than 150 mesh, the decoking and decolorization effects of shell charcoal and wood charcoal are better.

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Abstract

The invention relates to a cycling treatment method for waste acid produced in production of hydroquinone. The method comprises the following steps: (1) an extraction reaction: a step of allowing temperature to drop to 40 to 60 DEG C after a hydrolysis reaction in the synthesis process of hydroquinone is finished and adding an extracting agent into hydrolysate for extraction; (2) steam stripping: a step of putting a water layer obtained after extraction into a stripping vessel and carrying out stirring and heating, wherein a final temperature of steam stripping is 110 to 112 DEG C and the content of the extracting agent in stripping acid after steam stripping is lower than 1 wt%; (3) decoking and decolouring: a step of adding 50 wt% of the stripping acid and an adsorbent into a decolouring kettle, carrying out decoking and decolouring at a temperature of 100 DEG C, putting a reaction solution into a filter press for filtering after a reaction is ended so as to obtain decoloured acid and the recovered adsorbent, and merging and standing the decoloured acid and rest stripping acid for a next hydrolysis reaction; and (4) washing and recovery: putting water into the filter press to cyclically wash the recovered adsorbent so as to recover hydroquinone adsorbed by the adsorbent, subjecting the adsorbent to regeneration treatment with a solvent and adding the treated adsorbent into step (3) for cyclic usage.

Description

technical field [0001] The invention relates to a method for preparing hydroquinone from p-aminophenol raw materials, which mainly studies and solves the problem of recycling waste sulfuric acid in the reaction process, and belongs to the field of fine chemicals. Background technique [0002] Hydroquinone (1,4-Benzendiol) is also known as hydroquinone (Hydroquinone), the chemical formula is C 6 h 6 o 2 , relative molecular weight 110.11, colorless or white crystal, melting point 170~171℃, boiling point 285~287℃, density 1.332g / cm 3 . Hydroquinone is widely used as an important raw material and intermediate for medicine, pesticide, dyestuff, rubber, etc. Antioxidants, at present, the use of hydroquinone is constantly expanding, and it also has certain application prospects in the fields of wastewater treatment, chemical fertilizers, food and cosmetics. [0003] There are many preparation methods of hydroquinone, currently there are mainly aniline redox method, bisphenol ...

Claims

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Application Information

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IPC IPC(8): C07C39/08C07C37/68C07C37/72C07C37/76C07C37/82
Inventor 袁源徐林丁克鸿顾志强汪洋戚明甫李明苑庆奎
Owner JIANGSU YANGNONG CHEM GROUP
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