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A method for high-purity synthesis of anthraquinone and co-production of magnesium sulfate

A technology of magnesium sulfate and anthraquinone, which is applied in the field of high-purity synthetic anthraquinone co-production of magnesium sulfate, can solve the problems that enterprises cannot bear the cost of neutralization, increase the difficulty and cost of waste acid treatment, and pollute, so as to improve the application value and facilitate the production of magnesium sulfate. The effects of popularizing applications and easy process control

Active Publication Date: 2022-06-21
山东昌邑海能化学有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the disposal methods of this wastewater mainly include: (1) direct discharge into ditches or rivers, causing serious pollution problems; (2) neutralization with liquid caustic soda to recover salt, because the quality of salt is not high and the price is low, As a result, enterprises cannot bear the cost of neutralization; (3) Concentrate and recycle dilute sulfuric acid, and use it again for anthraquinone production
Although this method is simple, due to the strong corrosiveness of sulfuric acid, a large amount of acid mist will be generated during the concentration process, which greatly increases the difficulty and cost of waste acid treatment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The concrete steps of synthesizing anthraquinone co-producing magnesium sulfate in the present embodiment are as follows:

[0030] (1) Acylation reaction: Mix 400 parts by mass of phthalic anhydride, 300 parts by mass of benzene and 800 parts by mass of aluminum trichloride, react at 50°C for 2 hours to obtain a mixture, add 4200 parts by mass of the mixture to the mass percentage concentration of Acidizing and hydrolyzing in 7% sulfuric acid solution, the temperature of acidizing and hydrolyzing should not exceed 75℃;

[0031] (2) Separation: Add benzene at 60°C to the mixture obtained by acidification and hydrolysis in step (1), and the volume ratio of benzene to the mixture is 2:1. After constant stirring, the mixture is allowed to stand for 20 minutes, and then the benzene and o-benzol in the upper layer are separated. The first mixed solution of acyl benzoic acid, inject water in the first mixed solution, the volume ratio of water and the first mixed solution is 0....

Embodiment 2

[0042] The difference between this embodiment and the first embodiment is:

[0043] In step (1), 450 parts by mass of phthalic anhydride, 250 parts by mass of benzene and 850 parts by mass of aluminum trichloride were mixed, and the mixture was reacted at 70 ° C for 0.5 hours to obtain a mixture, and 4800 parts by mass of the mixture was added to the mass percentage concentration of 5 % sulfuric acid solution for acidification and hydrolysis;

[0044]In step (2), benzene at 40° C. is added to the mixture, and the volume ratio of benzene to the mixture is 3:1. After constant stirring, the first mixture of benzene and o-benzoyl benzoic acid in the upper layer is separated after standing for 10 minutes. Liquid, inject water in the first mixed solution, the volume ratio of water and the first mixed solution is 1.2:1, after stirring again, stand for 8 minutes and separate out the second mixed solution of benzene and o-benzoyl benzoic acid in the upper strata , then the second mixe...

Embodiment 3

[0049] The difference between this embodiment and the first embodiment is:

[0050] In step (1), 425 parts by mass of phthalic anhydride, 275 parts by mass of benzene and 825 parts by mass of aluminum trichloride are mixed, and the mixture is reacted at 60 ° C for 1.5 hours to obtain a mixture, and 4500 parts by mass of the mixture is added to the mass percentage concentration of 6 Acidification and hydrolysis in % sulfuric acid solution;

[0051] In step (2), benzene at 50° C. is added to the mixture, the volume ratio of benzene to the mixture is 2.5:1, and the mixture is kept for 15 minutes after constant stirring to separate the first mixture of benzene and o-benzoylbenzoic acid in the upper layer. Liquid, inject water in the first mixed solution, the volume ratio of water and the first mixed solution is 1:1, after stirring again, stand for 10 minutes and separate out the second mixed solution of benzene and o-benzoyl benzoic acid in the upper strata , then the second mixe...

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PUM

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Abstract

The invention discloses a high-purity method for synthesizing anthraquinone and co-producing magnesium sulfate, which belongs to the technical field of organic chemistry. It is prepared through eight processes of acylation reaction, separation, ring closure, filtration, neutralization reaction, filtration, adsorption and crystallization. Purity Anthraquinone and Magnesium Sulfate. This process uses benzene and water to wash and separate the o-benzoylbenzoic acid obtained by acidification and hydrolysis twice to reduce the content of inorganic salts, improve the purity of o-benzoylbenzoic acid entering the dehydration ring-closing reaction, and reduce impurities at the same time The impact on the ring-closing reaction enables the o-benzoylbenzoic acid to fully close the ring, increase the yield and purity of anthraquinone, and remove the impurities in the waste acid water through filtration, suspension degreasing and adsorption processes to obtain Magnesium sulfate with high quality and higher application value realizes the ideal recycling of waste acid water.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry, and in particular relates to a method for high-purity synthesis of anthraquinone to co-produce magnesium sulfate. Background technique [0002] Anthraquinone is an important chemical intermediate, which is widely used in the fields of dyes, medicine and pesticides. Using anthraquinone as raw material, through sulfonation, nitration, etc., dye intermediates with a wide range of applications are obtained, which are used to produce anthraquinone-based disperse dyes, acid dyes, reactive dyes and vat dyes, etc., and occupy a very important role in the field of synthetic dyes. status. Anthraquinone is also widely used as a pulping cooking agent in papermaking, the production of high-concentration hydrogen peroxide, and in the fertilizer industry for the manufacture of sodium anthraquinone disulfonate, a desulfurizer. [0003] The production of synthetic anthraquinone mainly includes phthali...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C50/18C07C46/10C07C46/00C01F5/40
Inventor 童金亭蒲国心蒲伟于强强
Owner 山东昌邑海能化学有限责任公司