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Clean production technique of 1,4-dihydroxy anthraquinone

A dihydroxyanthraquinone, clean production technology, applied in quinone preparation, quinone separation/purification, preparation of organic compounds, etc., can solve the problems of low reaction activity, low reaction yield, increased yield of side reactions, etc. The effect of production cost, elimination of pollution and resource saving

Inactive Publication Date: 2015-04-29
ZHEJIANG RUNTU INST
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  • Abstract
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Problems solved by technology

Although this method adopts recovered phthalic acid as raw material to directly synthesize 1,4-dihydroxyanthraquinone, however, due to the reactivity of phthalic acid is much lower than that of phthalic anhydride, and hydroquinone is relatively weak in concentrated sulfuric acid medium. It is easy to be oxidized, resulting in a very low reaction yield, only 67.7%. There are a large number of raw materials that are not completely reacted and the conversion rate of raw materials cannot be improved by increasing the reaction temperature, otherwise it will lead to an increase in side reactions and a lower yield. Afterwards, the phthalic acid contained in the wastewater cannot be recovered and used again (that is to say, the phthalic acid used can only come from the process of phthalic anhydride, and the process of its own process has not been realized), and there is a big problem in wastewater treatment. problem, so it has not been able to be applied in industry

Method used

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  • Clean production technique of 1,4-dihydroxy anthraquinone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add 215g of 20% oleum, 26g of boric acid and 67.8g of phthalic acid in the 500ml four-neck flask equipped with a condensation recovery device, heat up to 160°C and dehydrate for 2 hours (this process is mainly for boric acid to dehydrate to generate pyroboric acid and Metaboric acid, no phthalic anhydride was found in the sampling analysis), then 37.5g of p-chlorophenol was added dropwise, after the drop was completed, the temperature was raised to 195°C-200°C and the temperature was maintained for 6 hours. Cool down and wait for dilution.

[0041] Add 860g of hot water into a 2000ml beaker, put in the material to be diluted, and then keep it at 100°C-105°C for 4 hours for hydrolysis. Filter, collect mother liquor 1100g, CODcr content is 30000mg / L, sulfuric acid mass percentage concentration is 20.5%. The filter cake is washed with hot water, and the washing water is collected as the bottom water for the next batch of dilution. The filter cake is dried to obtain 1,4-d...

Embodiment 2

[0045] Add niacin 215g and boric acid 26g in a 500ml four-neck flask equipped with a condensation recovery device, and recycle 15g of phthalic acid in Example 1, add 57g of phthalic acid newly, heat up to 150°C for dehydration for 2 hours, add dropwise Chlorophenol 37.5g, after dripping, the temperature was raised to 195°C-200°C and the temperature was kept for 6 hours. Cool down and wait for dilution.

[0046] Add 1000 g of the washing water of Example 1 into a 2000 ml beaker, put in the material to be diluted, and then heat-preserve and hydrolyze at 100° C. to 105° C. for 4 hours. Filter, collect mother liquor 1220g, CODcr content is 36000mg / L, and sulfuric acid acidity is 19.8%. The filter cake is washed with hot water, and the washing water is collected as the bottom water for the next batch of dilution. The filter cake is dried to obtain 1,4-dihydroxyanthraquinone with a content of 97.8% and a yield of 90.6%.

[0047] Put the mother liquor into a 2000ml beaker, cool do...

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Abstract

The invention discloses a clean production technique of 1,4-dihydroxy anthraquinone, which comprises the following steps: phthalic acid is used as a raw material, synthesis technique washing water is directly used as diluting hydrolysis bottom water for the next batch, a mother solution wastewater is cooled, crystallized, separated and subjected to resin adsorption to recover sulfuric acid, the separated phthalic acid crude product and the resin desorption solution are together refined to recover the phthalic acid, and low-temperature drying is performed to directly reuse the phthalic acid into the product synthesis process. The technique can effectively treat wastewater generated in the 1,4-dihydroxy anthraquinone production process and recover the organic chemical raw materials phthalic acid and sulfuric acid in the wastewater, thereby implementing unification of the wastewater treatment and resource recovery and implementing clean production.

Description

technical field [0001] The invention belongs to the field of dye production, and specifically relates to a clean production process of 1,4-dihydroxyanthraquinone, in particular, using phthalic acid as the main raw material, recovering excessive phthalic acid and the treated phthalic acid from the mother liquor produced Dilute sulfuric acid reuse process. Background technique [0002] 1,4-Dihydroxyanthraquinone is dark orange powder, soluble in sulfuric acid, sodium hydroxide solution, chlorobenzene and dichlorobenzene, is an important dye intermediate, and itself is also an important dye. At present, phthalic anhydride is mainly used as raw material for synthesis in China, and the excess of phthalic anhydride is 20-50%. To produce 1 ton of 1,4-dihydroxyanthraquinone, 20-30 tons of orange mother liquor water with CODcr as high as 20,000-40,000mg / L will be discharged, mainly phthalic acid and a small amount of 1,4-dihydroxyanthraquinone and its by-products The product has a ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C50/34C07C46/00
CPCC07C46/00C07C46/10C07C2603/24C07C50/34
Inventor 陈宝兴夏骏钢陈海滨赵益明
Owner ZHEJIANG RUNTU INST
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