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Novel production method of benzanthrone

A technology of benzoanthrone and its production method, which is applied in the field of fine chemicals, can solve the problems such as difficult recycling of raw materials and reaction by-products, and achieve the effects of low cost, easy process control, and high recycling rate

Pending Publication Date: 2020-01-10
JIANGSU YABANG DYE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The first purpose of the present invention is to overcome the disadvantages of raw materials and reaction by-products in the prior art that are not easy to recycle, and provide a production method of benzoxantrone with high recycling rate of raw materials and easy control of process

Method used

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  • Novel production method of benzanthrone
  • Novel production method of benzanthrone
  • Novel production method of benzanthrone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Prepare anthraquinone 21kg (molecular weight 208.2, 101mol), ruthenium carbon (containing 5% palladium carbon) 0.26kg, 60% sulfuric acid 0.08kg, phase transfer catalyst sodium lauryl sulfate 210g, chlorobenzene 100kg, put the above-mentioned substances into 600L In a pressure reactor with a capacity of 2 At the same time, make the pressure in the container reach 1400kPa, stir at 175°C for 6.5h; cool the reaction solution to 110°C, and discharge the remaining H 2 Finally, filter the reaction solution, then wash in batches with 30L chlorobenzene, and the filter cake is used as the next batch of catalyst recycling;

[0033] Then the above-mentioned chlorobenzene residue and washing liquid are poured into a 500L clean reactor, and then 20.6kg (molecular weight 92.1, 200mol) of glycerine (glycerine) (glycerine) with a concentration of 85% is added, and heated to 105 while stirring. ℃;

[0034] Control the reaction temperature at 105-120°C and add 35.8kg of sulfuric acid (m...

Embodiment 2

[0037] Prepare anthraquinone 21kg (molecular weight 208.2, 101mol), ruthenium carbon 0.10kg, 60% sulfuric acid 0.04kg, phase transfer catalyst sodium lauryl sulfate 105g, chlorobenzene 65kg, put the above-mentioned material in the pressure reactor of 400L capacity, In access to H 2 At the same time, make the pressure in the container reach 1200kPa, stir at 180°C for 6h; cool the reaction solution to 110°C, and discharge the remaining H 2 Finally, filter the reaction solution, then wash in batches with 30L chlorobenzene, and the filter cake is used as the next batch of catalyst recycling;

[0038] Then, pour the above-mentioned chlorobenzene residue and washing liquid into a 500L clean reactor, then add 15.4kg of glycerol (molecular weight: 92.1, 150mol) with a concentration of 85%, and heat to 110°C while stirring;

[0039] Control the reaction temperature at 100-120°C and add 21.9kg of sulfuric acid (molecular weight: 98, 200mol) with a concentration of 85% dropwise. After t...

Embodiment 3

[0041]Prepare anthraquinone 21kg (molecular weight 208.2, 101mol), ruthenium carbon (containing 5% palladium carbon) 0.40kg, 80% sulfuric acid 0.26kg, phase transfer catalyst sodium lauryl sulfate 210g, chlorobenzene 160kg, put the above-mentioned substances into 800L In a pressure reactor with a capacity of 2 At the same time, make the pressure in the container reach 1600kPa, stir at 160°C for 8h; cool the reaction solution to 100°C, and discharge the remaining H 2 Finally, filter the reaction solution, then wash in batches with 30L chlorobenzene, and the filter cake is used as the next batch of catalyst recycling;

[0042] Then, pour the above-mentioned chlorobenzene residue and washing liquid into a 600L clean reactor, and then add 30.8kg (molecular weight 92.1, 300mol) of glycerine (glycerine) with a concentration of 85%, and heat it to 105 while stirring. ℃;

[0043] Control the reaction temperature at 105-120°C and add 54.8kg of sulfuric acid (molecular weight 98,500mo...

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Abstract

The invention relates to the field of fine chemical engineering, and concretely relates to a preparation method of benzanthrone. The method concretely comprises the following steps: adding anthraquinone, ruthenium carbon, sulfuric acid, a phase transfer catalyst and a solvent into a pressure reaction kettle, introducing H2, and performing a reaction; cooling the obtained reaction solution after the reaction is finished, discharging the residual H2, filtering the reaction solution, washing the obtained filtrate with a solvent, mixing the filtrate with the obtained washing solution, and transferring the obtained solution into a second reaction kettle; repeatedly using obtained filter residue as a catalyst for the next batch; adding glycerol into the second reaction kettle, adding a catalystsulfuric acid, and performing a cyclization reaction; and performing distillation after the reaction is finished to remove the solvent, washing residues with hot water, and drying the washed residuesto obtain the benzanthrone. Compared with the prior art, the production method of benzanthrone, provided by the invention, has the characteristics that high recycling rate of raw materials, easiness in process control, low cost, and obvious improvement of the product quality.

Description

technical field [0001] The invention relates to the field of fine chemical industry, in particular to a new production method of benzantrone. Background technique [0002] Dye is an indispensable fine chemical in modern society. As a traditional dye with complete color spectrum, bright color and good fastness, it has a history of thousands of years. It is a high-grade dye widely used in cotton dyeing. It is widely used in the overdyeing of cellulose fibers and polyester / cotton blends. Some of these vat dyes can also be used for polyester fiber and vinylon dyeing. As far as the environment is concerned, vat dyes do not contain azo substances that will be cracked under specific conditions to produce carcinogenic aromatic amines. After dyeing, they are comfortable to wear and will not cause allergies. They do not have carcinogenic acute toxicity, do not contain environmental hormones, and waste water when used. It has low chromaticity and low toxicity to fish, so vat dyes are...

Claims

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Application Information

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IPC IPC(8): C07C45/68C07C45/82C07C49/788
CPCC07C45/68C07C45/82C07C2603/42C07C49/788
Inventor 熊俊汤学斌周坚彪
Owner JIANGSU YABANG DYE
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