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Preparation method of isoviolanthrone

A technology of isoxanthrone and benzoxanthone, which is applied in the field of preparation of isoxanthrone, can solve problems such as increased production cost, unfriendly environment, environmental pollution, etc., and achieves avoiding waste of raw materials, reducing production cost, and reducing disposal volume effect

Active Publication Date: 2022-03-22
赤峰市恒祥化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A large amount of sulfur-containing wastewater will be produced in the above-mentioned process of preparing isovinanthrone, which is very unfriendly to the environment and easily pollutes the environment. At the same time, excessive alkali is wasted, which increases the production cost

Method used

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  • Preparation method of isoviolanthrone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1: Add 120g of potassium hydroxide, 80g of triethylene glycol, and 0.6g of tetrabutylammonium bromide into the reaction flask and mix evenly, then raise the temperature to 170-190°C, and keep it warm for 1h, so as to make the mixture more full and obtain a mixed solution; Then divide 60g of benzothrone evenly into 24 times, and add benzoxanthone each time when the temperature of the mixed solution drops to 170° C. During the ketone process, the compressed air with a pressure of 0.025MPa was always fed, and then the heat preservation was continued for 3 hours. After the heat preservation was completed, the compressed air was stopped and cooled naturally to 50-100°C to obtain 133ml of reaction materials, which were placed in 700ml Stir and dilute in water for 3 hours at a stirring speed of 700rpm, and then obtain 0.8L of mother liquor and solid material through filtration; the solid material is dried at 105-125°C after washing to obtain 59.5g of isoviolanthrone; th...

Embodiment 2

[0027] Example 2: Add 600g of potassium hydroxide, 600g of triethylene glycol and 3g of tetrabutylammonium bromide into the reaction flask and mix evenly, then raise the temperature to 170-190°C, keep it warm for 1h, the purpose is to make the mixture more full, and obtain a mixed solution; then Divide 60g of benzoxantrone evenly into 12 times, and add benzoxantrone each time when the temperature of the mixed solution drops to 170°C, so as to avoid adding too much at one time and causing the solution to become viscous and unable to fully react. During the process, the compressed air with a pressure of 0.025MPa has been introduced, and then the heat preservation is continued for 3h. After the heat preservation is completed, the compressed air is stopped and cooled naturally to 50-100°C to obtain 800ml of reaction materials, which are placed in a 3000ml Stir and dilute in water for 5 hours at a stirring speed of 500rpm, and then filter to obtain 3.4L of mother liquor and solid ma...

Embodiment 3

[0029] Example 3: Add 360g of potassium hydroxide, 60g of triethylene glycol, and 1.8g of tetrabutylammonium bromide into the reaction flask and mix evenly, then raise the temperature to 170-190°C and keep it warm for 1h to make the mixture more filling and obtain a mixed solution; Then divide 60g of benzothrone evenly into 30 times, and add benzoxanthone each time when the temperature of the mixed solution drops to 170°C, so as to avoid adding too much at one time to cause the solution to be viscous and then unable to fully react. During the ketone process, the compressed air with a pressure of 0.025MPa was continuously fed, and then the heat preservation was continued for 3 hours. After the heat preservation was completed, the compressed air was stopped and cooled naturally to 50-100°C to obtain 120ml of reaction materials, which were placed in 2400ml Stir and dilute in water for 30min at a stirring speed of 700rpm, and then obtain 2.4L of mother liquor and solid material by ...

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Abstract

The invention discloses a preparation method of isoviolanthrone. The preparation method sequentially comprises the following steps: (1) preparing a mixed solution; (2) redox reaction; and (3) preparing the isoviolanthrone. The preparation method has the beneficial effects that the reaction process is simple, the production efficiency is improved, and the yield of intermediate wastewater is reduced, so that the treatment capacity of the wastewater is reduced; according to the invention, zero emission is basically realized, the goal of green production is realized, raw material waste is avoided, and the production cost is reduced.

Description

Technical field: [0001] The patent of the present invention relates to the technical field of organic vat dyes, in particular to a preparation method of isoxanthrone. Background technique: [0002] Isoviolanthrone, commonly known as reduced violet 10, is soluble in o-chlorophenol and xylene and is red, with fluorescence, slightly soluble in acetone, chloroform, pyridine and toluene, and insoluble in ethanol. It is dark green in concentrated sulfuric acid, and there will be purple precipitate after dilution; it is dark red and light blue in alkaline hydrosulfuric acid solution; it is dark red in acidic hydrosulfuric acid solution. It is mainly used for dyeing, direct printing, resist printing and discharge printing of cotton and its blended fabrics, and it can also be used for dyeing viscose fibers. The existing method for preparing isoxanthrone is to obtain 3-bromobenzoxanthrone after bromination of benzoxanthrone, and 3-bromobenzoxanthrone is converted into the correspondi...

Claims

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Application Information

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IPC IPC(8): C07C45/39C07C49/665C09B3/34
CPCC07C45/39C07C45/72C07C29/68C09B3/34C07C2603/54C07C2603/42C07C49/665C07C35/46
Inventor 周林黄斌
Owner 赤峰市恒祥化工有限公司
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