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Preparation method of pigment violet 23 crude product

A technology for pigment purple and crude products, which is applied in the direction of bisazine oxazine dyes, etc., can solve the problems of complicated processes and environmental pollution, and achieve the effects of improving purity, saving energy and improving quality

Active Publication Date: 2020-05-05
浙江浩川科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In view of this, the present invention proposes a method for preparing crude Pigment Violet 23, which aims to solve the problems of complex processes, environmental pollution, safety accidents, etc. caused by the selection of catalysts in the prior art

Method used

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  • Preparation method of pigment violet 23 crude product
  • Preparation method of pigment violet 23 crude product
  • Preparation method of pigment violet 23 crude product

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preparation example Construction

[0025] The present invention provides a kind of preparation method of Pigment Violet 23 crude product, comprises the following steps:

[0026] Step 1, add a certain amount of heteropolyacid to the organic solution containing condensate 2,5-dichloro-3,6-bis(9-ethyl-3-carbazole amino)-1,4-benzoquinone as The ring-closing oxidation catalyst is reacted at 125-145° C. under normal pressure for a period of time, wherein the amount of the heteropolyacid added is 0.1-5.0% of the mass of the condensate.

[0027] The molecular formula of the condensate 2,5-dichloro-3,6-bis(9-ethyl-3-carbazolylamino)-1,4-benzoquinone is as follows:

[0028]

[0029] In this embodiment, the method for preparing the condensate 2,5-dichloro-3,6-bis(9-ethyl-3-carbazolylamino)-1,4-benzoquinone can adopt any one of the prior art made by a process. E.g:

[0030] The preparation process of the 2,5-dichloro-3,6-bis(9-ethyl-3-carbazole amino)-1,4-benzoquinone condensate is as follows:

[0031] 3-amino-N-eth...

Embodiment 1

[0049] To 200g condensate 2,5-dichloro-3,6-bis(9-ethyl-3-carbazolamino)-1,4-benzoquinone and o-dichlorobenzene solvent mixture (containing 6.1% condensation Add phosphomolybdic acid [H 3 P(M O3 o 10 ) 4 ·XH 2 O, CAS No.51429-74-4] 0.122g, keep warm in a three-neck flask at 140°C, reflux at normal pressure for 4 hours, filter, wash with ethanol first, then wash with hot water, and dry to obtain 11.25g of Pigment Violet 23 The crude product was dissolved in pyridine, filtered and washed to remove impurities, and 11.02 g of pure crude Pigment Violet 23 was obtained, with a calculated purity of about 98% and a yield of 92.7%.

[0050] Mass spectrometry data proved that the molecular weight of the product was consistent with the theoretical value. MALDI-TOF (DHBA, +H): 588, theoretical value 588.11.

Embodiment 2

[0052] To 200g 2,5-dichloro-3,6-bis(9-ethyl-3-carbazolamino)-1,4-benzoquinone and o-dichlorobenzene solvent mixture (containing 6.1% condensate) Add phosphotungstic acid equivalent to 0.5% weight of condensate [H 3 PO 4 (WO 3 )·X H 2 O, CASNo.12067-99-1] 0.061g, keep warm in a three-necked flask at 140°C, reflux at normal pressure for 4 hours, filter, wash with ethanol first, then wash with hot water, and dry to obtain 11.61g of crude pigment violet 23 , dissolved in pyridine, filtered and washed to remove impurities to obtain 11.49 g of pure crude Pigment Violet 23, with a calculated purity of about 99% and a yield of 95.6%.

[0053] Mass spectrometry data proved that the molecular weight of the product was consistent with the theoretical value. MALDI-TOF (DHBA, +H): 588, theoretical value 588.11.

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Abstract

The invention provides a preparation method of a pigment violet 23 crude product. The method comprises the following steps: adding a certain amount of heteropolyacid into an organic solution containing a condensation compound 2, 5-dichloro-3, 6-bis (9-ethyl-3-carbazole amino)-1, 4-benzoquinone as a closed-loop oxidation catalyst, carrying out a normal-pressure reaction at 125-145 DEG C for a period of time, performing filtering, washing, and drying to obtain a pigment violet 23 crude product. According to the invention, heteropolyacid is selected as a catalyst for a ring-closure oxidation reaction, and a condensate does not need to be dewatered, so that the process is simplified, and the energy is saved; the reaction can be carried out at a relatively low temperature; heteropoly acid has weak corrosivity to equipment, so that the corrosion resistance requirement on the equipment is reduced; after the reaction is finished, heteropolyacid enters the wastewater along with the filtrate, sothat the influence on the environment is relatively small; the yield and purity of the pigment violet 23 crude product prepared by the preparation method provided by the invention are greatly improved, and the quality of subsequent products is favorably improved.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a method for preparing crude Pigment Violet 23. Background technique [0002] The synthesis of the existing Pigment Violet 23 crude product comprises the following reaction steps: [0003] [0004] Carbazole (I) reacts with halide ethane in the presence of a strong base (usually high concentration sodium hydroxide), an organic solvent (usually chlorobenzene or o-dichlorobenzene) and a phase transfer agent to form ethyl carbazole (II). Ethyl carbazole is dissolved in an organic solvent, left standing to separate from the lye, rinsed until neutral, and 35%-40% nitric acid is added for nitration reaction to obtain 3-nitro-N-ethyl carbazole (Ⅲ). 3-amino-N-ethylcarbazole (Ⅳ) can be obtained by hydrogenation reduction of the neutral 3-nitro-N-ethylcarbazole after separation and washing. Under the vacuum condition of 95-100°C, the water generated by the reduction reaction i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B19/02
CPCC09B19/02
Inventor 陈发生喻李江赵汉斌张燕
Owner 浙江浩川科技有限公司
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