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Preparation technology of solvent dye

A preparation process and technology for solvent dyes, applied in anthracene dyes, organic dyes, chemical instruments and methods, etc., can solve the problems of low reaction yield, dark product color, low product purity, etc., and achieve the effect of reducing the difficulty of wastewater treatment

Inactive Publication Date: 2018-09-28
JIANGSU DAOBO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction yield is low, the product purity is low, the color of the product is dark, and the bulk density is only 0.2g / cm3

Method used

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  • Preparation technology of solvent dye
  • Preparation technology of solvent dye
  • Preparation technology of solvent dye

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a 500mL four-necked flask equipped with an electric stirrer, 215ml of o-dichlorobenzene, 6.5g of stannous chloride, 100g of 1,4-dihydroxyanthraquinone, and 86g of isopropylamine hydrochloride were put into the reactor, and the temperature was raised to React at 84°C for 10 hours. After the reaction, evaporate part of the o-dichlorobenzene solvent, add 50ml of ethanol and petroleum ether mixed solvent, filter, wash, and dry to obtain 118.86g of the target product. The yield is 88.7%, the purity is 99.2%, the shade DC is 0.51, and the bulk density is 0.60g / cm 3 .

Embodiment 2

[0027] Other conditions are the same as in Example 1. The experiment of detecting different mass ratios of isopropylamine hydrochloride / 1,4-dihydroxyanthraquinone is shown in Table 1.

[0028] Table 1 Experiments of different mass ratios of isopropylamine hydrochloride / 1,4-dihydroxyanthraquinone

[0029]

[0030] From the above results, it can be known that the mass ratio of isopropylamine hydrochloride / 1,4-dihydroxyanthraquinone is preferably 0.86 (Example 1).

Embodiment 3

[0032] Other conditions are the same as in Example 1, and the experiment of detecting different mass ratios of stannous chloride / 1,4-dihydroxyanthraquinone is shown in Table 2 for the experimental results.

[0033] Table 2 Experiments of different stannous chloride / 1,4-dihydroxyanthraquinone mass ratios

[0034]

[0035] It can be known from the above results that the mass ratio of stannous chloride / 1,4-dihydroxyanthraquinone is preferably 0.065 (Example 1).

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Abstract

The invention discloses a preparation technology of a solvent dye. O-dichlorobenzene is taken as a solvent, stannous chloride is taken as a catalyst, and condensation reaction is carried out on 1,4-dioxyanthraquinone and isopropylamine hydrochloride to prepare a target product. According to the preparation technology of the solvent dye, volatile solution isopropylamine is replaced with isopropylamine hydrochloride, the isopropylamine does not need to recycled, high-concentration nitrogen-containing wastewater cannot be generated, thereby reducing the difficulty of wastewater treatment; compared with an aqueous phase method, a solvent method is adopted to prepare 1,4-bi(1-isopropylamido) anthraquinone, and the wastewater quantity is sharply reduced; recrystallization is carried out on a mixed solvent of ethyl alcohol and petroleum ether, a sample of which the purity is 99.0% and the colored light is DC 0.5-1.5 specification can be prepared by adjusting a crystallization solvent, and thepreparation technology has a potential commercial prospect; the product yield can reach 92% or above, and the bulk density is 0.5 gram per cubic centimeter or above.

Description

technical field [0001] The invention relates to a preparation process of solvent dyes, in particular to a preparation process of 1,4-bis(1-isopropylamino)anthraquinone, which belongs to the field of dye preparation. Background technique [0002] 1,4-bis(1-isopropylamino)anthraquinone is a solvent dye with excellent performance, which is mainly suitable for the coloring of ABS, PC, HIPS, PMMS and other resins. [0003] Its molecular formula is C 20 h 22 N 2 o 2 , molecular weight 322.4, structural formula: [0004] [0005] The original production process is to use 1,4-dihydroxyanthraquinone as the raw material. In alkaline water, use hydrosulfite as the reducing agent to react with isopropylamine. After the reaction is completed, filter and wash with hot water to remove the unreacted isopropylamine. Finally dried to get the finished product. The reaction yield is low, the product purity is low, the product shade is dark, and the bulk density is only 0.2g / cm3. Cont...

Claims

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Application Information

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IPC IPC(8): C09B1/28
CPCC09B1/285
Inventor 陈路云刘学峰徐松郭维城
Owner JIANGSU DAOBO CHEM
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