Synthetic method of low-toxicity low-harm environment-friendly solvent green 3

An environment-friendly solvent and synthetic method technology, applied in chemical instruments and methods, preparation of organic compounds, physical/chemical process catalysts, etc., can solve problems affecting reaction selectivity, poor color reproducibility, operator poisoning, etc., to achieve Improved product purity, good high temperature stability, and improved safety

Pending Publication Date: 2019-12-27
安徽清科瑞洁新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The quality of solvent green 3 products produced by this process is poor, and the reproducibility of color and light is poor. The hue △E>0.5 accounts for about 50% of the total output. Some single-batch products need to be refined by solvents to achieve qualified quality, resulting in waste of resources. and excessive toxic solvents need reclaiming to toluidine, and the on-site environmen...

Method used

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  • Synthetic method of low-toxicity low-harm environment-friendly solvent green 3
  • Synthetic method of low-toxicity low-harm environment-friendly solvent green 3

Examples

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preparation example Construction

[0023] A kind of synthetic method of low toxicity and low harm environment-friendly solvent green 3 of the present invention comprises the following steps:

[0024] (a) Add N-butylimidazole and acetone to the reaction vessel, then slowly add bromoethane dropwise under stirring for reaction, add sodium tetrafluoroborate after reacting for 2-4h for anion exchange, and continue stirring for 4-6h, Acetone is removed by distillation under reduced pressure to obtain an ionic liquid; the mass ratio of N-butylimidazole, ethyl bromide, and sodium tetrafluoroborate is 1 to 1.1:1:1, and the mass ratio of acetone to N-butylimidazole is 1.2 ~1.5:1.

[0025] (b) Raise the temperature of the ionic liquid to 80-90°C, then add 1,4-dihydroxyanthraquinone, 1,4-dihydroxyanthraquinone leuco, and p-methylaniline to the ionic liquid, and stir to raise the temperature to 120- Condensation reaction was carried out at 130°C, and the end point of the reaction was determined by HPLC detection to obtain ...

Embodiment 1

[0030] This embodiment provides a synthetic method of low-toxicity, low-hazard and environment-friendly solvent green 3, which comprises the following steps:

[0031] (a) add 480 kilograms of N-butyl imidazoles, 600 kilograms of acetones in the reaction vessel, then slowly drip 450 kilograms of bromoethanes under stirring to react, add 450 kilograms of sodium tetrafluoroborates after reacting 3h and carry out anion exchange, Stirring was continued for 5h, and acetone was removed by distillation under reduced pressure to obtain an ionic liquid;

[0032] (b) Heat up the ionic liquid to 85°C, then add 900 kg of 1,4-dihydroxyanthraquinone, 300 kg of 1,4-dihydroxyanthraquinone leuco, and 1,800 kg of p-methylaniline to the ionic liquid, and stir The temperature is raised to 125°C for condensation reaction, and the end point of the reaction is determined by HPLC detection to obtain the first mixed solution;

[0033] (c) cooling the first mixed solution to 45°C for suction filtration...

Embodiment 2

[0035]The present embodiment provides a kind of synthetic method of low toxicity, low harm and environment-friendly solvent green 3, which is basically the same as that in Example 1, except that the amount of p-methylaniline added in step (b) is 1200 kilograms; finally After drying, crushing and packaging, 1991 kg of solvent green 3 finished product was obtained; the yield was 95.2%, the HPLC content was 98.65%, △E 0.486, △C 0.388 partial bright, pressure value 0.19.

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Abstract

The invention relates to a synthesis method of a low-toxicity low-harm environment-friendly solvent green 3, which comprises the following steps: (a) adding N-butylimidazole and acetone into a reaction vessel, slowly dropwise adding bromoethane for reaction, adding sodium tetrafluoroborate for anion exchange, and continuing stirring the reactants to obtain an ionic liquid; (b) adding 1,4-dihydroxyanthraquinone, a 1,4-dihydroxy anthraquinone leuco body and p-toluidine into the ionic liquid, and carrying out condensation reaction to obtain a first mixed solution; and (c) cooling the first mixedsolution, carrying out suction filtration to obtain a filter cake and a filtrate, and carrying out washing post-treatment on the filter cake to obtain the solvent green 3. According to the method, the synthesized ionic liquid is used as a solvent, the condensation reaction is double condensation through model selection of organic cations and anions in the ionic liquid, the product purity is obviously improved to 98% or above, the yield reaches 95% or above, in addition, the ionic liquid can be recycled, the cost is greatly reduced, and the pollutant discharge amount is reduced; the performances of the solvent green 3 dye as shown as follows: the [delta]E is less than 0.5, [delta]C is brilliant, and the pressure value is less than 0.2.

Description

technical field [0001] The invention relates to a synthesis method of a dye, in particular to a synthesis method of low-toxicity, low-hazard and environment-friendly solvent green 3. Background technique [0002] Solvent Green 3 is also known as Oil-Soluble Green 5B and Transparent Green 5B. Its chemical name is 1,4-bis(p-methylanilino)-anthraquinone, its English name is Solvent Green 3, and its molecular formula is C 28 h 22 N 2 o 2 , the molecular weight is 418.49, and the CAS number is 128-80-3. The appearance of this product is blue-black powder, insoluble in water, soluble in organic solvents such as chloroform, benzene, chlorobenzene, xylene, DMF, etc., blue in concentrated sulfuric acid, and blue-green precipitates after dilution with water. The melting point is 213°C. The light fastness in PS can reach grade 7-8, and the heat resistance in PS can reach 300°C. Solvent green 3 is mainly used for the coloring of various resins, as well as the coloring of polyester...

Claims

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Application Information

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IPC IPC(8): C07C221/00C07C225/34C09B1/32B01J31/02
CPCC07C221/00C09B1/325B01J31/0281C07C225/34
Inventor 周利霞陈胜杨庆水刘镛
Owner 安徽清科瑞洁新材料有限公司
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