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Production method of fast scarlet base G

A production method, red-based technology, applied in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc., can solve the problems of difficult disposal of waste acid, low yield, high energy consumption, etc., to reduce the concentration of nitric acid, production The effect of low risk and controlled reaction speed

Inactive Publication Date: 2019-06-28
山东世纪阳光科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the technical problems of high energy consumption, low yield and difficult disposal of waste acid in the production process of scarlet-based G in the prior art, the present invention provides a kind of scarlet-based G that can be nitrated at room temperature and can obviously improve the product yield. The production method has the advantages of low energy consumption, high yield, easy disposal of waste acid, etc.

Method used

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  • Production method of fast scarlet base G
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The production method of a kind of bright red base G of the present embodiment is characterized in that, comprises the steps:

[0028] a) Salt formation: pump o-methylaniline and glacial acetic acid into the reaction kettle, then add chloroacetic acid, raise the temperature to about 60°C, and extract the hydrogen chloride gas generated by the reaction through a micro-vacuum;

[0029] b) Nitrification: Control the temperature at 30°C, and add the mixture of glacial acetic acid and nitric acid dropwise from the high-level tank;

[0030] c) After the dropwise addition is completed, stir evenly and put it into the separation kettle, then pump methyl tert-butyl ether into the separation kettle, and separate the solid to the double decomposition kettle through pressure filtration, and the liquid to the distillation kettle;

[0031] d) Heating the distillation kettle to 55°C, condensing and recovering methyl tert-butyl ether and remaining glacial acetic acid;

[0032] e) Meta...

Embodiment 2

[0034] The production method of a kind of bright red base G of the present embodiment is characterized in that, comprises the steps:

[0035] b) Salt formation: pump o-methylaniline and glacial acetic acid into the reaction kettle, then add chloroacetic acid, raise the temperature to 62°C, and extract the hydrogen chloride gas generated by the reaction through a slight vacuum;

[0036] b) Nitrification: Control the temperature at 32°C, and add the mixture of glacial acetic acid and nitric acid dropwise from the elevated tank;

[0037] c) After the dropwise addition is completed, stir evenly and put it into the separation kettle, then pump methyl tert-butyl ether into the separation kettle, and separate the solid to the double decomposition kettle through pressure filtration, and the liquid to the distillation kettle;

[0038] d) Heating the distillation kettle to 55°C, condensing and recovering methyl tert-butyl ether and remaining glacial acetic acid;

[0039] e) Metathesis:...

Embodiment 3

[0041] The production method of a kind of bright red base G of the present embodiment is characterized in that, comprises the steps:

[0042] c) Salt formation: pump o-methylaniline and glacial acetic acid into the reaction kettle, then add chloroacetic acid, raise the temperature to 65°C, and extract the hydrogen chloride gas generated by the reaction through a slight vacuum;

[0043] b) Nitrification: Control the temperature at 35°C, and add the mixture of glacial acetic acid and nitric acid dropwise from the elevated tank;

[0044] c) After the dropwise addition is completed, stir evenly and put it into the separation kettle, then pump methyl tert-butyl ether into the separation kettle, and separate the solid to the double decomposition kettle through pressure filtration, and the liquid to the distillation kettle;

[0045] d) Heating the distillation kettle to 56°C, condensing and recovering methyl tert-butyl ether and remaining glacial acetic acid;

[0046] e) Metathesis:...

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Abstract

The invention provides a production method of fast scarlet base G, belonging to the field of production of pigment intermediates. The production method is characterized by comprising the following steps: salifying, nitration, double decomposition and the like. By carrying out salifying through o-toluidine and acetic acid, the oxidization of amino can be prevented, and an ortho-para group of aminocan be changed into a meta-position orientating group; mixed acid is prepared from acetic acid, so that the concentration of nitric acid can be effectively decreased, and the control speed can be controlled; and by carrying out material separation through methyl tert-butyl ether, the complete material separation can be realized, and the quantity of materials dissolved in acetic acid is decreased.Therefore, the nitration production of the fast scarlet base G can be realized at a normal temperature, the reaction conditions are mild, and the production risk is relatively low.

Description

technical field [0001] The invention relates to the production field of pigment intermediates, in particular to a production method of a scarlet base G. Background technique [0002] Scarlet base G is an organic pigment intermediate, which is an important component of insoluble azo dyes. It is mainly used for dyeing and printing cotton fabrics. It can also be used to dye bright red (flag red) by coupling with naphthol AS or AS-E Dyeing of silk, viscose and nylon fabrics. [0003] The existing production method of scarlet base G is to use o-methylaniline as raw material, form a salt with concentrated sulfuric acid at room temperature, then nitrate with mixed acid at minus 15°C, and then neutralize. The disadvantage of this process is that low temperature reaction is required, a large amount of frozen brine is consumed, and a large amount of waste sulfuric acid is produced at the same time, which cannot be applied mechanically and is difficult to handle. In addition, the yiel...

Claims

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Application Information

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IPC IPC(8): C07C209/62C07C211/52C07C227/08C07C227/16C07C229/18
Inventor 黄长亮梁传刚于宪松
Owner 山东世纪阳光科技有限公司
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