Method for preparing 3-chloro-p-toluidine-6-sulfonic acid by liquid-phase baking method

A p-toluidine, liquid-phase technology, applied in the production of chemical raw material intermediates, can solve problems such as increased energy consumption, and achieve the effects of reducing oxidative carbonization, extremely high waste water volume, and high conversion rate

Active Publication Date: 2019-01-11
浙江友联化学工业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Regardless of solid-phase method or liquid-phase method, due to the need for refining processes such as alkali dissolution, decolorization, filtration, acid precipitation, deh

Method used

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  • Method for preparing 3-chloro-p-toluidine-6-sulfonic acid by liquid-phase baking method
  • Method for preparing 3-chloro-p-toluidine-6-sulfonic acid by liquid-phase baking method
  • Method for preparing 3-chloro-p-toluidine-6-sulfonic acid by liquid-phase baking method

Examples

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Effect test

Embodiment 1

[0034] Content 99.7% 2B oil 700kg, dispersant (dichlorobenzene: D60 = 3:2, mass ratio) 1900kg, put into sulfonation reaction kettle; add 98% concentrated sulfuric acid 493kg after 50min, control the temperature of cooling circulating water at 100℃ Below; after the addition of sulfuric acid, start to heat up, keep the temperature at 126°C for 2 hours, transfer the material to the baking kettle to raise the temperature to 168°C, and carry out the dehydration and transposition reaction. The temperature of the heat transfer oil outlet of the baking kettle is controlled at about 190°C; Switch to the water separator after 30 minutes of solvent, control the gas phase temperature at the outlet of the water separator at 96°C, keep warm and dehydrate under normal pressure for 12 hours; after 12 hours, take a sample and test, the acid content of liquid chromatography 2B is 98.4%, start vacuum drying, Control the temperature of the heat transfer oil outlet of the baking kettle at 180°C, dr...

Embodiment 2

[0036] Content 99.7% 2B oil 695kg, dispersant (dichlorobenzene: D60 = 9: 1, mass ratio) 1900kg, put into sulfonation reaction kettle; add 98% concentrated sulfuric acid 487.65kg after 55min, control the temperature of cooling circulating water 100 Below ℃; start to heat up after adding sulfuric acid, keep the temperature at 130°C for 2 hours, transfer the material to the baking kettle to raise the temperature to 170℃, control the temperature of the heat transfer oil outlet of the baking kettle at about 190℃; switch to Water separator, control the gas phase temperature at the outlet of the water separator at 95°C, keep warm and dehydrate under normal pressure for 12 hours; after 12 hours, take a sample and test, the acid content of liquid chromatography 2B is 97.9%, start vacuum drying and drying, control the heat transfer oil of the baking kettle Oil outlet temperature 180°C, drying for 5.5 hours, sampling test: amino value 98.20%, whiteness 80.6, moisture 0.24%, ammonia insolu...

Embodiment 3

[0038] Content 99.7% 2B oil 694.8kg, dispersant (dichlorobenzene: D60 = 7:3, mass ratio) 1900kg, put into sulfonation reaction kettle; add 98% concentrated sulfuric acid 487.8kg after 60min, control the temperature of cooling circulating water Below 100°C; start to heat up after adding sulfuric acid, keep the temperature at 130°C for 2 hours, transfer the material to the baking kettle and raise the temperature to 168°C, and control the temperature of the heat transfer oil outlet of the baking kettle at about 190°C; switch after 30 minutes for heat preservation and water outlet. To the water separator, control the gas phase temperature at the outlet of the water separator at 96°C, keep warm and dehydrate under normal pressure for 13 hours; after 13 hours, take a sample and test, the acid content of liquid chromatography 2B is 98.5%, start vacuum drying, and control the heat conduction of the baking kettle Oil outlet temperature 180°C, dry for 5 hours, sampling test: amino value ...

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Abstract

The invention provides a method for preparing 3-chloro-p-toluidine-6-sulfonic acid by a liquid-phase baking method. The method comprises the following steps: mixing high-purity 2B oil as a raw material with an organic solvent serving as a liquid dispersant, performing a sulfonation reaction on the 2B oil and concentrated sulfuric acid in the liquid phase dispersant, and dehydrating and drying thesulfonated product to obtain 2B acid. By adopting the method, the high quality 2B acid is directly prepared by dehydrating and translocating in a liquid phase, and refining processes such as alkali dissolving, decolorizing, filtering, acid separating, dehydrating, drying and the like, so that the 'Three Wastes' can be greatly reduced, no solid waste is generated, waste gas and waste water have extremely small amount and can be easily treated, energy consumption can be reduced, and the existing sulfonating process is broken through. The method has the advantages of high conversion rate, low carbonization, few processes and low energy consumption.

Description

technical field [0001] The invention belongs to the production field of chemical raw material intermediates, and in particular relates to a method for preparing 3-chloro-p-toluidine-6-sulfonic acid by a liquid-phase baking method. Background technique [0002] 3-Chloro-p-toluidine-6-sulfonic acid, namely 2B acid, is one of the eight most important varieties of organic pigment intermediates. It is mainly used in the production of C.I. Pigment Red 48 series red pigments in the pigment industry. The pigment is widely used in paints, coatings, colored inks, rubber and plastic coloring, etc. [0003] In the preparation of 2B acid, concentrated sulfuric acid is usually used as a sulfonating agent, and 2B oil (3-chloro-4-methylaniline) is sulfonated into a salt, dehydrated and transpositioned to obtain a sulfonated product, which is then hydrolyzed by liquid alkali , decolorization, filtration, acid crystallization, dehydration, drying and other refining processes to obtain the pr...

Claims

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Application Information

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IPC IPC(8): C07C303/06C07C309/48
CPCC07C303/06C07C309/48
Inventor 俞卫祥杨卫东王成许青山芮毅张玉超
Owner 浙江友联化学工业有限公司
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