Synthesis device of 2,6-dichloro-4-amino phenol and application thereof

Abstract

A synthesis device of 2,6-dichloro-4-amino phenol comprises a first raw material storage tank group, a mixing kettle, a first raw material storage tank, a kettle type reactor, a first solid-liquid separator, a drying tower, a second raw material storage tank group, a second raw material storage tank, a tower type reactor, a second solid-liquid separator and a distillation tower; a discharging hole of the first raw material storage tank group is connected with a feeding hole of the mixing kettle; discharging holes of the mixing kettle and the first raw material storage tank are connected with a feeding hole of the kettle type reactor; a discharging hole of the kettle type reactor is connected to a feeding hole of the first solid-liquid separator; a solid-phase flow outlet of the first solid-liquid separator is connected with a feeding hole of the tower reactor, and a drying tower is arranged between the solid-phase flow outlet and the feeding hole; discharging holes of the second raw material storage tank group and the second raw material storage tank are connected with a feeding hole of the tower reactor; a discharging hole of the tower reactor is connected to a feeding hole of the second solid-liquid separator, and the distillation tower is arranged at a liquid phase flow outlet of the second solid-liquid separator. The device can efficiently and continuously synthesize 2,6-dichloro-4-amino phenol with high purity and high yield.

Description

technical field

[0001] The invention relates to the field of organic chemical industry, more specifically, it relates to a synthesis device of 2,6-dichloro-4-aminophenol and its application. Background technique

[0002] 2,6-dichloro-4-aminophenol is an important intermediate in the synthesis of hexaflumuron. Hexaflumuron is a benzoylurea insecticide, a chemical that is soluble in acetone and methylene chloride and has stable chemical properties. It belongs to chitin synthesis inhibitor, has high insecticidal and ovicidal activity, and is quick-acting, especially for the control of cotton bollworm.

[0003] At present, the main synthesis process of 2,6-dichloro-4-aminophenol is: using p-nitrophenol as raw material, chlorination reaction with chlorine gas in hydrochloric acid to generate 2,6-dichloro-4-nitrophenol , 2,6-dichloro-4-nitrophenol is reduced by a reducing agent at high temperature to generate 2,6-dichloro-4-aminophenol.

[0004] For the above-mentioned technolo...

Examples

Embodiment 1

[0045] Such as figure 1 Shown, a kind of synthesis device of 2,6-dichloro-4-aminophenol comprises the first raw material storage tank group 1, mixing tank 2, the first raw material storage tank 3, tank reactor 4, the first solid Liquid separator 5, standing pool 6, drying tower 7, second raw material storage tank group 8, second raw material storage tank 9, tower reactor 10, second solid-liquid separator 11, distillation tower 12, purification tower 13 and reflux tank 14.

[0046]In the first raw material storage tank group 1, 2,6-dichlorophenol of industrial purity 99.5%, tetrachlorethylene of industrial pure 99.5% and concentrated sulfuric acid of industrial pure 98% are isolated and stored, the first raw material storage tank group 1 The discharge port is connected to the feed port of the mixing tank 2 through a pipeline with a valve; the discharge port of the mixing tank 2 is connected to the feed port of the tank reactor 4 through a pipeline with a valve.

[0047] In th...

Embodiment 2

[0067] A kind of synthetic device of 2,6-dichloro-4-aminophenol, same as embodiment 1.

[0068] A kind of application of the synthesis device of 2,6-dichloro-4-aminophenol, for continuous synthesis of 2,6-dichloro-4-aminophenol, comprising the steps:

[0069] S1. Preparation of 2,6-dichloro-4-nitrophenol from 2,6-dichlorophenol:

[0070] S1-1. From the first raw material storage tank group 1 to the mixing tank 2 that is always running at 600r / min, put 2,6-dichlorophenol into it at 2Kg / h, flow into tetrachlorethylene at 6L / h, and feed it at 0.06 L / h flows into concentrated sulfuric acid;

[0071] S1-2. The tank reactor 4 is always kept at 35°C and stirred at 600r / min; nitric acid is always flowed from the first raw material storage tank 3 to the tank reactor 4 at 1.08L / h; every 2h, the mixing tank 2 The medium mixture flows into the tank reactor at 10L / h for 43h;

[0072] S1-3, every 5 hours, the mixture in the tank reactor 4 flows into the first solid-liquid separator 55 ho...

technical field

[0001] The invention relates to the field of organic chemical industry, more specifically, it relates to a synthesis device of 2,6-dichloro-4-aminophenol and its application. Background technique

[0002] 2,6-dichloro-4-aminophenol is an important intermediate in the synthesis of hexaflumuron. Hexaflumuron is a benzoylurea insecticide, a chemical that is soluble in acetone and methylene chloride and has stable chemical properties. It belongs to chitin synthesis inhibitor, has high insecticidal and ovicidal activity, and is quick-acting, especially for the control of cotton bollworm.

[0003] At present, the main synthesis process of 2,6-dichloro-4-aminophenol is: using p-nitrophenol as raw material, chlorination reaction with chlorine gas in hydrochloric acid to generate 2,6-dichloro-4-nitrophenol , 2,6-dichloro-4-nitrophenol is reduced by a reducing agent at high temperature to generate 2,6-dichloro-4-aminophenol.

[0004] For the above-mentioned technolo...

Examples

Embodiment 1

[0045] Such as figure 1 Shown, a kind of synthesis device of 2,6-dichloro-4-aminophenol comprises the first raw material storage tank group 1, mixing tank 2, the first raw material storage tank 3, tank reactor 4, the first solid Liquid separator 5, standing pool 6, drying tower 7, second raw material storage tank group 8, second raw material storage tank 9, tower reactor 10, second solid-liquid separator 11, distillation tower 12, purification tower 13 and reflux tank 14.

[0046]In the first raw material storage tank group 1, 2,6-dichlorophenol of industrial purity 99.5%, tetrachlorethylene of industrial pure 99.5% and concentrated sulfuric acid of industrial pure 98% are isolated and stored, the first raw material storage tank group 1 The discharge port is connected to the feed port of the mixing tank 2 through a pipeline with a valve; the discharge port of the mixing tank 2 is connected to the feed port of the tank reactor 4 through a pipeline with a valve.

[0047] In th...

Embodiment 2

[0067] A kind of synthetic device of 2,6-dichloro-4-aminophenol, same as embodiment 1.

[0068] A kind of application of the synthesis device of 2,6-dichloro-4-aminophenol, for continuous synthesis of 2,6-dichloro-4-aminophenol, comprising the steps:

[0069] S1. Preparation of 2,6-dichloro-4-nitrophenol from 2,6-dichlorophenol:

[0070] S1-1. From the first raw material storage tank group 1 to the mixing tank 2 that is always running at 600r / min, put 2,6-dichlorophenol into it at 2Kg / h, flow into tetrachlorethylene at 6L / h, and feed it at 0.06 L / h flows into concentrated sulfuric acid;

[0071] S1-2. The tank reactor 4 is always kept at 35°C and stirred at 600r / min; nitric acid is always flowed from the first raw material storage tank 3 to the tank reactor 4 at 1.08L / h; every 2h, the mixing tank 2 The medium mixture flows into the tank reactor at 10L / h for 43h;

[0072] S1-3, every 5 hours, the mixture in the tank reactor 4 flows into the first solid-liquid separator 55 ho...

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