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Production process of byproduct potassium bromide in propiconazole synthesis

A production process and technology of potassium bromide, applied in the chemical industry, organic chemistry, alkali metal halide purification and other directions, can solve the problems of high separation and purification cost, waste of resources, difficult separation of potassium bromide, etc., and reduce the cost of separation and purification. , resource saving, high purity effect

Active Publication Date: 2019-08-16
浙江禾本科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to overcome the deficiencies in the prior art, to provide a production process for the by-product potassium bromide in the synthesis of propiconazole, which can solve the difficulty in separating the by-product potassium bromide in the process of generating propiconazole at present, and the resource Severe waste and high cost of separation and purification

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  • Production process of byproduct potassium bromide in propiconazole synthesis

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Embodiment 1

[0029] A kind of production technology of by-product potassium bromide in the synthesis of propiconazole

[0030] Proceed as follows:

[0031] Step 1. Put 425kg of potassium triazole, 1460kg of DMF, and 980kg of bromide into a 3000L kettle, raise the temperature to 135°C at a rate of 5°C / min and keep it warm for 5.5 hours. Recover DMF under pressure, and stop recovery when the temperature of the reactant drops to 135°C;

[0032] Among the above, the bromide is 2-bromomethyl-(2,4-dichlorophenyl)-4-propyl-1,3-dioxolane; the content of bromide in the reaction is 0.42%.

[0033] Step 2. After the DMF is removed, add 1160kg of toluene to the reactant, raise the temperature to 100°C, and then transfer all the materials to a three-in-one filter equipment, and use nitrogen pressure filtration, wherein the pressure is 0.5MPa, and the solid after filtration is Add 500kg of toluene again, turn on the three-in-one stirring and heating equipment, raise the temperature to 100°C, heat and ...

Embodiment 2

[0036] A kind of production technology of by-product potassium bromide in the synthesis of propiconazole

[0037] Proceed as follows:

[0038] Step 1: Put 445kg of potassium triazole, 1520kg of DMF, and 1020kg of bromide into a 3000L kettle, heat up to 155°C at a rate of 15°C / min and keep warm for 6.5 hours. Recover DMF under pressure, and stop the recovery when the temperature of the reactant drops to 140°C;

[0039] Among the above, the bromide is 2-bromomethyl-(2,4-dichlorophenyl)-4-propyl-1,3-dioxolane; the content of bromide in the reaction is 0.38%.

[0040]Step 2: After the DMF is removed, add 1240kg of toluene to the reactant, raise the temperature to 120°C, and then transfer all the materials to the three-in-one filter equipment, and use nitrogen pressure filtration, wherein the pressure is 0.8MPa, and the solid after filtration is Add 500kg of toluene again, turn on the three-in-one stirring and heating equipment, raise the temperature to 120°C, heat and stir for 8...

Embodiment 3

[0043] A kind of production technology of by-product potassium bromide in the synthesis of propiconazole

[0044] Step 1. Put 430kg of potassium triazole, 1480kg of DMF, and 990kg of bromide into a 3000L kettle, and raise the temperature to 140°C at a rate of 8°C / min and keep it warm for 6.5 hours. After the reaction is completed, under the condition of vacuum degree of -0.098MPa, Recover DMF under reduced pressure, and stop the recovery when the temperature of the reactant drops to 1360°C;

[0045] Among the above, the bromide is 2-bromomethyl-(2,4-dichlorophenyl)-4-propyl-1,3-dioxolane; the content of bromide in the reaction is 0.25%.

[0046] Step 2. After the DMF is removed, add 1180kg of toluene to the reactant, raise the temperature to 105°C, and then transfer all the materials to a three-in-one filter equipment, and use nitrogen pressure filtration, wherein the pressure is 0.6MPa, and the solid after filtration is Add 500kg of toluene again, turn on the three-in-one st...

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Abstract

The invention discloses a production process of byproduct potassium bromide in propiconazole synthesis. The production process of the byproduct potassium bromide in propiconazole synthesis comprises the processes of product desolvation, toluene separation, DMF separation and purification, drying and high-temperature calcination and purification. According to the production process of the byproductpotassium bromide in propiconazole synthesis, after potassium triazole and a bromide are condensed by taking DMF as a solvent to generate propiconazole, firstly the solvent DMF is removed, a crude propiconazole product is separated in batches by using toluene, then the potassium triazole is separated by using the DMF solvent, finally the remaining solid, namely the potassium bromide is purified by drying and high-temperature calcination to obtain a potassium bromide solid with a purity of more than 98%.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a production process for by-product potassium bromide in the synthesis of propiconazole. Background technique [0002] Propiconazole is a systemic triazole fungicide with protective and therapeutic effects. It has the characteristics of wide bactericidal spectrum, high activity, fast bactericidal speed, long-lasting effect, and strong systemic conductivity. It can effectively control Diseases caused by most higher fungi. At present, there are two routes for the synthesis of the original drug of propiconazole, that is, the first halogenation and then the cyclization process, and the first condensation and then the cyclization process. Generally, the intermediate 2,4-dichloroacetophenone, pentylene glycol, bromine, bromide, triazole, etc. are used as the main raw materials, and are prepared through cyclization, bromination, condensation, and purification. About 70%, the...

Claims

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Application Information

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IPC IPC(8): C01D3/18C07D405/06
CPCC01D3/18C07D405/06Y02P20/10
Inventor 李冬良马达飞王进曾挺潘光飞
Owner 浙江禾本科技股份有限公司
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