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A kind of catalyst for preparing chlorothalonil and its preparation method and application

A catalyst, chlorothalonil technology, applied in the preparation of chlorothalonil catalyst and its preparation field, can solve the problems of poor activity, poor selectivity, and low conversion rate of domestic catalysts, achieve good promotion and application value, improve performance, and prepare The effect of simple method

Active Publication Date: 2020-05-12
JIANGSU XINHE AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a catalyst for preparing chlorothalonil and its preparation method and application in order to overcome the problems of poor activity, poor selectivity and low conversion rate of domestic catalysts.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Catalyst preparation

[0023] 165gFeCl 3 , 94.5gCuCl2, 89gCaCl2 and 15gCsCl were added to a solution containing 50ml of concentrated hydrochloric acid and 1450ml of distilled water, and 1500g of 15-60 mesh coconut shell activated carbon was added, stirred and heated, soaked at 90°C until dry, and then dried at 120°C for 24 hours. That is, the required catalyst is obtained.

[0024] Chlorination of isophthalonitrile

[0025] Fill 200g of the prepared catalyst into a fluidized bed reactor, pass nitrogen gas at 120°C, gas velocity 0.11m / s, dry for 4 hours, then pass chlorine gas at 260°C, activate at 40g / h for 6 hours , according to the ratio of isophthalonitrile: chlorine: nitrogen = 1:2.5:2.5 (mass ratio), the mixed gas is passed into the reactor, and the temperature is controlled at 300 ° C to react to obtain chlorothalonil, and the molar yield of chlorothalonil is The rate is 98.1%.

Embodiment 2

[0027] Catalyst preparation

[0028] 165gFeCl 3 , 108gCuCl2, 89gCaCl2 and 7.5gKCl were added together to a solution containing 50ml of concentrated hydrochloric acid and 1450ml of distilled water, and 1500g of 15-60 mesh coconut shell activated carbon was added, stirred and heated, soaked at 90°C until dry, and then dried at 120°C for 24 hours. That is, the required catalyst is obtained.

[0029] Chlorination of isophthalonitrile

[0030] Fill 200g of the prepared catalyst into a fluidized bed reactor, pass nitrogen gas at 120°C, gas velocity 0.11m / s, dry for 4 hours, then pass chlorine gas at 260°C, activate at 40g / h for 6 hours , according to the ratio of isophthalonitrile: chlorine: nitrogen = 1:2.5:2.5 (mass ratio), the mixed gas is passed into the reactor, and the temperature is controlled at 300 ° C to react to obtain chlorothalonil, and the molar yield of chlorothalonil is The rate is 98.4%.

Embodiment 3

[0032] Catalyst preparation

[0033] 165gFeCl 3 , 81gCuCl2, 78gCaCl2 and 6gNaCl were added together to a solution containing 50ml of concentrated hydrochloric acid and 1450ml of distilled water, 1500g of 15-60 mesh coconut shell activated carbon was added, stirred and heated, soaked at 90°C until dry, and then dried at 120°C for 24 hours, that is obtain the required catalyst.

[0034] Chlorination of isophthalonitrile

[0035] Fill 200g of the prepared catalyst into a fluidized bed reactor, pass nitrogen gas at 120°C, gas velocity 0.11m / s, dry for 4 hours, then pass chlorine gas at 260°C, activate at 40g / h for 6 hours , according to the ratio of isophthalonitrile: chlorine: nitrogen = 1:2.5:2.5 (mass ratio), the mixed gas is passed into the reactor, and the temperature is controlled at 300 ° C to react to obtain chlorothalonil, and the molar yield of chlorothalonil is The rate is 98.3%.

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PUM

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Abstract

The invention relates to a catalyst for preparation of chlorothalonil, a preparation method and application thereof. Activated carbon is adopted as the carrier, the main active substance is FeCl3, the auxiliary active substances are chlorides of Cu and Ca and at least one of Na, K or Cs, wherein the molar ratio of Fe, Cu and Ca is 1:0.1-0.8:0.1-0.9, the mole ratio of Fe to Na, K or Cs is 1:0.01-0.3, and the main active substance and auxiliary active substances account for 5-20wt% of the total catalyst. The catalyst can be used in a high temperature chlorination reaction fluidized for preparation of chlorothalonil from isophthalonitrile. Compared with the prior art, the catalyst provided by the invention has the advantages of high chlorothalonil yield and high content, simple preparation process, low cost and long service life, and can be used for industrial production.

Description

technical field [0001] The invention relates to a pesticide catalyst, in particular to a catalyst for preparing chlorothalonil, a preparation method and application thereof. Background technique [0002] Chlorothalonil is a high-efficiency, low-toxicity, broad-spectrum, low-residue protective fungicide, which is widely used in the control of fungal diseases in agriculture and forestry, especially in vegetables, fruits and other economic crops. According to Japanese data, chlorothalonil can prevent and control fifty-two diseases of more than thirty kinds of crops. In addition, chlorothalonil also has important uses in the anti-mold industry, such as the manufacture of anti-mold paint, anti-mold wallpaper, anti-mold of electrical appliances, and anti-mold of apples and wood. The production scale of chlorothalonil in China is constantly expanding, and it has become one of the high-quality large-tonnage pesticide varieties in the world. [0003] Chlorothalonil is an important ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/138C07C253/30C07C255/50
CPCB01J27/138B01J37/0201C07C253/30C07C255/50
Inventor 李强王海波胡清禚文峰
Owner JIANGSU XINHE AGROCHEM