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Method of preparing alpha-chlorothalonil

A technology of chlorothalonil and mixture, which is applied in the field of pesticide preparation, can solve the problems of high equipment and operation requirements, imperfect detection methods, high equipment investment, etc., and achieve the effects of low energy consumption and investment, simple operation, reliable and stable quality

Active Publication Date: 2009-02-18
溧阳常大技术转移中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process not only requires high energy consumption and equipment investment, but also requires high equipment and operation requirements; at the same time, due to the imperfect detection method, the product is likely to carry a small amount of untransformed chlorothalonil residue

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Put 20 grams of chlorothalonil-based materials based on β-type chlorothalonil in a four-necked round-bottomed flask with a volume of 150 ml equipped with a reflux condenser, a stirrer, a thermometer and a sampling port with a ground plug. Inject absolute ethanol into the sampling port. The amount of absolute ethanol injected is just enough to submerge the chlorothalonil material. The flask assembly was placed in a constant temperature bath and heated until a small amount of solvent reflux occurred (reflux temperature about 78° C.), at which point stirring was started and timing was started. Every two hours, stop stirring, open the sampling port, and use a sampler with a semi-fused glass filter plate to take out part of the wet solid phase sample from the bottom of the flask for testing. Return the liquid phase remaining in the sampler when sampling to the flask. After sampling, continue to start stirring. After the wet solid phase sample was dried in a vacuum drying ...

Embodiment 2

[0024] Put 20 grams of chlorothalonil-based materials based on β-type chlorothalonil in a four-necked round-bottomed flask with a volume of 150 ml equipped with a reflux condenser, a stirrer, a thermometer and a sampling port with a ground plug. Inject toluene into the sampling port. The amount of toluene injected is just enough to submerge the chlorothalonil material. The flask assembly was placed in a constant temperature bath and heated until a small amount of solvent reflux occurred (reflux temperature about 111° C.), at which point stirring was started and timing was started. Sampling time and processing method are identical with embodiment one. After the wet solid phase sample was dried in a vacuum oven with a maximum temperature of 80° C., the characteristic peak of β-type chlorothalonil was detected by X-ray powder diffraction method (2-theta=26.5±0.1°). The characteristic peak of β-type chlorothalonil in the first sampling has disappeared. No characteristic peak of...

Embodiment 3 7

[0026] The experimental condition of embodiment three-seven is identical with embodiment one.

[0027] The experimental conditions different from Example 1 are listed in the table below.

[0028] Example number

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PUM

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Abstract

A process for preparing alpha-chlorothalonil includes such steps as loading the raw chlorthalonil into a container, filling solvent, stirring or adding more solvent, adding alpha-chlorothalonil powder as crystal seeds, transform reaction at temp lower than 150 deg.C, and vacuum drying.

Description

technical field [0001] The present invention relates to pesticide preparation technology, in particular to a method for preparing α-type chlorothalonil through transformation using chlorothalonil containing other configurations as raw materials. Other configurations of chlorothalonil refer to β-type (type 2) , 3-type chlorothalonil or a mixture of β-type (2-type) and 3-type chlorothalonil. The invention is particularly suitable for transforming chlorothalonil produced by a gas-phase chlorination method into alpha-type chlorothalonil with isophthalonitrile as a raw material. Background technique [0002] The English name of chlorothalonil is 2, 4, 5, 6-Tetrachloro-1, 3-benzenedicarbonitile, and its English trade name is Chlorothalonil. The α-type chlorothalonil referred to in the present invention is: the isomer stable at low temperature among the three isomers of chlorothalonil. For detailed information, see: Document 1: α-type in "Thermochimica Acta 428 (2005) 19-23"; Doc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/51C07C253/32A01N29/10
Inventor 席海涛朱方平杜晓刚顾浩
Owner 溧阳常大技术转移中心有限公司
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