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Cyhalofop-butyl powder and preparation method thereof

A technology of cyhalofop-fop and powder, which is applied in the field of cyhalofop-powder and its preparation, can solve the problems of inconvenient use of cyhalofop-like solid wax, and achieve the effects of easy storage, high content and easy use

Inactive Publication Date: 2009-03-04
HUNAN GOFAR FINE CHEM IND TECH CO LDT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, it is very inconvenient for customers to use cyhalofop, whether it is oily or waxy solid

Method used

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  • Cyhalofop-butyl powder and preparation method thereof
  • Cyhalofop-butyl powder and preparation method thereof
  • Cyhalofop-butyl powder and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: Synthesize cyhalofop oil according to the conventional method, and the measured specific gravity is 113 grams per 100 milliliters. Add 50ml of the oily substance to 100ml of hexane and mix it at a stirring speed of 200 rpm. Use an external circulation cold pump to cool the mixture. As the temperature of the mixed solution continues to decrease, a large amount of crystals will precipitate out. When the temperature of the mixed solution reaches minus 10°C After keeping stirring for 30-60 minutes, filter with a suction filter funnel, and put the obtained solid into a vacuum desiccator for vacuum drying (at room temperature) to constant weight. A mixed powder of cyhalofopin amorphous and crystal was obtained, and the measured bulk density was 43.7 g / 100 ml. After (HPLC) analysis and quantification by external standard method, the purity is 99.4%.

Embodiment 2

[0019] Example 2: 200ml of cyhalofop oil was added to 600ml of heptane to mix, the stirring speed was 100 rpm, and the mixture was cooled by an external circulation cold pump, and a large amount of crystals were precipitated as the temperature of the mixed solution continuously decreased. After the temperature of the liquid reaches minus 5°C and keeps stirring for 30-60 minutes, filter with a suction filter funnel, and put the obtained solid into a vacuum desiccator for vacuum drying (at room temperature) to constant weight. The mixed powder of amorphous and crystalline cyhalofop was obtained, and the measured bulk density was 44.1 g / 100 ml. After (HPLC) analysis and quantification by external standard method, the purity is 99.3%.

Embodiment 3

[0020] Example 3: 500ml of cyhalofop oil was added to 1500ml of petroleum ether and mixed, the stirring speed was 85 rpm, and the mixture was cooled by an external circulation cold pump. As the temperature of the mixed solution continued to decrease, a large amount of crystals were precipitated. After the temperature of the liquid reaches 0°C and keeps stirring for 30-60 minutes, filter with a suction filter funnel, and put the obtained solid into a vacuum desiccator for vacuum drying (at room temperature) to constant weight. The mixed powder of amorphous and crystalline cyhalofop was obtained, and the measured bulk density was 44.3 g / 100 ml. After (HPLC) analysis and quantification by external standard method, the purity is 99.1%.

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Abstract

The invention provides a cyhalofop-butyl powder which is a formless crystallization mixed powder, with bulk density being 43.0g / 100ml-45.0g / 100ml and purity quotient being over 99 percent. The preparation method comprises the following steps: mixing a cyhalofop-butyl oily substance and a chain alkane compound, cooling the mixture in the process of stirring, so as to enable cyhalofop-butyl to separate out in the form of formless crystallization mixed powder, filtering, and vacuum drying to acquire the cyhalofop-butyl powder. The cyhalofop-butyl powder has the advantages of high content, easy storage, and convenient use.

Description

technical field [0001] The invention relates to a cyhalofop-ethyl powder and a preparation method thereof. Background technique [0002] The chemical name of cyhalofop-ethyl: (R)-2-[4-(4-cyano-2-fluorophenoxy)phenoxy]butyl propionate, molecular formula: C20H20FN04, structural formula as follows: [0003] [0004] It is an excellent special herbicide for paddy fields. [0005] In "ThePesticideManual12thed.2000.223", (R)-2-[4(4-cyano-2-fluorophenoxy)phenoxy]-butyl propionate (cyhalofop-ester) is described, its physical and chemical properties: The pure product is white crystal with a relative density of 1.172. It does not indicate that it has other states. [0006] In U.S. Patents: US4897481 and US4894085: (R)-2-[4(4-cyano-2-fluorophenoxy)phenoxy]-butyl propionate (cyhalofop-ester) synthesized by the description is A viscous oil. [0007] In "Pesticide Research and Application" 2007 No. 1: "Synthesis of Cyhalofop-methyl" published by Luo Liangming of Hunan Research Ins...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A01N37/34A01N25/12A01P13/00
Inventor 黄榕
Owner HUNAN GOFAR FINE CHEM IND TECH CO LDT