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Flusilazole-thiophanate methyl pesticide eutectic crystal and preparation method thereof

A technology of thiophanate-methyl and flusilazole, applied in botany equipment and methods, chemical instruments and methods, biocides, etc., can solve the problems of easy aggregation and precipitation, unstable storage of pesticides, etc., and achieve the goal of improving stability Effect

Inactive Publication Date: 2018-09-07
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The two are often used in combination to improve the efficacy of farmland pesticides, but the mixed pesticides are unstable during storage and tend to aggregate and precipitate

Method used

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  • Flusilazole-thiophanate methyl pesticide eutectic crystal and preparation method thereof
  • Flusilazole-thiophanate methyl pesticide eutectic crystal and preparation method thereof
  • Flusilazole-thiophanate methyl pesticide eutectic crystal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh the reactant flusilazole: thiophanate-methyl=1:1 molar ratio, and accurately weigh 0.5321g flusilazole and 0.5776g thiophanate-methyl in a 25ml crystallizer with an analytical balance;

[0028] Use a pipette gun to measure 4 mL of methanol and 12 mL of water into a crystallizer to form a suspension with a solute mass content of 6.95%. Stir at constant temperature and magnetic force for 2 h at 40°C.

[0029] After the stirring is stopped, the reaction solution is filtered, and the filtered product is dried in a vacuum oven at 40° C., and the obtained product is the pesticide eutectic of flusilazole and thiophanate-methyl.

[0030] The XRD pattern of the obtained product is as follows figure 1 Shown, is a pure eutectic, DSC shows its melting point is 128 °C.

Embodiment 2

[0032] Weigh the reactant flusilazole: thiophanate-methyl=1:1.05 molar ratio, and weigh 0.7526g flusilazole and 0.8579g thiophanate-methyl in a 25mL crystallizer with an analytical balance;

[0033] Use a pipette gun to measure 4 mL of methanol and 12 mL of water into a crystallizer to form a suspension with a solute mass content of 10.03%. Constant magnetic stirring at 30°C for 2.5h.

[0034] After the stirring is stopped, the reaction solution is filtered, and the filtered product is dried in a vacuum oven at 40° C., and the obtained product is the pesticide eutectic of flusilazole and thiophanate-methyl.

[0035] The XRD pattern of the obtained product is as follows figure 1 Shown, is a pure eutectic, DSC shows its melting point is 126 °C.

Embodiment 3

[0037] Weigh the reactant flusilazole: thiophanate-methyl=1:1.2 molar ratio, and weigh 0.8659g flusilazole and 1.1280g thiophanate-methyl in a 50mL crystallizer with an analytical balance;

[0038] Measure 10.2 mL of n-propanol and 30.6 mL of water into a crystallizer with a pipette gun to form a suspension with a solute mass content of 5%. Stir at constant temperature and magnetic force for 3 h at 27°C.

[0039] After the stirring is stopped, the reaction solution is filtered, and the filtered product is dried in a vacuum oven at 40° C., and the obtained product is the pesticide eutectic of flusilazole and thiophanate-methyl.

[0040] The XRD pattern of the obtained product is as follows figure 1 As shown, it is a pure eutectic, and DSC shows its melting point is 128°C.

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Abstract

The invention relates to a flusilazole-thiophanate methyl pesticide eutectic crystal and a preparation method thereof. The flusilazole-thiophanate methyl pesticide eutectic crystal has a series of characteristic peaks at 7.4+ / -0.2, 8.1+ / -0.2, 10.6+ / -0.2, 11.7+ / -0.2, 15.5+ / -0.2, 15.8+ / -0.2, 16.6+ / -0.2, 17.0+ / -0.2, 17.3+ / -0.2, 17.7+ / -0.2, 18.3+ / -0.2, 19.0+ / -0.2, 19.7+ / -0.2, 20.7+ / -0.2, 22.1+ / -0.2, 22.9+ / -0.2, 25.1+ / -0.2, 26.0+ / -0.2 and 26.8+ / -0.2 in a PXRD spectrogram, and the melting point of the eutectic crystal is 124-130 DEG C. The flusilazole-thiophanate methyl pesticide eutectic crystal isprepared by virtue of a solution-mediated transformation method or a grinding method. The pesticide eutectic crystal prepared by virtue of the preparation method has the beneficial effects that the melting point of flusilazole can be effectively increased, and the diversity of the dose forms of pesticides is enriched; and meanwhile, by virtue of mutual action force between two types of moleculesin a flusilazole-thiophanate methyl pesticide eutectic crystal structure, the stability of the pesticide eutectic crystal is higher than that of a common physically-blended mixture of two pesticides.

Description

technical field [0001] The invention belongs to the technical field of pesticide co-crystals, and in particular relates to a pesticide co-crystal of flusilazole and thiophanate-methyl and a preparation method thereof. Background technique [0002] According to statistics, in 2011, there were 17 types of pesticides with global annual sales exceeding US$500 million. Among these 17 types of pesticides, 14 types of raw materials were crystalline products. It can be seen that the quality of crystals is closely related to the quality of pesticides, and the crystal form is the essential factor determining the quality of pesticide crystals. During the crystallization process of pesticides, due to different pesticide processing processes, preparation methods, storage and application methods, the requirements for crystal quality are different. As far as different preparations are concerned, powders have higher requirements on the fineness, fluidity and bulk density of crystals, which...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/10C07C335/28A01N25/04
CPCC07F7/10A01N25/04C07C335/28
Inventor 龚俊波靳沙沙侯宝红杜世超
Owner TIANJIN UNIV
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