Continuous pyraclostrobin suspending agent preparation method

A technology of pyraclostrobin and suspending agent, which is applied in the field of preparation of pyraclostrobin suspending agent, can solve the problems of low utilization rate, achieve high utilization rate, significant progress, and good product performance

Active Publication Date: 2015-02-25
SHANDONG UNITED PESTICIDE IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of continuous operation to realize the preparation

Method used

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  • Continuous pyraclostrobin suspending agent preparation method

Examples

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Example Embodiment

[0039] Example 1: Preparation by the method of the present invention

[0040] 1: Take 100 grams of commercially available pyraclostrobin, add 5 grams of water, add 200 ml of methanol, heat up to 60 degrees, stir, pyraclostrobin is completely dissolved, slowly (cool down at a rate of 0.5 °C per minute, ) Cool down to 20 degrees, crystals will precipitate, continue to cool down to 0-5 degrees, and keep at 0-5 degrees for 4 hours;

[0041] 2: Keep heating at a rate of 5°C / min, heat up to 40°C, and the sample is partially undissolved, continue to cool down at a rate of 5°C / min; cool down to 0-5°C and hold for 4 hours.

[0042] 3: Repeat the operation of operation 2 for 3 times.

[0043] 4: After operation 3 is completed, the methanol is distilled off under reduced pressure until the methanol content of the residue is less than 1%, the vacuum degree is controlled to be less than 10 mmHg, and the temperature is not more than 45 degrees.

[0044] 5: After the distillation is compl...

Example Embodiment

[0046] Example 2: Preparation by the method of the present invention

[0047] 1: Take 100 grams of commercially available pyraclostrobin, add 20 grams of water, add 200 ml of methanol, heat up to 64 degrees, stir until pyraclostrobin is completely dissolved, slowly (cool down at a rate of 1°C per minute, ) Cool down to 10 degrees, crystals will precipitate, continue to cool down to 0-5 degrees, and keep at 0-5 degrees for 8 hours;

[0048] 2: Keep heating at a rate of 1°C / min, heat up to 45°C, and part of the sample is undissolved, continue to cool down at a rate of 1°C / min; cool down to 0-5°C and hold for 10 hours.

[0049] 3: Repeat the operation of operation 2 for 5 times.

[0050] 4: After operation 3 is completed, the methanol is distilled off under reduced pressure until the methanol content of the residue is less than 0.5%, the vacuum degree is controlled to be less than 20 mmHg, and the temperature is not more than 30 degrees.

[0051] 5: After the distillation is ...

Example Embodiment

[0053] Example 3: Preparation by the method of the present invention

[0054] 1: Take 100 grams of commercially available pyraclostrobin, add 2 grams of water, add 200 ml of methanol, heat up to 40 degrees, stir, pyraclostrobin is completely dissolved, slowly (cool down at a rate of decreasing 5 degrees per minute, ) Cool down to 20 degrees, crystals will precipitate, continue to cool down to 0-5 degrees, and keep at 0-5 degrees for 10 hours;

[0055] 2: Keep heating at a rate of 0.5°C / min, heat up to 30°C, and the sample is partially undissolved, continue to cool down at a rate of 2°C / min; cool to 0-5°C for 24 hours.

[0056] 3: Repeat the operation of operation 2 for 2 times.

[0057] 4: After operation 3 is completed, the methanol is distilled off under reduced pressure until the methanol content of the residue is less than 2%, the vacuum degree is controlled to be less than 20 mmHg, and the temperature is not more than 30 degrees.

[0058] 5: After the distillation is co...

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Abstract

The invention belongs to the technical field of suspending agent preparation, and particularly relates to a continuous pyraclostrobin suspending agent preparation method and application of the same in plant protection. The preparation method includes dissolving pyraclostrobin in an alcohol-water solution, wherein alcohols solvents are methanol, alcohol, propanol and isopropanol, weight ratio of alcohol and water is 100:1-10, and quantity of added alcohol-water meets the condition that pyraclostrobin can be dissolved completely at temperature of 40-64 DEG C. Utilization rate of currently-commercial pyraclostrobin which is input reaches 100%, so that freeness of loss is realized, and utilization rate is high. The pyraclostrobin suspending agent prepared by the method is good in performance and low in cost.

Description

technical field [0001] The invention belongs to the technical field of suspension concentrate preparation, and in particular relates to a continuous preparation method of pyraclostrobin suspension concentrate. Background technique [0002] Patent CN101203136B describes that currently commercialized pyraclostrobin is a kind of amorphous pyraclostrobin. Due to its low melting point, in the process of preparing suspending agent, the grinding equipment is blocked due to its viscosity, so it is not too difficult. The currently commercially available pyraclostrobin can be prepared into a suspension by conventional methods. [0003] Patent CN101203136B proposes a preparation method of a new crystal form. By further processing the currently commercialized pyraclostrobin through crystallization method, pyraclostrobin suitable for the preparation of suspensions is obtained, while the current pyraclostrobin The quality of kresoxim-methyl has reached 97.5%. This treatment method will c...

Claims

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Application Information

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IPC IPC(8): A01N25/04A01N47/24A01P1/00A01P3/00
Inventor 唐剑峰刘杰刘振邦李凝牛芳宿景池
Owner SHANDONG UNITED PESTICIDE IND CO LTD
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