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A crystallization treatment method for improving the product quality of mesotrione

A technology for mesotrione and crystallization treatment, applied in the directions of organic chemistry methods, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of increased production costs, low fluidity of powder products, and increased bulk density, etc. The effect of improving bulk density, large particle size and reducing moisture content

Active Publication Date: 2022-05-31
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although powdering and drying can increase the quantitative content of the product, it not only increases the production cost, but also the lower fluidity and bulk density of the powdered product will also increase the transportation cost of the product

Method used

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  • A crystallization treatment method for improving the product quality of mesotrione
  • A crystallization treatment method for improving the product quality of mesotrione
  • A crystallization treatment method for improving the product quality of mesotrione

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Step 1, seed crystal preparation process:

[0049] 1) Take 16g of the powder raw material product and add it to a 250mL crystallizer filled with 100g of dichloroethane solvent;

[0050] 2) Warm up to 55°C to dissolve the liquid, and the stirring speed is 250rpm;

[0051] 3) Cool down to 15°C at a uniform speed within 120 minutes;

[0052] 4) Cultivate crystals at a constant temperature for 5 hours at 15°C, filter, and dry to obtain 9.8 g of seed crystals;

[0053] Step 2, crystallization process strengthening:

[0054] 1) Take 340gm of organic mother liquor (mass concentration is about 0.16), add 5.1g of acidic activated carbon powder, and stir for 60min in an oil bath at 55°C at a stirring speed of 250rpm;

[0055] 2) Use a preheated round-bottomed flask and funnel to filter the decolorized mother liquor, quickly place the filtered mother liquor in a crystallizer whose temperature is controlled by an ice machine at 55°C, and program to cool down to 45°C within 60 mi...

Embodiment 2

[0063] Step 1, seed crystal preparation process:

[0064] 1) Take 14g of the original powder product and add it to a 250mL crystallizer filled with 100g dichloroethane solvent;

[0065] 2) Warm up to 50°C to dissolve the liquid, and the stirring rate is 200rpm;

[0066] 3) Cool down to 10°C at a uniform speed within 240 minutes;

[0067] 4) Cultivate crystals at a constant temperature for 3 hours at 10°C, filter, and dry to obtain 8.7 g of seed crystals;

[0068] Step 2, crystallization process strengthening:

[0069] 1) Take 329gm of organic mother liquor (mass concentration is about 0.17), add 3.3g of acidic activated carbon powder, and stir for 20min in an oil bath at 50°C at a stirring speed of 200rpm;

[0070] 2) Use a preheated round-bottomed flask and funnel to filter the decolorized mother liquor, quickly place the filtered mother liquor in a crystallizer whose temperature is controlled by an ice machine at 50°C, and program to cool down to 40°C within 20 minutes; ...

Embodiment 3

[0078] Step 1, seed crystal preparation process:

[0079] 1) Take 15g of the original powder product and add it into a 250mL crystallizer filled with 100g dichloroethane solvent;

[0080] 2) Warm up to 53°C to dissolve the liquid, and the stirring speed is 230rpm;

[0081] 3) Cool down to 13°C at a uniform speed within 120 minutes;

[0082] 4) Cultivate crystals at a constant temperature for 4 hours at 13°C, filter, and dry to obtain 9.1 g of seed crystals;

[0083] Step 2, crystallization process strengthening:

[0084] 1) Take 247.4gm of organic mother liquor (mass concentration is about 0.17), add 3.7g of acidic activated carbon powder, and stir for 40min in an oil bath at 53°C at a stirring speed of 230rpm;

[0085] 2) Use a preheated round bottom flask and funnel to filter the decolorization mother liquor, quickly place the filtered mother liquor in a crystallizer whose temperature is controlled by an ice machine at 53°C, and program to cool down to 43°C within 40 minu...

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Abstract

The invention provides a crystallization treatment method for improving the product quality of mesotrione, which mainly includes two steps of seed crystal preparation process and crystallization process strengthening. Seed crystal preparation process: use dichloroethane solvent system to recrystallize mesotrione solid powder, grow crystals at constant temperature, filter and dry to obtain mesotrione seed crystals; crystallization process enhancement: decolorize mesotrione with activated carbon The organic mother liquor of oxalone is cooled to the metastable zone by programming, and the prepared sieved seed crystals are added, and crystal growth, programming cooling, crystal growth, filtration, rinsing and drying are performed to obtain mesotrione crystals. Through the crystallization method in the present invention, the moisture content of mesotrione is reduced to 3% to 6%, and the bulk density of the product reaches 0.75g / cm 3 ~0.85g / cm 3 , the quantitative content of the product is increased to more than 98.0%, the main particle size can reach 300μm-500μm, and it has good fluidity.

Description

technical field [0001] The invention belongs to the technical field of pesticide crystallization, and in particular relates to a crystallization treatment method for improving the product quality of mesotrione. Background technique [0002] Mesotrione, also known as Mesotrione, belongs to the class of preemergence and postemergence broad-spectrum selective herbicides that inhibit hydroxyphenylpyruvate dioxygenase (HPPD), and are effective against major broadleaf Grasses and some grasses. Molecular formula is C 14 h 13 NO 7 S, the molecular weight is 339.32, and the chemical name is 2-(4-methylsulfonyl)-2-nitrobenzoyl-cyclohexane-1,3-dione. The chemical structural formula is: [0003] [0004] Mesotrione is a triketone herbicide first developed by Syngenta. It was launched in Europe in 2001 under the trade name Callisto. The synthetic reaction of mesotrione is relatively mature, and the synthetic route is: using 4-thiamphenicol-2-nitrobenzoic acid as raw material, d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C317/24C07C315/06
CPCC07C315/06C07C2601/14C07B2200/13C07C317/24
Inventor 龚俊波万旭兴吴送姑王磊杜世超倪肖元尚丽霞汤伟伟吴坤石鹏乔振
Owner TIANJIN UNIV
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