Preparation method of small-particle-size benzoyl peroxide

A technology of benzoyl peroxide and small particle size, which is applied in the preparation of peroxide compounds, organic compounds, chemical instruments and methods, etc., to achieve the effect of accelerating the stirring rate and reducing the crystallization temperature

Active Publication Date: 2021-08-06
RUYUAN HEC PHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN201610246064.9 discloses a chemical preparation method of micronized benzoyl peroxide, mainly by dissolving benzoyl peroxide and mixing it with a diluent, and using different physical and chemical properties between solvents to obtain micronized powder The benzoyl peroxide method is used to control its particles below 50 μm, but diluents need to be introduced in the production process. Since the pharmacopoeia stipulates that the moisture content of peroxide is between 20% and 30%, there are restrictions on the drug crystallization solvent , so this method has limitations in practical application

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  • Preparation method of small-particle-size benzoyl peroxide

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Embodiment 1

[0029]

[0030] Synthesis of crude benzoyl peroxide: Add SDS (0.3g) and water (700g) to a 1000mL reaction flask equipped with mechanical stirring at room temperature, stir to dissolve, then add solid sodium hydroxide (34.14g), stir to dissolve And lower the temperature; add hydrogen peroxide solution (56.6g) dropwise between 0-5°C for 20 minutes, then keep warm and stir for 1.0h after dropping; keep warm and add benzoyl chloride (100g) dropwise between 0-5°C for about 30min After the dropwise addition, keep warm and continue to stir for 2 hours; stop stirring after 2 hours of reaction, filter under reduced pressure, rinse the product with water (300mL) until the filtrate is neutral. The wet product was drained as much as possible, and the solid benzoyl peroxide crude product weighed 71.5g white powder.

[0031] Refining benzoyl peroxide: Add crude BPO (71.5g) and acetone (350g) in turn to a 1000mL reaction bottle, heat to 35°C under stirring, and the solution becomes clear;...

Embodiment 2

[0033] Refining benzoyl peroxide: add crude BPO (70g) and acetone (350g) in turn to a 1000mL reaction flask, heat to 40°C under stirring, and the solution becomes clear; Add dropwise to aqueous potassium solution (1051g), and the dropwise addition is completed in about 30 minutes. Stir at -10°C for 30 minutes, and prepare for suction filtration; filter under reduced pressure, rinse the product with water (300g), and drain to obtain 119g of white powder. The detected particle size D90<5μm.

Embodiment 3

[0035] Refining benzoyl peroxide: Add crude BPO (70g) and acetone (560g) in sequence to a 1000mL reaction flask, heat to 25°C under stirring, and the solution becomes clear; Add dropwise to an aqueous potassium solution (1200g), and the dropwise addition is completed in about 35 minutes. Stir at -15°C for 30 minutes and prepare for suction filtration; filter under reduced pressure, rinse the product with water (300g), and drain to obtain 125g of white powder. The detected particle size D90<5μm.

[0036] The particle diameter result that the embodiment of the present invention draws is as follows:

[0037] Example D10 / μm D50 / μm D90 / μm Example 1 0.364 0.879 1.939 Example 2 0.389 0.998 3.374 Example 3 0.404 0.895 2.880

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Abstract

The invention provides a preparation method of small-particle-size benzoyl peroxide, which comprises the following steps: dissolving lauryl sodium sulfate and sodium hydroxide in water, dropwise adding hydrogen peroxide at a low temperature, stirring and mixing uniformly while keeping the temperature, dropwise adding benzoyl chloride after the temperature is constant, and keeping the temperature for continuous reaction after dropwise adding; after the reaction is completed, filtering under reduced pressure, and leaching with water to be neutral to obtain a benzoyl peroxide crude product; and dissolving the benzoyl peroxide crude product in acetone, heating and stirring until the solution is clear, dropwise adding the solution into an inorganic salt aqueous solution, carrying out heat-preservation stirring, and filtering to obtain small-particle-size benzoyl peroxide. The minimum particle size is achieved by improving the crystallization method, the water solution is adopted as the crystallization solvent, the water content specified by pharmacopeia can be met, and the prepared small-particle-size benzoyl peroxide is beneficial to improvement of the curative effect of the preparation.

Description

technical field [0001] The invention relates to the technical field of medicinal chemistry, in particular to a preparation method of benzoyl peroxide with a small particle size. Background technique [0002] Benzoyl peroxide is a compound containing peroxy bonds, which belongs to organic peroxides. It is a strong oxidizing agent, extremely unstable and flammable. It can explode when impacted, heated and rubbed, and burn when sulfuric acid is added. Generally, benzoyl peroxide produced industrially is snowball-sized particles with a diameter of 0.01-0.5 cm; or salt-sized particles with a diameter of 60-150 μm. If benzoyl peroxide with such particle size is used in gel or cream, there must be problems with the particle size, and the particle size must be pulverized to less than 50 μm by pulverization. However, when benzoyl peroxide is pulverized , easy to generate friction or heat up, so it is easy to explode, leading to safety accidents. [0003] However, with the rapid de...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C407/00C07C409/34
CPCC07C407/00C07C407/003C07C409/34
Inventor 徐形典林德章贺江华张志勇陈磊杨波葛玉聪
Owner RUYUAN HEC PHARM
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