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Purification method of high-safety hydroquinone composition

A purification method and high-safety technology, which is applied in the field of purification of hydroquinone compositions, can solve problems affecting the purity, quality, stability, appearance, appearance of hydroquinone and its products, affecting people's life safety, and damaging hemoglobin, so as to achieve high efficiency. Separation and detection, high sensitivity, good specificity

Active Publication Date: 2021-03-05
广东人人康药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

p-Benzoquinone is the main oxidative degradation product of hydroquinone, and it is easy to form colored complexes with hydroquinone, which in turn affects the purity, quality, stability and appearance of hydroquinone and its products.
In addition, hydroquinone will also introduce process impurities and by-products during its preparation, such as aniline
Aniline is a carcinogen, and it can also damage the hemoglobin that transports oxygen in the blood. Acute high exposure will cause dizziness, headache, irregular heartbeat, convulsions, coma and death, seriously affecting people's life safety

Method used

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  • Purification method of high-safety hydroquinone composition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0151] Example 1 The preparation of hydroquinone of the present invention

[0152] The preparation method of hydroquinone, comprises the steps:

[0153] 1) MnO 2 Add 280g, 430g of 98% sulfuric acid, and 2.0L of water into the reaction flask, slowly add 100g of aniline dropwise at 5-10°C, stir, and gradually raise the temperature to about 25°C until the reaction is complete. The reaction liquid is steam distilled at 60-90°C, and the collected p-benzoquinone condensate is introduced into another reaction flask;

[0154] 2) Under the condition of shading and nitrogen protection, add 42g of iron powder to the collected p-benzoquinone condensate, stir and react for 3-4 hours at 90-100°C, until the reaction is complete, filter, and depressurize the collected filtrate Concentrating to a hydroquinone content of 35% in the concentrated solution;

[0155] 3) Add 550mg of sodium metabisulfite, 2.2g of activated carbon, and 330mg of zinc powder to the concentrated solution, heat to ...

Embodiment 2

[0156] Example 2 The preparation of hydroquinone of the present invention

[0157] The preparation method of hydroquinone, comprises the steps:

[0158] 1) MnO 2 Add 350g, 500g of 98% sulfuric acid, and 2.0L of water into the reaction flask, slowly add 100g of aniline dropwise at 5°C-8°C, stir, and gradually raise the temperature to about 25°C until the reaction is complete. The reaction liquid is steam distilled at 60-90°C, and the collected p-benzoquinone condensate is introduced into another reaction flask;

[0159] 2) Under the conditions of shading and nitrogen protection, add 60g of iron powder to the collected p-benzoquinone condensate, stir and react for 2-3 hours at 90-100°C, until the reaction is complete, filter, collect the filtrate and concentrate under reduced pressure To the hydroquinone content in the concentrated solution is 25%;

[0160] 3) Add 750 mg of sodium pyrosulfite, 3.1 g of activated carbon, and 500 mg of iron powder to the concentrated solutio...

Embodiment 3

[0161] Example 3 The preparation of hydroquinone of the present invention

[0162] The preparation method of hydroquinone, comprises the steps:

[0163] 1) MnO 2 Add 250g, 370g of 98% sulfuric acid, and 2.5L of water into the reaction flask, slowly add 100g of aniline dropwise at 6-10°C, stir, and gradually raise the temperature to about 25°C until the reaction is complete. The reaction liquid is steam distilled at 70-95°C, and the collected p-benzoquinone condensate is introduced into another reaction flask;

[0164] 2) Under the conditions of shading and nitrogen protection, add 31g of iron powder to the collected p-benzoquinone condensate, stir and react at 90-100°C for 2-3 hours, until the reaction is complete, filter, collect the filtrate and concentrate it under reduced pressure to The content of hydroquinone in the concentrated solution is 30%;

[0165] 3) Add 550 mg of sodium pyrosulfite, 2.20 g of activated carbon, and 350 mg of zinc powder to the concentrated s...

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Abstract

The invention provides a purification method of a high-safety hydroquinone composition, wherein the method is characterized by comprising the following steps: 1) dissolving hydroquinone to be refinedin a crystallization solvent at the temperature of 80-100 DEG C to prepare a crystallization solution; and 2) adding a reducing agent into the prepared crystallization solution, stirring, separating,collecting the separation liquid, cooling, crystallizing, separating, collecting the crystal, and drying to obtain the product. The method has the advantages of simplicity and convenience in operation, good repeatability, suitability for industrial production, high yield, high purity and the like.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and in particular relates to a method for purifying a high-safety hydroquinone composition. Background technique [0002] As a tyrosinase inhibitor, hydroquinone (also known as hydroquinone) mainly inhibits tyrosinase activity through complexation, regulates the metabolic process of melanocytes, and significantly reduces the number of dopa-positive melanocytes in the epidermis, resulting in reversible Sexual skin discoloration. Oettel first proposed in 1936 that hydroquinone has the effect of whitening the skin. Since the 1960s, many countries have used hydroquinone as a whitening agent in cosmetics and in dermatology for the treatment of pigmentation, freckles and other external preparations. But the amount of hydroquinone must be strictly controlled. [0003] [0004] Hydroquinone is unstable and is susceptible to oxidative degradation reactions under the influence of environ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/34A61K8/34A61Q19/02C07C39/08C07C37/84C07C37/86C07C37/00A61K31/05A61P17/00
CPCA61K31/05A61K8/347A61Q19/02A61P17/00G01N30/06G01N30/34C07C37/84C07C37/86C07C37/002C07C46/00G01N2030/027A61K2800/782C07C39/08C07C50/04
Inventor 苏冠荣尹贝立
Owner 广东人人康药业有限公司
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