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A kind of purification method of methylene blue

A purification method and methylene blue technology, applied in the direction of organic chemistry, etc., can solve the problems of difficult quality control of high-purity methylene blue, and achieve the effect of general and easy method, large operation plasticity and high purity.

Active Publication Date: 2020-06-19
SHANGHAI WOKAI BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] The purpose of the present invention is to prepare a kind of methylene blue with high content, adopt the method of zinc removal with sodium bicarbonate and sodium carbonate mixed precipitant, provide a kind of methylene blue with wide reaction conditions, high purity, high yield and good quality stability The purification method of blue, to solve the difficult problem of the quality control of preparing high-purity methylene blue in the prior art

Method used

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  • A kind of purification method of methylene blue
  • A kind of purification method of methylene blue
  • A kind of purification method of methylene blue

Examples

Experimental program
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Effect test

Embodiment 1

[0029] A purification method of methylene blue:

[0030] Add 150g of raw salt-based lake blue BB, add 2250g of water, and when heated to 60~90℃, gradually add a mixed solution of sodium bicarbonate and sodium carbonate under stirring (40g sodium bicarbonate plus 0.8g sodium carbonate, dissolved in 500ml water), Control the pH of the reaction solution at 7.5-9, add it in about 30 minutes, keep it for 30 minutes, and pass it into the crystallization tank through a filter. 75 g of hydrochloric acid was added to the filtrate, and after stirring for 15 minutes, it was allowed to cool to precipitate bright dark green crystals. The crystals were centrifuged and dried to obtain 64.1 g of methylene blue, the content was greater than or equal to 98.5%, and the yield was 90.7%. The results meet the requirements of the Pharmacopoeia and are far higher than the analytical methylene blue content index.

Embodiment 2

[0032] A purification method of methylene blue:

[0033] Add 150g of raw salt-based lake blue BB, add 1950g of water, and when heated to 60~90℃, gradually add a mixed solution of sodium bicarbonate and sodium carbonate under stirring (40g sodium bicarbonate plus 0.04g sodium carbonate, dissolved in 500ml water), Control the pH of the reaction solution at 7.5-9, add it in about 30 minutes, keep it warm for 60 minutes, and enter the crystallization tank through a filter. 60 g of hydrochloric acid was added to the filtrate, and after stirring for 15 minutes, it was allowed to cool to precipitate bright dark green crystals. The crystals are centrifuged and dried to obtain 63.6 g of methylene blue, the content is greater than or equal to 98.6%, and the yield is 90%. The results meet the requirements of the Pharmacopoeia and are far higher than the analytical methylene blue content index.

Embodiment 3

[0035] A purification method of methylene blue:

[0036] Add 150g of raw salt-based lake blue BB, add 2400g of water, and when heated to 60~90℃, gradually add a mixed solution of sodium bicarbonate and sodium carbonate under stirring (52.5g sodium bicarbonate plus 0.8g sodium carbonate, dissolved in 500ml water) , Control the pH of the reaction solution at 7.5-9, add it in about 30 minutes, keep it for 100 minutes, pass the filter into the crystallization tank. Add 90 g of hydrochloric acid to the filtrate, and after stirring for 15 minutes, it was allowed to cool to precipitate shiny dark green crystals. The crystals were centrifuged and dried to obtain 64.5 g of methylene blue, the content was greater than or equal to 98.5%, and the yield was 91.3%. The results meet the requirements of the Pharmacopoeia and are far higher than the analytical methylene blue content index.

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Abstract

The invention relates to the technical field of biological dyeing reagent synthesis and purification, in particular to a methylene blue purification method. The methylene blue purification method includes: allowing zinc chloride in dye methylene blue BB to have replacement reaction with the mixture of sodium bicarbonate and sodium carbonate to generate water-fast zinc carbonate, filtering to remove the zinc carbonate precipitate, adding concentrated hydrochloric acid into the filtrate to separate out needle crystals, filtering to obtain the crystals, performing centrifuge dripping, and dryingto obtain the bright green methylene blue needle crystals. The method has the advantages that the method using the mixture of sodium bicarbonate and sodium carbonate to remove zinc is used, and the method is universal, practicable, sufficient in raw material, high in operation flexibility and simple in operation.

Description

Technical field [0001] The invention relates to the field of synthesis and purification of biological staining reagents, and the specific field is a purification method of high-purity methylene blue. Background technique [0002] Methylene blue is also known as methylene blue, tetramethyl blue, and salt-based lake blue. [0003] The structural formula is: [0004] [0005] Methylene blue is a bright dark green needle-like crystal, soluble in water, slightly soluble in ethanol, and the solution is sky blue. [0006] Methylene blue is widely used. It is used as a nuclear stain in histology, in vivo staining of nerve tissue, and as a blood stain together with eosin. It is used as a bactericide, antidote, a redox indicator in chemical analysis, and an adsorption indicator. Reagents, and the determination of various metals such as mercury and tin. [0007] Analytical pure methylene blue is purified by removing zinc from industrial dye salt-based lake blue BB as the main raw material. [000...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D279/20
CPCC07D279/20
Inventor 薛循育柯德宏王涛戴林荣
Owner SHANGHAI WOKAI BIOTECH
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