Environment-friendly refining method of theobromine

A refining method, theobromine technology, applied in the field of environmental protection theobromine refining, can solve problems such as incomplete reaction, increased refining steps and standing times, and affecting the quality of theobromine finished products, so as to reduce the residual rate and loss Effect

Inactive Publication Date: 2018-06-15
安徽省百花香料香精有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction of 3-methylxanthine in the process of producing theobromine through methylation reaction is incomplete, and the residual 3-methylxanthine in the crude product of theobromine is about 1-3%. At the same time, affected by trace impurities, theobromine products The appearance is yellow-green, which affects the quality of theobromine finished products
In order to meet the product quality standard, it is necessary to increase the refining steps and the number of standing times, resulting in an increase in the cost of theobromine products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Dissolving the crude product to make sodium salt: add 100g of theobromine crude product into 1000g of water, and slowly add 30% sodium hydroxide solution dropwise under stirring to completely dissolve the theobromine, then heat to 50-60°C and keep stirring for 10-60min. Filtrate while hot, filter out insoluble impurities, and take the filtrate;

[0023] (2) Decolorization: Add 8g of 100-mesh activated carbon to the filtrate obtained above, heat up to 70-80°C and heat-preserve and stir for 10-60min, filter while it is hot, and filter out the decolorizing agent to obtain the decolorizing solution;

[0024] (3) Acidification and crystallization: Cool the decolorizing solution to room temperature naturally, then add dropwise 5% hydrochloric acid solution to adjust the pH value to 9-10, accompanied by crystal precipitation, and transfer it to an environment of 0-5°C to seal and stand still. Filter when the production amount no longer increases, wash the filter cake 3 tim...

Embodiment 2

[0026] (1) Dissolving the crude product to make sodium salt: add 100g of theobromine crude product into 1000g of water, and slowly add 30% sodium hydroxide solution dropwise under stirring to completely dissolve the theobromine, then heat to 50-60°C and keep stirring for 10-60min. Filtrate while hot, filter out insoluble impurities, and take the filtrate;

[0027] (2) Decolorization: Add 8 g of decolorizing agent to the filtrate obtained above, heat up to 70-80° C. and keep stirring for 10-60 minutes, filter while it is hot, and remove the decolorizing agent to obtain the decolorizing solution;

[0028] (3) Acidification and crystallization: Cool the decolorizing solution to room temperature naturally, then add dropwise 5% hydrochloric acid solution to adjust the pH value to 9-10, accompanied by crystal precipitation, and transfer it to an environment of 0-5°C to seal and stand still. Filter when the production amount no longer increases, wash the filter cake 3 times with wate...

Embodiment 3

[0031] (1) Dissolving the crude product to make sodium salt: add 100g of theobromine crude product into 1000g of water, and slowly add 30% sodium hydroxide solution dropwise under stirring to completely dissolve the theobromine, then heat to 50-60°C and keep stirring for 10-60min. Filtrate while hot, filter out insoluble impurities, and take the filtrate;

[0032] (2) Decolorization: Add 8 g of decolorizing agent to the filtrate obtained above, heat up to 70-80° C. and keep stirring for 10-60 minutes, filter while it is hot, and remove the decolorizing agent to obtain the decolorizing solution;

[0033] (3) Acidification and crystallization: Cool the decolorizing solution to room temperature naturally, then add dropwise 5% hydrochloric acid solution to adjust the pH value to 9-10, accompanied by crystal precipitation, and transfer it to an environment of 0-5°C to seal and stand still. Filter when the production amount no longer increases, wash the filter cake 3 times with wate...

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Abstract

The invention discloses an environment-friendly refining method of theobromine, and relates to the technical field of synthetic chemistry. The method comprises the following steps: (1) dissolving a crude product to prepare a sodium salt; (2) carrying out decoloration; and (3) carrying out acidification and crystallization. According to the method provided by the invention, the theobromine in a theobromine crude product is converted into a sodium salt by adding a sodium hydroxide solution and insoluble impurities are filtered out; then, the decoloration effect is ensured by use of a decolorant,and pigment impurities are removed; and then, by controlling the pH value during acidification, the residual rate of theobromine in crystallization mother liquor can be reduced and the purity of theobromine in precipitated crystals can be increased. The prepared finished product of theobromine is white or creamy in appearance, and the residual rate of 3-methylxanthine is less than 0.15% or more,and meets requirements of the quality standard of theobromine; and the refining yield reaches 95% or more, thus reducing the loss amount of theobromine in a refining process.

Description

Technical field: [0001] The invention relates to the technical field of synthetic chemistry, in particular to an environment-friendly refining method of theobromine. Background technique: [0002] Theobromine, chemical name 3,7-dihydro-3,7-dimethyl-1H-purine-2,6-dione, is the main alkaloid in cocoa beans. Cocoa beans contain 1.5-3% theobromine, so theobromine is found in chocolate, kola nuts and tea. As a methylated xanthine, theobromine is a potent inhibitor of cyclic adenosine monophosphate phosphodiesterase, inhibiting the conversion of phosphodiesterase from the active cAMP to the inactive form, which is present in various metabolic systems second messenger. In addition, theobromine can be used as a starting material for the preparation of pentoxifylline, a derivative of methylxanthine, which is used to improve blood flow and treat intermittent claudication and vascular dementia. [0003] At present, the industrial production of theobromine at home and abroad is mainl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/10
CPCC07D473/10
Inventor 谢技
Owner 安徽省百花香料香精有限公司
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