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Method for extracting ferulic acid, p-coumaric acid and pentosan from corn husks

A technology of corn husk and ferulic acid, applied in oligosaccharides, chemical instruments and methods, separation/purification of carboxylic acid compounds, etc. problem, to achieve the effect of good economic benefits, short production cycle and low solvent consumption

Inactive Publication Date: 2012-03-21
刘启民
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent 200810029566.1 is a preparation method of trans-ferulic acid, p-coumaric acid and pentosan, which is relatively sufficient in the comprehensive utilization of corn bran, but it is difficult to extract and refine p-coumaric acid and ferulic acid. Adopt resin method, because the resin exchange of unit mass or the amount of adsorption organic phenolic acid are less, thereby industrialized production processing ability is weak, and the production cycle such as the elution regeneration of resin is long, and the consumption of organic solvent (alcohol) is also bigger (this The ethanol solution used for eluting in the patent is a hundred times the volume of the resin), which generally leads to high costs for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 1. Add 100 kg of corn husks at room temperature, add 1000 kg of 0.6% sodium hydroxide solution, and then add 300 g of sodium hydrosulfite, stir and soak for 8 hours under the action of ultrasound with a power of 8 kW. After filtering, the filtrate was neutralized to pH=4 with dilute sulfuric acid, and the solution became cloudy. The solution was concentrated in vacuo to 60 liters, 10 liters of ethyl acetate was added, the layers were separated after vigorous stirring, and the p-coumaric acid was extracted into the ethyl acetate phase, and extracted twice. The extracted aqueous phase is used for later use. The two extracted ethyl acetate phases were combined to a total of about 20 liters, concentrated in vacuo to 2 liters, and 10 liters of high-boiling point petroleum ether was added to precipitate p-coumaric acid. The precipitate was collected by filtration and dried to obtain 700 grams of crude p-coumaric acid, which was recrystallized with 20% dilute alcohol to obtai...

Embodiment 2

[0020] 1. Add 2000 kg of 0.6% sodium carbonate solution to 100 kg of corn husks at room temperature, then add 300 g of sodium sulfite powder, and stir and soak for 3 hours under the action of ultrasound with a power of 8 kW. After filtration, the filtrate was neutralized to pH=4 with dilute hydrochloric acid, and the solution became cloudy. The solution was concentrated in vacuo to 60 liters, 10 liters of ethyl acetate was added, the layers were separated after vigorous stirring, and the p-coumaric acid was extracted into the ethyl acetate phase, and extracted twice. The extracted aqueous phase is used for later use. The two extracted ethyl acetate phases were combined to a total of about 20 liters, concentrated in vacuo to 2 liters, and 10 liters of high-boiling point petroleum ether was added to precipitate p-coumaric acid. The precipitate was collected by filtration and dried to obtain 700 grams of crude p-coumaric acid, which was recrystallized with 20% dilute alcohol to ...

Embodiment 3

[0025]1. Add 1500 kg of 0.6% potassium carbonate solution to 100 kg of corn husks at room temperature, then add 100 g of sodium metabisulfite powder, stir and soak for 20 hours under the action of ultrasound with a power of 8 kW. After filtration, the filtrate was neutralized to pH=4 with dilute phosphoric acid, and the solution became cloudy. The solution was concentrated in vacuo to 60 liters, 10 liters of ethyl acetate was added, the layers were separated after vigorous stirring, and the p-coumaric acid was extracted into the ethyl acetate phase, and extracted twice. The extracted aqueous phase is used for later use. The two extracted ethyl acetate phases were combined to a total of about 20 liters, concentrated in vacuo to 2 liters, and 10 liters of high-boiling point petroleum ether was added to precipitate p-coumaric acid. The precipitate was collected by filtration and dried to obtain 700 grams of crude p-coumaric acid, which was recrystallized with 20% dilute alcohol ...

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Abstract

The invention discloses a method for extracting ferulic acid, p-coumaric acid and pentosan from corn husks, which belongs to the technical field of chemical industry. The method includes firstly, soaking corn husks into alkali solution, filtering and extracting p-coumaric acid after filtrate is neutralized to meet PH (potential of hydrogen) = 3-4 and concentrated, secondly, soaking the corn husks filtered from the first step into alkali solution, filtering and extracting ferulic acid by ethyl acetate after the filtrate is neutralized to meet PH (potential of hydrogen) = 3-4 and vacuum concentration is completed, thirdly, merging aqueous phase after the extraction of ethyl acetate in the step one and the step two, fourthly, desalinizing and condensing by means of nanofiltration, and fifthly, collecting pentosan by means of centrifugal settling after precipitated pentosan is dissolved out. The method for extracting ferulic acid, p-coumaric acid and pentosan from corn husks is short in production cycle and lower in solvent consumption, and thereby production efficiency can be further improved for enterprises.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and relates to the comprehensive utilization of corn bran. Background technique [0002] Corn bran is a by-product of starch production, which accounts for about 10-12% of corn kernels and is currently mainly used for the production of feed. Pentosan in corn bran is about 20-25%, ferulic acid is about 3-4%, and p-coumaric acid is 0.5-1.0%. Ferulic acid is a product widely used in medicine, cosmetics and other fields. Sodium ferulic acid and sodium chloride injection, sodium ferulic acid tablets, and piperazine ferulic acid are all approved for clinical use Drugs; p-coumaric acid is mainly used as an intermediate of the pesticide Warfarin, Warfarin, Bromadiolone, Brodifacoum, Shudeke, Fludifafarum, Thiafafarum, and Clofacoum, etc. It can also be used in Anticoagulant drugs such as dicoumarin ethyl ester and ketobenzylcoumarin are used in medicine, and they are also intermediates of the ...

Claims

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Application Information

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IPC IPC(8): C07C59/64C07C59/52C07C51/42C07H3/06C07H1/08
Inventor 刘启民
Owner 刘启民
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