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Vanillin extraction method

An extraction method and vanillin technology, applied in the field of vanillin extraction, can solve the problems of inability to effectively remove ferulic acid impurities, emulsification, etc., and achieve the effects of ensuring continuous and stable operation, reducing requirements, and smooth extraction process.

Active Publication Date: 2015-05-13
浙江普洛生物科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to meet the market demand for natural green products, on the one hand, it solves the problem that impurities such as ferulic acid, vanillic acid and guaiacol cannot be effectively removed in the extraction and separation process of vanillin prepared by microbial fermentation in the prior art ; On the other hand, solve the emulsification problem in the vanillin extraction process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A method for extracting vanillin, comprising the steps of:

[0030] 2L of fermented broth containing 10.6g / L vanillin produced by microbial transformation method, adjust the pH value to 3.0 with 10mol / L sulfuric acid, add 30g of perlite powder (a filter aid commonly used in fermentation industry filtration operations), vacuum pump After filtration, 300ml of water was added for rinsing to obtain 2230ml of acidified filtrate.

[0031] The filtrate was adjusted to pH 7.0 with NaOH, then concentrated in vacuo at 70°C to 450ml, cooled to 24°C, and the pH of the filtrate was adjusted to 6.5 with sulfuric acid, then extracted twice with equal volume of ethyl acetate, stirring for 30 minutes each time Then add 0.5g of dodecyltrimethylammonium chloride, continue to stir for 5 minutes, let stand, separate layers, combine the two extracts to obtain a total of 890ml of extracts.

[0032] Add 100ml of water to the extract, add NaOH solution while stirring to adjust the pH value of ...

Embodiment 2

[0036] A method for extracting vanillin, comprising the steps of:

[0037] 2L of fermented liquid containing vanillin 9.7g / L produced by microbial transformation method was used to adjust the pH value to 3.5 with 10mol / L sulfuric acid, 30g of perlite powder was added, after vacuum filtration, 300ml of water was added for rinsing to obtain 2220ml of acidified filtrate.

[0038] The filtrate was adjusted to pH 6.0 with NaOH, then concentrated in vacuo at 70°C to 470ml, cooled to 24°C, and the pH of the filtrate was adjusted to 5.0 with sulfuric acid, then extracted twice with equal volume of ethyl acetate, stirring for 30 minutes each time Then add 0.1 g of dodecyltrimethylammonium chloride, continue to stir for 5 minutes, let stand, separate layers, and combine the two extracts to obtain a total of 930 ml of extracts.

[0039] Add 300ml of water to the extract, and while stirring, add KOH solution to adjust the pH value of the water phase to 6.0, wash with weak alkali, let stan...

Embodiment 3

[0043] A method for extracting vanillin, comprising the steps of:

[0044] 2L of fermented liquid containing vanillin 10.2g / L produced by microbial conversion method was adjusted to pH 3.8 with 10mol / L sulfuric acid, 30g of perlite powder was added, after vacuum filtration, 300ml of water was added for rinsing to obtain 2230ml of acidified filtrate.

[0045] The filtrate was adjusted to pH 6.7 with NaOH, then concentrated in vacuo at 70°C to 450ml, cooled to 24°C, and the pH of the concentrated filtrate was adjusted to 8.0 with NaOH, then extracted twice with an equal volume of butyl acetate, stirring for 30 ml each time. Add 0.5g of dodecyltrimethylammonium chloride after 1 minute, continue to stir for 5 minutes, let stand, separate layers, combine two extracts to obtain a total of 890ml of extracts.

[0046] Add 500ml of water to the extract, add KOH solution while stirring to adjust the pH value of the water phase to 6.8, wash with weak alkali, let stand, and separate layer...

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PUM

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Abstract

The invention belongs to the field of essence perfumes and food additives, and particularly relates to a vanillin extraction method, which comprises: sequentially carrying out acidification, filtration, filtrate concentration, neutral extraction, weak alkali water washing, extraction solution concentration and crystallization aging treatment on a vanillin-containing microorganism conversion fermentation broth to obtain the yellowish or white-like crystal powder of vanillin, wherein an ionic demulsifier is added during the extraction process. With the extraction method, vanillic acid, ferulic acid, guaiacol and other impurities can be effectively removed from the fermentation broth; the adaptability on the fermentation broths with different qualities is strong; and with the efficient demulsification method, the extraction process is smooth, and continuous and stable operation of industrial production is ensured.

Description

technical field [0001] The invention belongs to the field of flavors and fragrances and food additives, and in particular relates to a method for extracting vanillin. Background technique [0002] Vanillin, scientific name 3-methoxy-4-hydroxybenzaldehyde, also known as vanillin. It exists naturally in essential oils such as vanilla bean, clove oil, Peru balsam, and tolu balsam. The price of vanillin obtained by different production methods varies greatly, mainly as follows: (1) Extracted from plants containing natural vanillin, the market price is 4,000 US dollars / kg. (2) Chemical synthesis methods can be divided into guaiacol method, lignin method, safrole method, eugenol method, p-hydroxybenzaldehyde method, 4-methylguaiacol method, p-cresol method according to the starting raw materials There are several kinds of methods, such as guaiacol method, which is mainly used in industry at present, and the market price is 10 US dollars / kg. (3) Vanillin is produced by microbial...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/58C07C45/78C07C45/85C07C45/80
CPCC07C45/78C07C45/80C07C47/58
Inventor 周晋武吕文进金明平王文涛纪春华
Owner 浙江普洛生物科技有限公司