CN103910622A - Method for extracting ferulic acid from waste liquid produced by preparation process of corn bran dietary fibers - Google Patents
Method for extracting ferulic acid from waste liquid produced by preparation process of corn bran dietary fibers Download PDFInfo
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- CN103910622A CN103910622A CN201310713194.5A CN201310713194A CN103910622A CN 103910622 A CN103910622 A CN 103910622A CN 201310713194 A CN201310713194 A CN 201310713194A CN 103910622 A CN103910622 A CN 103910622A
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- waste liquid
- preparation process
- ethanol
- forulic acid
- food fibre
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the field of deep processing technology of corns, and particularly relates to a method for extracting ferulic acid from waste liquid produced by a preparation process of corn bran dietary fibers. The method comprises the following steps of centrifuging the waste liquid, concentrating by evaporation, adjusting a pH value of the waste liquid by using concentrated hydrochloric acid after impurities and ethanol are removed; adsorbing the acidified waste liquid by using a macroporous resin; carrying out ferulic acid elution on a saturated resin by using ethanol; centrifuging and evaporating eluent; extracting by using ethyl acetate; taking an ester phase; concentrating the ester phase at a reduced pressure and evaporating ethyl acetate to obtain a product. The method is simple in steps and low in production cost. Ferulic acid is extracted from the waste liquid produced by the preparation process of the corn bran dietary fibers, so that resource waste can be prevented; environment pollution is overcome; wastes are changed into valuables; and social and economic effects are produced.
Description
(1) technical field
The present invention relates to corn deep processing technology field, particularly a kind of waste liquid producing from cmaize peel food fibre preparation process, extract the method for forulic acid.
(2) background technology
China's corn yield accounts for 20% left and right of world's corn ultimate production at present, occupy the second in the world, but China's corn commercial production level is low, most starches processing enterprise only utilizes the composition of corn kernel 50-60% to prepare commodity starch, and the maize peel that accounts for corn over dry quality 14-20% is only sold as feed, added value is extremely low.Cmaize peel food fibre can dilute carcinogenic substance and the toxic substance in food; accelerating it removes; protect fragile digestive tube and prevent colon cancer simultaneously; therefore prepare cmaize peel food fibre by maize peel and become the focus of current research; wherein comparatively advanced technology is to adopt zytase enzymolysis process to prepare cmaize peel food fibre, but contains valuable composition in the waste liquid that the method produces.
The chemistry Ferulic acid by name of forulic acid, it is ubiquitous a kind of phenolic acid in plant, have the physiological functions such as the free radical, antithrombotic, reducing blood-fat of removing, it is mainly crosslinked by ester bond and ehter bond and cell wall polysaccharides, xylogen, formation cytoskeleton.The preparation method of forulic acid mainly, take 4-hydroxyl-3-methoxylbenxaldehyde as raw material, synthesizes by chemical process, but this legal system is lower for forulic acid yield, and long reaction time, and reagent dosage is large.
Maize peel contains forulic acid, vanillic acid isoreactivity material, wherein ferulaic acid content is up to 3%, prepare cmaize peel food fibre waste liquid and separate forulic acid from zytase enzymolysis process, not only avoid the wasting of resources, solve environmental pollution, turn waste into wealth again simultaneously, produce good society and economic benefit, and provide new thinking for maize peel high-efficiency comprehensive utilization.
(3) summary of the invention
The present invention is in order to make up the deficiencies in the prior art, provides a kind of and economize on resources, extracted the waste liquid producing from cmaize peel food fibre preparation process of protection of the environment the method for forulic acid.
The present invention is achieved through the following technical solutions:
The waste liquid producing from cmaize peel food fibre preparation process, extract a method for forulic acid, the waste liquid producing take cmaize peel food fibre preparation process, as raw material, comprises the steps:
(1) by centrifugal waste liquid removal large granular impurity, then concentration and evaporation goes out the ethanol in waste liquid;
(2) adopt concentrated hydrochloric acid that removal of impurities is adjusted to 2-3 except the pH value of waste liquid after ethanol;
(3) absorption of the waste liquid after to acidifying with macroporous adsorbent resin, adopts iron(ic) chloride and Tripotassium iron hexacyanide mixed solution as colored indicator, by with the colour developing situation of effluent liquid, determine the saturated terminal of resin absorption;
(4) adopt ethanol to carry out forulic acid wash-out to saturated resin, determine wash-out terminal by iron(ic) chloride and Tripotassium iron hexacyanide mixed solution and elutriant color reaction;
(5) elutriant concentration and evaporation is removed to ethanol, then be extracted with ethyl acetate, get ester phase concentrating under reduced pressure and volatilize ethyl acetate, products obtained therefrom is forulic acid.
More excellent technical scheme of the present invention is:
In step (1), waste liquid is centrifugal 10-15min under 3000r/min, then concentration and evaporation ethanol under 50 ℃ ,-0.1MPa.
In step (3), the model of macroporous adsorbent resin is HDP-100, AB-8, NKA, HDP-722, HDP-750 or D101, the absorption flow velocity of waste liquid is 2-3BV/h, shows the iron(ic) chloride of 1% massfraction and the Tripotassium iron hexacyanide mixed solution of 1% massfraction that indicator is fresh configuration.
In step (4), wash-out is 60-80% by the mass concentration of ethanol, and flow velocity is 1-2BV/h, and color reaction is used the iron(ic) chloride of 1% massfraction and the Tripotassium iron hexacyanide mixed solution of 1% massfraction of fresh configuration.
In step (5), elutriant concentration and evaporation under 50 ℃ ,-0.1MPa falls ethanol, then with the ethyl acetate extraction of 2 times of volumes of elutriant, and ester is concentrating under reduced pressure under 40-45 ℃ ,-0.1MPa.
Step of the present invention is simple, and production cost is low, from the waste liquid of cmaize peel food fibre production process, forulic acid is extracted, and has not only avoided the wasting of resources, has solved environmental pollution, turns waste into wealth simultaneously, has produced economic results in society.
(4) embodiment
Embodiment:
(1) waste liquid separates: the waste liquid 5000mL that food fibre preparation process is produced, after packing under 3000r/min centrifugal 10-15min, remove large granular impurity wherein, get supernatant liquor, at 50 ℃, the concentrated ethanol evaporating in waste liquid under-0.1MPa.
(2) acidification: the pH value that adopts concentrated hydrochloric acid that removal of impurities is removed to the concentrating spent liquor after ethanol is adjusted to 2-3.
(3) resin absorption: the waste liquid with HDP-100, AB-8, NKA, HDP-722, HDP-750 or D101 macroporous adsorbent resin after to acidifying adsorbs, flow velocity is 2-3BV/h, iron(ic) chloride with freshly prepared 1% and 1% Tripotassium iron hexacyanide mixed solution are as colored indicator, by with the colour developing situation of effluent liquid, determine the saturated terminal of resin absorption; Treat effluent liquid and show that indicator is obvious blue and reacts, stopping absorption.
(4) wash-out: adopt 60-80% ethanol, by the flow velocity of 1 ~ 2BV/h, saturated resin is carried out to forulic acid wash-out, determine that 2BV is and collects unit, the iron(ic) chloride with freshly prepared 1% and 1% Tripotassium iron hexacyanide mixed solution and elutriant color reaction are determined wash-out terminal.
(5) solvent extraction: first at 50 ℃, the concentrated ethanol of removing under-0.1MPa, then extract by the ethyl acetate of 2 times of volumes, gets ester phase to elutriant, and 40 ~ 45 ℃ ,-0.1MPa concentrating under reduced pressure is flung to ethyl acetate, obtains product forulic acid 1.2g.
Claims (5)
1. the waste liquid that a kind produces from cmaize peel food fibre preparation process, extract the method for forulic acid, the waste liquid producing take cmaize peel food fibre preparation process is as raw material, it is characterized by, comprise the steps: that (1) is by centrifugal waste liquid removal large granular impurity, then concentration and evaporation goes out the ethanol in waste liquid; (2) adopt concentrated hydrochloric acid that removal of impurities is adjusted to 2-3 except the pH value of waste liquid after ethanol; (3) absorption of the waste liquid after to acidifying with macroporous adsorbent resin, adopts iron(ic) chloride and Tripotassium iron hexacyanide mixed solution as colored indicator, by with the colour developing situation of effluent liquid, determine the saturated terminal of resin absorption; (4) adopt ethanol to carry out forulic acid wash-out to saturated resin, determine wash-out terminal by iron(ic) chloride and Tripotassium iron hexacyanide mixed solution and elutriant color reaction; (5) elutriant concentration and evaporation is removed to ethanol, then be extracted with ethyl acetate, get ester phase concentrating under reduced pressure and volatilize ethyl acetate, products obtained therefrom is forulic acid.
2. the waste liquid producing from cmaize peel food fibre preparation process according to claim 1, extract the method for forulic acid, it is characterized in that: in step (1), waste liquid is centrifugal 10-15min under 3000r/min, then concentration and evaporation ethanol under 50 ℃ ,-0.1MPa.
3. the waste liquid producing from cmaize peel food fibre preparation process according to claim 1, extract the method for forulic acid, it is characterized in that: in step (3), the model of macroporous adsorbent resin is HDP-100, AB-8, NKA, HDP-722, HDP-750 or D101, the absorption flow velocity of waste liquid is 2-3BV/h, shows the iron(ic) chloride of 1% massfraction and the Tripotassium iron hexacyanide mixed solution of 1% massfraction that indicator is fresh configuration.
4. the waste liquid producing from cmaize peel food fibre preparation process according to claim 1, extract the method for forulic acid, it is characterized in that: in step (4), wash-out is 60-80% by the mass concentration of ethanol, flow velocity is 1-2BV/h, and color reaction is used the iron(ic) chloride of 1% massfraction and the Tripotassium iron hexacyanide mixed solution of 1% massfraction of fresh configuration.
5. the waste liquid producing from cmaize peel food fibre preparation process according to claim 1, extract the method for forulic acid, it is characterized in that: in step (5), elutriant concentration and evaporation under 50 ℃ ,-0.1MPa falls ethanol, again with the ethyl acetate extraction of elutriant 2 times of volumes, ester is concentrating under reduced pressure under 40-45 ℃ ,-0.1MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310713194.5A CN103910622A (en) | 2013-12-23 | 2013-12-23 | Method for extracting ferulic acid from waste liquid produced by preparation process of corn bran dietary fibers |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310713194.5A CN103910622A (en) | 2013-12-23 | 2013-12-23 | Method for extracting ferulic acid from waste liquid produced by preparation process of corn bran dietary fibers |
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| CN103910622A true CN103910622A (en) | 2014-07-09 |
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| CN201310713194.5A Pending CN103910622A (en) | 2013-12-23 | 2013-12-23 | Method for extracting ferulic acid from waste liquid produced by preparation process of corn bran dietary fibers |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101980816B1 (en) * | 2017-11-15 | 2019-05-22 | 대한민국 | Composition for prevention, treatment or improvement of obesity comprising ferulic acid in italian ryegrass as an active ingredient |
| CN113429289A (en) * | 2021-06-18 | 2021-09-24 | 山东星光首创生物科技有限公司 | Method for extracting ferulic acid from waste liquid generated in preparation of corn bran dietary fibers |
| CN115340453A (en) * | 2022-09-06 | 2022-11-15 | 张家宾 | Preparation method of sodium naphthalene acetate for fertilizer additive |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103254064A (en) * | 2013-05-22 | 2013-08-21 | 暨南大学 | Preparation method of ferulic acid |
-
2013
- 2013-12-23 CN CN201310713194.5A patent/CN103910622A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103254064A (en) * | 2013-05-22 | 2013-08-21 | 暨南大学 | Preparation method of ferulic acid |
Non-Patent Citations (2)
| Title |
|---|
| 宋晓凯: "《植物化学研究方法选论》", 31 December 2008, article "《植物化学研究方法选论》", pages: 26-29 * |
| 肖培根: "《新编中药志》", 31 December 2007, article "新编中药志", pages: 1136 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101980816B1 (en) * | 2017-11-15 | 2019-05-22 | 대한민국 | Composition for prevention, treatment or improvement of obesity comprising ferulic acid in italian ryegrass as an active ingredient |
| CN113429289A (en) * | 2021-06-18 | 2021-09-24 | 山东星光首创生物科技有限公司 | Method for extracting ferulic acid from waste liquid generated in preparation of corn bran dietary fibers |
| CN115340453A (en) * | 2022-09-06 | 2022-11-15 | 张家宾 | Preparation method of sodium naphthalene acetate for fertilizer additive |
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Application publication date: 20140709 |