CN108530288A - A kind of more effect components separation of wood vinegar and complete utilization method - Google Patents
A kind of more effect components separation of wood vinegar and complete utilization method Download PDFInfo
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- CN108530288A CN108530288A CN201810477165.6A CN201810477165A CN108530288A CN 108530288 A CN108530288 A CN 108530288A CN 201810477165 A CN201810477165 A CN 201810477165A CN 108530288 A CN108530288 A CN 108530288A
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- Prior art keywords
- wood vinegar
- fraction
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- ethyl acetate
- volume ratio
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- 239000002023 wood Substances 0.000 title claims abstract description 81
- 239000000052 vinegar Substances 0.000 title claims abstract description 77
- 235000021419 vinegar Nutrition 0.000 title claims abstract description 77
- 230000000694 effects Effects 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000000926 separation method Methods 0.000 title abstract description 11
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 140
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 70
- 238000004821 distillation Methods 0.000 claims abstract description 29
- 239000000243 solution Substances 0.000 claims abstract description 29
- 239000012071 phase Substances 0.000 claims abstract description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 12
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 12
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 238000000605 extraction Methods 0.000 claims abstract description 6
- 239000012074 organic phase Substances 0.000 claims abstract description 3
- 235000019439 ethyl acetate Nutrition 0.000 claims description 44
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 3
- 244000105624 Arachis hypogaea Species 0.000 claims description 3
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 3
- 235000018262 Arachis monticola Nutrition 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims description 3
- 235000007164 Oryza sativa Nutrition 0.000 claims description 3
- 240000008866 Ziziphus nummularia Species 0.000 claims description 3
- 239000000284 extract Substances 0.000 claims description 3
- 239000010903 husk Substances 0.000 claims description 3
- 235000020232 peanut Nutrition 0.000 claims description 3
- 235000009566 rice Nutrition 0.000 claims description 3
- 235000006708 antioxidants Nutrition 0.000 abstract description 9
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 4
- 201000004624 Dermatitis Diseases 0.000 abstract description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 15
- 230000003026 anti-oxygenic effect Effects 0.000 description 7
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 6
- 150000007524 organic acids Chemical class 0.000 description 6
- 150000002989 phenols Chemical class 0.000 description 6
- 150000001299 aldehydes Chemical class 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 3
- 229930003268 Vitamin C Natural products 0.000 description 3
- 230000000845 anti-microbial effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000855 fungicidal effect Effects 0.000 description 3
- 239000000417 fungicide Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000001629 suppression Effects 0.000 description 3
- 229930003231 vitamin Natural products 0.000 description 3
- 239000011782 vitamin Substances 0.000 description 3
- 235000013343 vitamin Nutrition 0.000 description 3
- 229940088594 vitamin Drugs 0.000 description 3
- 235000019154 vitamin C Nutrition 0.000 description 3
- 239000011718 vitamin C Substances 0.000 description 3
- 150000003722 vitamin derivatives Chemical class 0.000 description 3
- 241000588724 Escherichia coli Species 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000002260 anti-inflammatory agent Substances 0.000 description 2
- 229940121363 anti-inflammatory agent Drugs 0.000 description 2
- 230000000840 anti-viral effect Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 244000144972 livestock Species 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000256602 Isoptera Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 208000036142 Viral infection Diseases 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000003266 anti-allergic effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000001556 anti-picornavirus Effects 0.000 description 1
- 239000003429 antifungal agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- KLIDCXVFHGNTTM-UHFFFAOYSA-N syringol Natural products COC1=CC=CC(OC)=C1O KLIDCXVFHGNTTM-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 241000712461 unidentified influenza virus Species 0.000 description 1
Classifications
-
- 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
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N31/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic oxygen or sulfur compounds
- A01N31/08—Oxygen or sulfur directly attached to an aromatic ring system
- A01N31/16—Oxygen or sulfur directly attached to an aromatic ring system with two or more oxygen or sulfur atoms directly attached to the same aromatic ring system
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/02—Saturated carboxylic acids or thio analogues thereof; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3481—Organic compounds containing oxygen
- A23L3/3499—Organic compounds containing oxygen with doubly-bound oxygen
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/004—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by obtaining phenols from plant material or from animal material
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/72—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/80—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/06—Systems containing only non-condensed rings with a five-membered ring
- C07C2601/08—Systems containing only non-condensed rings with a five-membered ring the ring being saturated
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- Environmental Sciences (AREA)
- Pest Control & Pesticides (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
- Microbiology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Anti-Oxidant Or Stabilizer Compositions (AREA)
- Medicines Containing Plant Substances (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention relates to a kind of more effect component separation of wood vinegar and complete utilization methods, and wood vinegar level-one is taken to distill, and collect 98 DEG C of fraction secondary distillation, 96 DEG C and 97 DEG C of component is collected in secondary distillation；Residue after level-one is distilled, it is extracted with ethyl acetate three times, merge ethyl acetate phase three times, for level-one extracting solution, twice with the aqueous solution extraction of NaOH by level-one extracting solution, merge water phase twice, this is two level extracting solution, two level extracting solution is acidified to pH to 26 with hydrochloric acid, it is 3/7 7/3 two level extracting solution to be further purified three times with ethyl acetate/n-hexane volume ratio, retain organic phase, discard water phase, the antioxidant composition detached, it is precisely separated anti-oxidant, antibacterial, anti- dermatitis and food-grade wood vinegar, improve the commercial value and economic benefit of wood vinegar.
Description
Technical field
The invention belongs to wood vinegar separation technology fields, and in particular to a kind of more effect components separation of wood vinegar and complete utilization
Method.
Background technology
Wood vinegar be slowly be pyrolyzed by the biomass of plant generation cigarette it is condensed after the yellowish-brown that is formed or dark-brown coagulate
Object is tied, main component is water, organic acid and phenolic compound.Wood vinegar has powerful anti-oxidant and antibacterial isoreactivity, leads to
Often it is used as the multiple fields such as food additives, anti-inflammatory agent or antifungal drug.The antibacterial activity of wood vinegar with it is wherein organic
The content of acid, phenol derivatives and carbonyls is proportionate.The kill termite activity and organic acid, phenols content of wood vinegar have
Direct relation, the especially aldehydes matter containing some substituent groups.In addition, other sp acts of wood vinegar, for example, it is anti-inflammatory and
Antiallergic activity, it is also directly related with the content of organic acid or phenolic compound.Although the active and organic acid of wood vinegar
Or the content of phenolic compound is nearly all proportionate, but the main component to work in different activities is different.It is reported that
2- methoxyl group -4- methylphenols are the main antiinflammation compounds in wood vinegar, and phenol then rises in antiviral activity mainly
Effect.Research shows that the synergistic effect of phenol and acetic acid has larger impact to the activity of the anti-picornavirus of wood vinegar,
It is potentially assisted to antimicrobial and antioxidant activity the research of wood vinegar, it was also found that existing between organic acid and aldehydes matter
Same-action.The research of the polishing purification process of wood vinegar is focused primarily upon organic acid with the alkaline solution of different pH at present and
Phenolic compound is detached from wood vinegar.But many useless components, functional component are usually contained in separated extract
Be precisely separated still be not implemented, it is relatively low so as to cause the added value of wood vinegar, be not easy large-scale industrial production and commercialization.Cause
This, it is very necessary to accurately identify functional component and the synergistic effect between them in wood vinegar.
Invention content
The object of the present invention is to provide a kind of more effect component separation of wood vinegar and complete utilization methods, will be effective in wood vinegar
Component is precisely separated and the reasonable utilization of none waste, and simple for process, at low cost and environmentally friendly, improves the economy of wood vinegar
Added value.
The purpose of the present invention is achieved through the following technical solutions：
A kind of more effect components separation of wood vinegar and complete utilization method, its step are as follows：
A. it takes crude wood vinegar to carry out level-one distillation, collects 98 DEG C of fraction and carry out secondary distillation, collected in secondary distillation
96 DEG C of component is named as fraction 1, collects 97 DEG C of component and is named as fraction 2, when the solution of secondary distillation becomes brown or depth
When brown, stops secondary distillation, the residue after secondary distillation is named as fraction 3.
B. antioxidant composition is extracted from the residue after level-one distillation in step a, the residue after level-one is distilled is used
Ethyl acetate (EtOAc) extracts three times, merges ethyl acetate phase three times, is level-one extracting solution, by level-one extracting solution 1mol/
The aqueous solution extraction of LNaOH twice, merges water phase twice, this be two level extracting solution, the level-one distillation after residue,
The volume ratio of the aqueous solution of primary ethyl acetate and primary NaOH is 3：1：1；
C. the two level extracting solution obtained in step b is acidified to pH to 2-6 with hydrochloric acid, with ethyl acetate/n-hexane volume
Than two level extracting solution is further purified three times for 3/7-7/3, retains organic phase, discard water phase, obtain three-level extracting solution, as
The antioxidant composition of separation, the body of residue and the mixed liquor of primary ethyl acetate and n-hexane after level-one distillation
Product is than being 3：1.
Further, the pH is 2, and ethyl acetate/n-hexane volume ratio is named as fraction 4 for 7/3.
Further, the pH is 3, and ethyl acetate/n-hexane volume ratio is named as fraction 5 for 7/3.
Further, the pH is 4, and ethyl acetate/n-hexane volume ratio is named as fraction 6 for 7/3.
Further, the pH is 4, and ethyl acetate/n-hexane volume ratio is named as fraction 7 for 1/1.
Further, the pH is 4, and ethyl acetate/n-hexane volume ratio is named as fraction 8 for 3/7.
Further, the pH is 5, and ethyl acetate/n-hexane volume ratio is named as fraction 9 for 7/3.
Further, the pH is 6, and ethyl acetate/n-hexane volume ratio is named as fraction 10 for 7/3.
Further, the wood vinegar is toothed oak wood wood vinegar, jujube nucleus wood vinegar, rice husk wood vinegar, peanut shell wood vinegar
Liquid, corncob wood vinegar etc..
Beneficial effects of the present invention are as follows：
Method provided by the invention is combined using level-one distillation, liquid-liquid extraction, secondary distillation three from wood vinegar smart
Anti-oxidant, antibacterial, anti-dermatitis and food-grade wood vinegar are really detached, the comprehensive utilization of wood vinegar and the pipe of agricultural wastes are contributed to
Reason and application, and the production process of wood vinegar can be promoted more economical, improve the commercial value of wood vinegar and economic effect
Benefit.Fraction 1 is a kind of potential fungicide, can safely be applied to extensively in agricultural and the living environment of the mankind, such as inactivate dynamic
Object virus spread and prevention livestock, mankind's epidemic disease, fraction 2 may be used as food-grade wood vinegar.The maximum suppression of fraction 3 dilutes
Degree is 20 times of wood vinegar, and according to the literature, there is bacteriostasis property more stronger than wood vinegar.
Description of the drawings
Fig. 1 provides the process flow chart of the more effect component separation of wood vinegar and its method utilized for the present invention；
Fig. 2 is the vitamin equivalent comparison diagram of the TIC figure and oxidation resistance of wood vinegar and separate fraction；
Fig. 3 is the vitamin equivalent comparison diagram of the oxidation resistance of fraction 4-10；
Fig. 4 is the influence comparison diagram of wood vinegar and the separate fraction Escherichia coli Growth situation later to logarithmic phase；
Fig. 5 is the influence comparison diagram of the various concentration Escherichia coli Growth situation later to logarithmic phase of fraction 3.
Specific implementation mode
Below in conjunction with attached drawing detailed description of the present invention technical solution, the embodiment of the present invention is only to illustrate the skill of the present invention
Art scheme and it is unrestricted, although the present invention is described in detail with reference to preferred embodiments, the ordinary skill people of this field
Member it should be appreciated that can be modified or replaced equivalently to technical scheme of the present invention, without departing from the present invention spirit and
Range should all cover in scope of the presently claimed invention.
Embodiment 1：
As shown in Figure 1, the more effect component separation of toothed oak wood wood vinegar and complete utilization method, are as follows：
D. it takes 100 parts of crude toothed oak wood wood vinegar to carry out level-one distillation, collects 98 DEG C of fraction and carry out secondary distillation, secondary steaming
It evaporates the middle component for collecting 96 DEG C and is named as fraction 1, collect 97 DEG C of component and be named as fraction 2, when the solution of secondary distillation becomes
When brown or dark brown, stops secondary distillation, the residue after secondary distillation is named as fraction 3.
E. antioxidant composition is extracted from 6 parts of residue after level-one distillation in step a, the remnants after level-one is distilled
Object three times with ethyl acetate (EtOAc) extraction every time with 2 parts of ethyl acetate, merges ethyl acetate phase three times, is carried for level-one
Liquid is taken, twice with the aqueous solution extraction of 1mol/LNaOH by level-one extracting solution, uses the aqueous solution of 2 parts of NaOH every time, merging is twice
Water phase, this be two level extracting solution；
F. the two level extracting solution obtained in step b is acidified to pH to 2-6 with hydrochloric acid, with ethyl acetate/n-hexane volume
Than two level extracting solution is further purified three times for 3/7-7/3, every time with 2 parts of ethyl acetate and n-hexane mixed liquor, remain with
Machine phase, discards water phase, obtains three-level extracting solution, the antioxidant composition as detached, is named as fraction 4, and the pH is 2, second
Acetoacetic ester/n-hexane volume ratio is 7/3.
Embodiment 2
The present embodiment is that the pH is 3 with the difference place of embodiment 1, and ethyl acetate/n-hexane volume ratio is 7/3
It is named as fraction 5.
Embodiment 3
The present embodiment is that the pH is 4 with the difference place of embodiment 1, and ethyl acetate/n-hexane volume ratio is 7/3
It is named as fraction 6.
Embodiment 4
The present embodiment is that pH 4, ethyl acetate/n-hexane volume ratio is named as 1/1 with the difference place of embodiment 1
Fraction 7.
Embodiment 5
The present embodiment is that further, the pH is 4, ethyl acetate/n-hexane body with the difference place of embodiment 1
Product for 3/7 than being named as fraction 8.
Embodiment 6
The present embodiment is that further, the pH is 5, ethyl acetate/n-hexane body with the difference place of embodiment 1
Product for 7/3 than being named as fraction 9.
Embodiment 7
The present embodiment is that further, the pH is 6, ethyl acetate/n-hexane body with the difference place of embodiment 1
Product for 7/3 than being named as fraction 10.
Embodiment 8
The present embodiment is that the pH is 3 with the difference place of embodiment 1, and ethyl acetate/n-hexane volume ratio is 7/3,
The wood vinegar is rice husk wood vinegar, and the antioxygenic property vitamin C equivalent proportion fraction 5 of gained fraction lacks 25mg/L.
Embodiment 9
The present embodiment is that pH 4, ethyl acetate/n-hexane volume ratio is 1/1, described with the difference place of embodiment 1
Wood vinegar is corncob wood vinegar, and the antioxygenic property vitamin C equivalent proportion fraction 7 of gained fraction lacks 32mg/L.
Embodiment 9
The present embodiment is that the pH is 5 with the difference place of embodiment 1, and the wood vinegar is peanut shell wood vinegar,
Ethyl acetate/n-hexane volume ratio is 7/3, and gained fraction antioxygenic property vitamin C equivalent proportion fraction 9 lacks 7mg/L.
Embodiment 10
The present embodiment is that the pH is 6 with the difference place of embodiment 1, and the wood vinegar is jujube nucleus wood vinegar,
Ethyl acetate/n-hexane volume ratio is 7/3, and the vitamin equivalent and fraction 10 of the antioxygenic property of gained fraction maintain an equal level.
As shown in Fig. 2, the main component of the isolated each fraction of method provided by the invention is very different, wherein 1
It is 3- methyl-1s for acetic acid, 2,2- cyclopentanediones, 3 be 2,6- syringol, and 4 be 1- hydroxyl -2- acetone, and 5 be 2- methoxies
Base phenol, 6 be 2- methoxyl group -4- methyl-phenols, and 7 be phenol.Antioxidant composition is distributed mainly on the residue after level-one distillation
In.Due to the comprehensive utilization of wood vinegar be conducive to resource make full use of and environmental protection, the present invention to level-one distill after
Residue in antioxygen object separation carried out condition optimizing.Main component in fraction 1 is acetic acid, 1- hydroxyl -2- acetone and
Some a small amount of aldehydes matters, such as 2- metoxyphenols, 2- methoxyl group -4- methylphenols and phenol, and fraction 2 is by acetic acid and one
The aldehydes matter composition measured slightly.Since phenol and acetic acid are formed by the antiviral compound that acid medium is excellent, evaporate
It is a kind of potential fungicide to divide 1, can be safely applied to extensively in agricultural and the living environments of the mankind, such as inactivation animal infection
Viral (such as avian influenza virus) and prevent livestock, mankind's epidemic disease.Because 2- methoxyl group -4- methylphenols are the masters in wood vinegar
Antiinflammation compound is wanted, so fraction 1 can also be as the potential source of anti-inflammatory agent.Since all toxic components are gone
It removes, fraction 2 may be used as food-grade wood vinegar.
As shown in figure 3, after distillation, by different volumes than ethyl acetate/n-hexane extraction residue or adjustment pH to 2-
6, obtain fraction 4-10.The antioxygenic property of fraction 4-10 is very different.Ethyl acetate/n-hexane (v/v) in extractant
Ratio the antioxygenic property of each fraction is had a significant impact, meanwhile, the pH value of the solution after being acidified with HCl also resists fraction
Oxidation susceptibility also has a significant impact.The antioxygenic property of fraction 4-10 thus decreasing order：Fraction 6>Fraction 4>Fraction 5>Fraction 7
>Fraction 8>Fraction 9>Fraction 10.In summary experimental result can show that pH=4 is the Optimal pH of the solution after being acidified with HCl
Value, and volume ratio 7/3 is the optimal proportion of ethyl acetate/n-hexane.
As shown in figure 4, fraction 3 has very strong anti-microbial property, the anti-microbial property of other fractions relatively weak.In Fig. 4 (a)
There is identical lowercase person difference not significantly (P>0.05), person's significant difference (P that differs lowercase<0.05).
As shown in figure 5, the maximum suppression dilution of fraction 3 is 2000 times, and according to the literature, the maximum suppression of wood vinegar
Dilution processed is 100 times or so, so fraction 3 has bacteriostasis property more stronger than wood vinegar, it may be considered that as food fresh keeping
Agent and fungicide use.There is identical lowercase person difference not significantly (P in Fig. 5>0.05), the person's difference that differs lowercase is aobvious
Write (P<0.05).
After method provided by the present invention processing, all components are obtained for reasonable utilization in wood vinegar, none
Waste, not only realizes the comprehensive utilization of wood vinegar, is also effectively improved the economic value added of wood vinegar.
Claims (9)
1. a kind of more effect components of wood vinegar detach and complete utilization method, which is characterized in that steps are as follows：
A. it takes crude wood vinegar to carry out level-one distillation, the component life of 96 DEG C of collection after secondary distillation is carried out after the fraction of 98 DEG C of collection
Entitled fraction 1 collects 97 DEG C of component and is named as fraction 2, when the solution of secondary distillation becomes brown or dark brown, stops two
Grade distillation, fraction 3 is named as by the residue after secondary distillation；
B. antioxidant composition is extracted from the residue after level-one distillation in step a, the residue after level-one is distilled uses acetic acid
Ethyl ester (EtOAc) extracts three times, merges ethyl acetate phase three times, is level-one extracting solution, by level-one extracting solution 1mol/
The aqueous solution extraction of LNaOH twice, merges water phase twice, this be two level extracting solution, the level-one distillation after residue,
The volume ratio of the aqueous solution of primary ethyl acetate and primary NaOH is 3：1：1；
C. the two level extracting solution obtained in step b is acidified to pH to 2-6 with hydrochloric acid, is with ethyl acetate/n-hexane volume ratio
Two level extracting solution is further purified three times, retain organic phase, discard water phase, obtain three-level extracting solution, as detach
Antioxidant composition, the volume ratio of residue and the mixed liquor of primary ethyl acetate and n-hexane after level-one distillation
It is 3：1.
2. a kind of more effect components of wood vinegar as described in claim 1 detach and complete utilization method, it is characterised in that：
The pH is 2, and ethyl acetate/n-hexane volume ratio is named as fraction 4 for 7/3.
3. a kind of more effect components of wood vinegar as described in claim 1 detach and complete utilization method, it is characterised in that：
The pH is 3, and ethyl acetate/n-hexane volume ratio is named as fraction 5 for 7/3.
4. a kind of more effect components of wood vinegar as described in claim 1 detach and complete utilization method, it is characterised in that：
The pH is 4, and ethyl acetate/n-hexane volume ratio is named as fraction 6 for 7/3.
5. a kind of more effect components of wood vinegar as described in claim 1 detach and complete utilization method, it is characterised in that：
The pH is 4, and ethyl acetate/n-hexane volume ratio is named as fraction 7 for 1/1.
6. a kind of more effect components of wood vinegar as described in claim 1 detach and complete utilization method, it is characterised in that：
The pH is 4, and ethyl acetate/n-hexane volume ratio is named as fraction 8 for 3/7.
7. a kind of more effect components of wood vinegar as described in claim 1 detach and complete utilization method, it is characterised in that：
The pH is 5, and ethyl acetate/n-hexane volume ratio is named as fraction 9 for 7/3.
8. a kind of more effect components of wood vinegar as described in claim 1 detach and complete utilization method, it is characterised in that：Described
PH is 6, and ethyl acetate/n-hexane volume ratio is named as fraction 10 for 7/3.
9. a kind of more effect components of wood vinegar as described in claim 1 detach and complete utilization method, it is characterised in that：Described
Wood vinegar is one kind in toothed oak wood wood vinegar, jujube nucleus wood vinegar, rice husk wood vinegar, peanut shell wood vinegar, corncob wood vinegar.
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