CN107163972A - A kind of preparation method of functional food level pyrolkigneous liquid - Google Patents
A kind of preparation method of functional food level pyrolkigneous liquid Download PDFInfo
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- CN107163972A CN107163972A CN201710543497.5A CN201710543497A CN107163972A CN 107163972 A CN107163972 A CN 107163972A CN 201710543497 A CN201710543497 A CN 201710543497A CN 107163972 A CN107163972 A CN 107163972A
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- pyrolkigneous liquid
- pyrolkigneous
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C5/00—Production of pyroligneous acid distillation of wood, dry distillation of organic waste
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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- Life Sciences & Earth Sciences (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The present invention relates to a kind of preparation method of functional food level pyrolkigneous liquid.Comprise the following steps：Raw material obtains rough pyrolkigneous liquid through destructive distillation, condensation；Adopt and the rough pyrolkigneous liquid is extracted with ethyl acetate three times, merge the extract of three gained, obtain primary acetum pyrolignosum rectificatum liquid；Using 0.6mol/L NaHCO3The solution extraction primary acetum pyrolignosum rectificatum liquid three times, merges the extract of three gained, obtains secondary acetum pyrolignosum rectificatum liquid；Concentrated phosphoric acid is inserted in the secondary acetum pyrolignosum rectificatum liquid, after the color of secondary acetum pyrolignosum rectificatum liquid is changed into light yellow from claret, secondary acetum pyrolignosum rectificatum liquid is placed in flask and distilled, collect the cut between 97 100 DEG C；It is to be distilled to finish, cut is shaken up, active carbon powder is added, decolourized in water-bath, suction filtration obtains food-grade pyrolkigneous liquid.Food-grade pyrolkigneous liquid prepared by the method for the invention not only eliminates a large amount of poisonous aldehydes matters and aldehyde material, and remains the micro aldehydes matter beneficial to human body.
Description
Technical field
The present invention relates to a kind of preparation method of functional food level pyrolkigneous liquid.
Background technology
Pyrolkigneous liquid is a kind of yellowish-brown liquid containing materials such as acids, ketone, phenols.People for it application it is earliest
Originating from ancient Chinese, for resolving sputum etc..In modern age, be at first Japan using the country of pyrolkigneous liquid.By development for many years, people
Find that pyrolkigneous liquid can treat the intestines problem of human body, skin disease, or even also have certain curative effect to cardiovascular and cerebrovascular disease.
Pyrolkigneous liquid has been made health care green beverage by South Korea, people.But, the country is to pyrolkigneous liquid in field of food and drug field
Research be almost blank.Because pyrolkigneous liquid contains a variety of harmful materials, such as phenol, the carcinogenic substance such as BaP
Matter, so pyrolkigneous liquid has to pass through polishing purification and just can apply to food and medicine.The wooden vinegar of food-grade commonly used in the world at present
The preparation method of liquid is multi-step pressure reduction distillation, and the poisonous and harmful substance in pyrolkigneous liquid is separated step by step.Although the method can be obtained
To more pure safe food-grade pyrolkigneous liquid, but the method takes time and effort and expensive.
The food-grade pyrolkigneous liquid preparation method in current more forward position also has distillation-ozone-ultraviolet line combined method, although this side
Method can effectively remove the carcinogens such as phenol in pyrolkigneous liquid, tar, but still contain part aldehydes noxious material and yield
It is relatively low.
In summary, the problem of preparation method of current food-grade pyrolkigneous liquid has more and defect.Therefore, it is necessary to
Effective technical scheme is proposed, is solved the above problems.
The content of the invention
In order to overcome the technological deficiency of the above and promote pyrolkigneous liquid in the extensive use of food and medical domain, purport of the present invention
Proposing the preparation method of functional food level pyrolkigneous liquid a kind of easy to operate and efficient, inexpensive.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：
A kind of preparation method of functional food level pyrolkigneous liquid, comprises the following steps：
(1) raw material obtains rough pyrolkigneous liquid through destructive distillation, condensation；The raw material is that toothed oak is wooden, jujube nucleus, corncob, walnut shell,
One kind in rice husk and peanut shell；
(2) adopt and the rough pyrolkigneous liquid is extracted with ethyl acetate three times, merge the extract of three gained, obtain primary essence
Pyrolkigneous liquid processed；
(3) using 0.6mol/L NaHCO3The solution extraction primary acetum pyrolignosum rectificatum liquid three times, merges three gained
Extract, obtains secondary acetum pyrolignosum rectificatum liquid；
(4) concentrated phosphoric acid is inserted in the secondary acetum pyrolignosum rectificatum liquid, treats that the color of secondary acetum pyrolignosum rectificatum liquid is become by claret
After light yellow, secondary acetum pyrolignosum rectificatum liquid is placed in flask and distilled, collect the cut between 97-100 DEG C；
(5) it is to be distilled to finish, cut is shaken up, active carbon powder is added, decolourized in water-bath, suction filtration obtains the wooden vinegar of food-grade
Liquid.
It is preferred that, ethyl acetate described in step (2) extracts rough pyrolkigneous liquid three times, and extraction process is：By same volume
Ethyl acetate add in three times in rough pyrolkigneous liquid, at room temperature vibrate 5 minutes, stratification.
The volume ratio of rough pyrolkigneous liquid and ethyl acetate is used for 1:1, this ratio can ensure that in pyrolkigneous liquid beyond tar removing
Other extracting substances it is complete；And a point three-level extraction is extracted with ethyl acetate than once, effect of extracting is more preferable；And point three-level extraction
Than being once extracted with ethyl acetate, effect of extracting is more preferable.
It is preferred that, NaHCO described in step (3)3Solution extracts primary acetum pyrolignosum rectificatum liquid three times, and extraction process is：Will be same
The 0.6mol/L of sample volume NaHCO3Solution is added in primary acetum pyrolignosum rectificatum liquid in three times, is vibrated 5 minutes at room temperature, is stood
Layering.
Using secondary acetum pyrolignosum rectificatum liquid and NaHCO3The volume ratio of solution is 1:1, this ratio can ensure that acetic acid in pyrolkigneous liquid
Extraction is complete；And a point three-level extraction is extracted with ethyl acetate than once, effect of extracting is more preferable.
It is preferred that, the volume ratio of secondary acetum pyrolignosum rectificatum liquid and concentrated phosphoric acid is 1 described in step (4):25.
The volume ratio of secondary acetum pyrolignosum rectificatum liquid and concentrated phosphoric acid is used for 1:25, can accurate adjustment pyrolkigneous liquid pH value, it is ensured that
The acid content of pyrolkigneous liquid is optimal.
It is preferred that, the mass ratio of active carbon powder and cut described in step (5) is 1:60.
It is preferred that, the condition decolourized described in step (5) in water-bath is specially：Bath temperature is 40 DEG C, and water bath time is
30min, and swayed once every 10min.
The present invention also provides a kind of functional food level pyrolkigneous liquid, according to the preparation side of above-mentioned functions food-grade pyrolkigneous liquid
The food-grade pyrolkigneous liquid that method is prepared.
The present invention also provides a kind of application of functional food level pyrolkigneous liquid in field of health care products, the functional food
Level pyrolkigneous liquid is prepared according to the preparation method of above-mentioned functions food-grade pyrolkigneous liquid.
Beneficial effect：Food-grade pyrolkigneous liquid prepared by the method for the invention not only eliminates a large amount of poisonous aldehydes matters
And aldehyde material, and remain the micro aldehydes matter beneficial to human body such as 2- metoxyphenols, 2,6- syringol,
Both aldehydes matters have very strong antioxygenic property and radical scavenging activity, and particularly 2,6- xylenols have very
Strong radical scavenging activity, contributes to the food-grade pyrolkigneous liquid prepared by the present invention to be applied to the fields such as health products.
Brief description of the drawings
Some specific embodiments of the present invention are described in detail by way of example, and not by way of limitation with reference to the accompanying drawings hereinafter.
Identical reference denotes same or similar part or part in accompanying drawing.It should be appreciated by those skilled in the art that these
What accompanying drawing was not necessarily drawn to scale.In accompanying drawing：
Fig. 1 is rough jujube nucleus pyrolkigneous liquid, primary refined jujube nucleus pyrolkigneous liquid, the GC- of food-grade pyrolkigneous liquid composition contrast
MS spectrograms.
Embodiment
The present invention relates to a kind of preparation method of functional food level pyrolkigneous liquid, this method steams the first solvent extraction of raw material again
Evaporate, obtain functional food level pyrolkigneous liquid.Contain micro 2- metoxyphenols, 2,6- diformazans in functional food level pyrolkigneous liquid
Epoxide phenol, under the acid condition of pyrolkigneous liquid inherently, with very strong radicals scavenging effect, has medical treatment well to protect
Strong effect.
It is that rough pyrolkigneous liquid first is made by raw material that the Materials Solvents extraction process, which is specifically, then to primary acetum pyrolignosum rectificatum liquid,
Secondary acetum pyrolignosum rectificatum liquid is arrived again.
Functional food level pyrolkigneous liquid of the present invention is different according to selected raw material, can prepare the wooden pyrolkigneous liquid of toothed oak, jujube nucleus
Pyrolkigneous liquid, corncob pyrolkigneous liquid, walnut shell pyrolkigneous liquid, rice husk pyrolkigneous liquid, peanut shell pyrolkigneous liquid etc..
The method that the present invention is combined using solvent extraction and distillation, is cheap and efficient functional food level wood
The preparation method of vinegar liquid, has obtained more pure and safe functional food level pyrolkigneous liquid.
As one embodiment of the present of invention, raw material is to obtain rough pyrolkigneous liquid through destructive distillation, condensation, wherein, destructive distillation, condensation
Technique takes conventional existing process, such as specific destructive distillation, condensation process can be：A destructive distillation：Raw material is put into charcoal kiln, entered
Row heating destructive distillation；B is condensed：After the gas flue gas separation that destructive distillation is produced, yellowish-brown gas part is condensed, is collected in condensing unit
Component between 90-170 DEG C, obtains rough pyrolkigneous liquid.
As one embodiment of the present of invention, Materials Solvents reconcile pH value redistillation, institute of the present invention after extracting through concentrated phosphoric acid
When stating concentrated phosphoric acid conciliation PH, the volume ratio of secondary acetum pyrolignosum rectificatum liquid and concentrated phosphoric acid is 1:25 (V/V) are important, and aldehydes matter can
To be changed into molecular state from ionic state completely, while can also avoid introducing excessive acetic acid, and the food-grade that this ratio is obtained
Pyrolkigneous liquid acetic acid content is more, is also the optimum pH value of food-grade pyrolkigneous liquid (PH is 3).
It is to collect the cut between 97-100 DEG C during distillation, vapo(u)rizing temperature needs strict as one embodiment of the present of invention
Control, to prevent bringing excess moisture and poisonous and harmful substances into.
Embodiment 1
The present invention relates to a kind of preparation method of feature jujube nucleus food-grade pyrolkigneous liquid, comprise the following steps：
(1) jujube nucleus obtain rough pyrolkigneous liquid through destructive distillation, condensation；
(2) adopt and the rough pyrolkigneous liquid is extracted with ethyl acetate three times, merge the extract of three gained, obtain primary essence
Pyrolkigneous liquid processed；The technique for wherein extracting the rough pyrolkigneous liquid three times is specially：300mL ethyl acetate is added in three times
In the rough pyrolkigneous liquid of 300mL, 100mL is added every time, is to vibrate 5 minutes at room temperature every time, stratification, aqueous phase discarded,
Leave organic phase；
(3) using 0.6mol/L NaHCO3The solution extraction primary acetum pyrolignosum rectificatum liquid three times, merges three gained
Extract, obtains secondary acetum pyrolignosum rectificatum liquid；Wherein extraction process is specially：By 300mL0.6mol/L NaHCO3Solution point three
In the primary acetum pyrolignosum rectificatum liquid of secondary addition 300mL, 100mL is added every time, is to vibrate 5 minutes at room temperature every time, stratification,
Aqueous phase discarded, leaves organic phase；NaHCO of the present invention3Solution is important, this concentration relationship to wooden vinegar using 0.6mol/L
Whether acid can be kept completely separate in liquid, using the NaHCO of secondary concentration3Acid can be complete in solution, pyrolkigneous liquid
Separation；
(4) 2500mL concentrated phosphoric acids are inserted in secondary acetum pyrolignosum rectificatum liquid described in 100mL, treats the color of secondary acetum pyrolignosum rectificatum liquid
After being changed into light yellow from claret, secondary acetum pyrolignosum rectificatum liquid is placed in flask and distilled, collect the cut between 97-100 DEG C；This
It is important that temperature is collected in invention distillation, is only limitted to collect the cut between 97-100 DEG C；
(5) it is to be distilled to finish, cut is shaken up, active carbon powder is added, decolourized in water-bath, it is decolourized complete, suction filtration
Obtain food-grade pyrolkigneous liquid.The mass ratio of the active carbon powder and cut is 1:60；The condition decolourized in the water-bath is specific
For：Bath temperature is 40 DEG C, and water bath time is 30min, and swayed once every 10min.
Table 1 is the main matter and content table in the jujube nucleus pyrolkigneous liquid obtained by GC/MS-SCAN scanning analysis.
Main matter and content table in the jujube nucleus pyrolkigneous liquid of table 1
| Sequence number | Compound name | Retention time (min) | Percentage contents (%) |
| 1 | 1- hydroxyl -2- acetone | 4.44 | 2.21 |
| 2 | 2- cyclopentene-1-ones | 5.598 | 0.69 |
| 3 | Acetic acid | 7.08 | 95.48 |
| 4 | Propionic acid | 9.068 | 1.55 |
The content of acetic acid how much be a critically important food-grade pyrolkigneous liquid criterion.As shown in table 1, this hair is utilized
The jujube nucleus food-grade pyrolkigneous liquid that bright preparation method is obtained, the content of acetic acid is up to 95.48%, and the content of propionic acid is
1.55%.
Fig. 1 is rough jujube nucleus pyrolkigneous liquid, primary refined jujube nucleus pyrolkigneous liquid, the GC- of food-grade pyrolkigneous liquid composition contrast
MS spectrograms.As shown in figure 1, rough pyrolkigneous liquid is first made through preparation method of the present invention in raw material, then to primary acetum pyrolignosum rectificatum liquid, finally
To food-grade pyrolkigneous liquid, eliminate a large amount of poisonous and harmful substances such as phenol, and acetic acid yield also close to second in rough pyrolkigneous liquid
The content of acid.
Embodiment 2
Embodiment 2 is identical with the preparation method of embodiment 1.It the difference is that only, the raw material in embodiment 1 is acid
Jujube core, the product that embodiment 1 is obtained is jujube nucleus food-grade pyrolkigneous liquid；And the raw material in embodiment two is toothed oak wood, implement
The product that example 2 is obtained is the wooden food-grade pyrolkigneous liquid of toothed oak.
Table 2 is the refined front and rear constituent content contrast table of the wooden food-grade pyrolkigneous liquid of toothed oak obtained by the present invention.
The rough toothed oak of table 2 wood pyrolkigneous liquid and the wooden food-grade pyrolkigneous liquid constituent content contrast table of toothed oak
As shown in table 2, the food-grade pyrolkigneous liquid that prepared by the method for the invention not only eliminates a large amount of poisonous phenolic materials
Matter and aldehyde material, and remain the micro aldehydes matter beneficial to human body such as 2- metoxyphenols, 2,6- dimethoxy benzenes
Phenol, both aldehydes matters have very strong antioxygenic property and radical scavenging activity, particularly 2,6- xylenols tool
There is very strong radical scavenging activity, contribute to the food-grade pyrolkigneous liquid prepared by the present invention to be applied to the fields such as health products.
The present invention can be summarized with others without prejudice to the concrete form of the spirit or essential characteristics of the present invention.Therefore, nothing
By from the point of view of which point, the embodiment above of the invention can only all be considered the description of the invention and can not limit this hair
Bright, claims indicate the scope of the present invention, and above-mentioned explanation does not point out the scope of the present invention, therefore, with this
Any change in claims of invention suitable implication and scope, is all considered as being included in the claim of the present invention
In the range of book.
Claims (8)
1. a kind of preparation method of functional food level pyrolkigneous liquid, it is characterised in that comprise the following steps：
(1) raw material obtains rough pyrolkigneous liquid through destructive distillation, condensation；The raw material is toothed oak wood, jujube nucleus, corncob, walnut shell, rice husk
With one kind in peanut shell；
(2) adopt and the rough pyrolkigneous liquid is extracted with ethyl acetate three times, merge the extract of three gained, obtain primary refined wood
Vinegar liquid；
(3) using 0.6mol/L NaHCO3The solution extraction primary acetum pyrolignosum rectificatum liquid three times, merges the extraction of three gained
Liquid, obtains secondary acetum pyrolignosum rectificatum liquid；
(4) concentrated phosphoric acid is inserted in the secondary acetum pyrolignosum rectificatum liquid, treats that the color of secondary acetum pyrolignosum rectificatum liquid is changed into shallow from claret
After yellow, secondary acetum pyrolignosum rectificatum liquid is placed in flask and distilled, collect the cut between 97-100 DEG C；
(5) it is to be distilled to finish, cut is shaken up, active carbon powder is added, decolourized in water-bath, suction filtration obtains food-grade pyrolkigneous liquid.
2. the preparation method of functional food level pyrolkigneous liquid as claimed in claim 1, it is characterised in that described in step (2)
Ethyl acetate extracts rough pyrolkigneous liquid three times, and extraction process is：The ethyl acetate of same volume is added into rough wooden vinegar in three times
In liquid, vibrate 5 minutes at room temperature, stratification.
3. the preparation method of functional food level pyrolkigneous liquid as claimed in claim 2, it is characterised in that described in step (3)
NaHCO3Solution extracts primary acetum pyrolignosum rectificatum liquid three times, and extraction process is：By the 0.6mol/L of same volume NaHCO3Solution point
In the primary acetum pyrolignosum rectificatum liquid of three additions, vibrate 5 minutes at room temperature, stratification.
4. the preparation method of functional food level pyrolkigneous liquid as claimed in claim 3, it is characterised in that described in step (4)
The volume ratio of secondary acetum pyrolignosum rectificatum liquid and concentrated phosphoric acid is 1:25.
5. the preparation method of functional food level pyrolkigneous liquid as claimed in claim 4, it is characterised in that described in step (5)
The mass ratio of active carbon powder and cut is 1:60.
6. the preparation method of functional food level pyrolkigneous liquid as claimed in claim 5, it is characterised in that described in step (5)
The condition decolourized in water-bath is specially：Bath temperature is 40 DEG C, and water bath time is 30min, and swayed once every 10min.
7. a kind of functional food level pyrolkigneous liquid, it is characterised in that according to any one of the 1-6 wooden vinegar of functional food level
The food-grade pyrolkigneous liquid that the preparation method of liquid is prepared.
8. a kind of application of functional food level pyrolkigneous liquid in field of health care products, it is characterised in that the functional food level
Pyrolkigneous liquid is prepared according to the preparation method of any one of the 1-6 functional food level pyrolkigneous liquid.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108530288A (en) * | 2018-05-18 | 2018-09-14 | 吉林大学 | A kind of more effect components separation of wood vinegar and complete utilization method |
| CN108719215A (en) * | 2018-03-28 | 2018-11-02 | 宜州市壮之都丝绸家纺有限公司 | A kind of high-yield cultivation method of silkworm |
| CN111635760A (en) * | 2020-06-30 | 2020-09-08 | 中国林业科学研究院林产化学工业研究所 | Preparation method and application of wood vinegar rich in phenols |
| CN111646882A (en) * | 2020-04-10 | 2020-09-11 | 吉林大学 | Efficient and environment-friendly method for extracting functional phenolic substances from pyroligneous liquor |
| CN113575010A (en) * | 2021-08-12 | 2021-11-02 | 上海景观实业发展有限公司 | Saline-alkali soil planting method |
| JP2022025685A (en) * | 2020-07-29 | 2022-02-10 | キユーピー株式会社 | Vinegar, food and drink, method for giving smoke flavor, and method for masking unpleasant odor |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108719215A (en) * | 2018-03-28 | 2018-11-02 | 宜州市壮之都丝绸家纺有限公司 | A kind of high-yield cultivation method of silkworm |
| CN108530288A (en) * | 2018-05-18 | 2018-09-14 | 吉林大学 | A kind of more effect components separation of wood vinegar and complete utilization method |
| CN111646882A (en) * | 2020-04-10 | 2020-09-11 | 吉林大学 | Efficient and environment-friendly method for extracting functional phenolic substances from pyroligneous liquor |
| CN111635760A (en) * | 2020-06-30 | 2020-09-08 | 中国林业科学研究院林产化学工业研究所 | Preparation method and application of wood vinegar rich in phenols |
| JP2022025685A (en) * | 2020-07-29 | 2022-02-10 | キユーピー株式会社 | Vinegar, food and drink, method for giving smoke flavor, and method for masking unpleasant odor |
| CN113575010A (en) * | 2021-08-12 | 2021-11-02 | 上海景观实业发展有限公司 | Saline-alkali soil planting method |
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