CN108434782A - The enrichment method of acid and aldehydes matter in a kind of wood vinegar - Google Patents
The enrichment method of acid and aldehydes matter in a kind of wood vinegar Download PDFInfo
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- CN108434782A CN108434782A CN201810350267.1A CN201810350267A CN108434782A CN 108434782 A CN108434782 A CN 108434782A CN 201810350267 A CN201810350267 A CN 201810350267A CN 108434782 A CN108434782 A CN 108434782A
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- acid
- aldehydes matter
- wood vinegar
- ether
- extractant
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0492—Applications, solvents used
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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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses the enrichment method of acid and aldehydes matter in a kind of wood vinegar, crude pyroligneous acid carries out that acetum pyrolignosum rectificatum liquid is obtained by extraction using extractant, and the extractant is the mixed extractant that ether and methanol mix.The ether is with methanol according to volume ratio 1~5:1 is mixed.Acid and aldehydes matter content are up to 26.91% and 63.18% in the acetum pyrolignosum rectificatum liquid.Using hybrid extraction liquid after mixed extractant repeatedly extraction when extraction, stands under extract liquor room temperature and volatilize up to acetum pyrolignosum rectificatum liquid.The present invention selects ether and methanol mixed extractant, by adjusting the two mixing ratio, make full use of methanol ether highly polar and molten effect altogether, effectively it is enriched acid and aldehydes matter in wood vinegar, acid and aldehydes matter content greatly improve the orientation refining effect of wood vinegar up to 26.91% and 63.18%.
Description
Technical field
The invention belongs to biomass energy technology field, acid and aldehydes matter in a kind of wood vinegar are related generally to
Enrichment method.
Background technology
China is large agricultural country, while forest resourceies also enrich, therefore utilizable biomass resource reserves very may be used
It sees.Effective comprehensive utilization of biomass resource, is not only able to turn waste into wealth, it helps reduces waste pollution, meets China
Development tactics.According to statistics, the agriculture and forestry organic waste material that China generates every year reaches as many as several hundred million tons, wherein utilized by thermochemical study
About 50% or so.Wood vinegar is a major product during biomass thermal chemical conversion utilizes, and yield is huge.Wood vinegar
The dry distillation of wood derived from middle period the 17th century is gathered up, is started in middle period the 1990s after being passed to Japan the eighties in 18th century
It is a large amount of to develop and utilize research work.Early stage wood vinegar is mainly applied to the industry production such as production acetic acid, methanol and acetone
Product, but with the rise of compound probability and fermentation industry, high-cost dry distillation of wood industry has gradually exited the arena of history.Closely
Over a little years, research and the application of wood vinegar enter new developing stage, initially as bacteriostatic agent, insecticide, antioxidant with
And plant growth regulator etc. is applied to the fields such as medicine, food and pesticide.
The main component of wood vinegar is water, while also having unit containing acids, phenols, alcohols, aldoketones and esters etc.
Point.Therefore, by refining a large amount of moisture and harmful tar ingredient in removal wood vinegar and being targetedly enriched with organic component
It is the premise that wood vinegar is efficient, comprehensively utilizes.The common process for purification of wood vinegar mainly have settled process, the way of distillation, extraction and
Filtration method etc. is several, and wherein extraction is widely used due to easy to operate, significant effect.Ether is commonly to extract
Agent, but since polarity is relatively weak, refining effect is to be improved.Therefore, the extractant that a kind of polarity is strong, is easily isolated is explored,
Refined for wood vinegar has great importance, it helps the comprehensive high-efficiency of wood vinegar utilizes.
Invention content
The purpose of the invention is to overcome in the prior art the disadvantage that enrichment is weak, refining effect is poor, one is provided
The enrichment method of acid and aldehydes matter, simple for process in kind wood vinegar, being capable of mild, green, effective enrichment wood vinegar
Acid and aldehydes matter in liquid.
The technical scheme is that：The enrichment method of acid and aldehydes matter, crude pyroligneous acid in a kind of wood vinegar
It carries out that acetum pyrolignosum rectificatum liquid is obtained by extraction using extractant, the extractant is the hybrid extraction that ether and methanol mix
Agent, acid content ＞ 19%, aldehydes matter content ＞ 58% in the acetum pyrolignosum rectificatum liquid.
The ether is with methanol according to volume ratio 1~5:1 is mixed.
The volume ratio of the crude pyroligneous acid and ether-methanol mixed extractant is 2~5:1.
Using hybrid extraction liquid after mixed extractant repeatedly extraction when extraction.
It stands and is volatilized up to acetum pyrolignosum rectificatum liquid under extract liquor room temperature.
Advantageous effect：
1. methanol and ether mixed preparing are obtained mixed extractant by the present invention, by enhance the polarity of mixed extractant come
Extraction ability is promoted, acid and aldehydes matter in wood vinegar is effectively enriched, greatly improves the orientation of wood vinegar
Refining effect.
2. preparation method operating procedure is simple, mild, green, efficient, there is fine promotion potential.
Specific implementation mode
Embodiment 1：
Crude pyroligneous acid is stood at normal temperatures, it is spare；It is accurate to measure 10ml crude pyroligneous acids, it is 1 with 3ml volume ratios:1 second
Ether-methanol extracting mixed extractant crude pyroligneous acid 6 times merges the extract liquor of 6 gained, obtains acetum pyrolignosum rectificatum liquid, with GC-MS points
Analyse the component of acetum pyrolignosum rectificatum liquid.Analysis result is shown：For acid content up to 19.56%, aldehydes matter content is reachable
57.39%.Wherein acid main component is acetic acid, propionic acid, and aldehydes matter main component is phenol, 2- methylphenols, 4-
Methylphenol, 2- metoxyphenols, 4- ethyl -phenols, 2- methoxyl group -4- ethyl -phenols, 2,4- xylenols etc..
Embodiment 2：
Crude pyroligneous acid is stood at normal temperatures, it is spare；It is accurate to measure 10ml crude pyroligneous acids, it is 1 with 2ml volume ratios:1 second
Ether-methanol extracting mixed extractant crude pyroligneous acid 6 times merges the extract liquor of 6 gained, obtains acetum pyrolignosum rectificatum liquid, with GC-MS points
Analyse the component of acetum pyrolignosum rectificatum liquid.Analysis result is shown：For acid content up to 17.34%, aldehydes matter content is reachable
56.26%.Wherein acid main component is acetic acid, propionic acid, and aldehydes matter main component is phenol, 2- methylphenols, 4-
Methylphenol, 2- metoxyphenols, 4- ethyl -phenols, 2- methoxyl group -4- ethyl -phenols, 2,4- xylenols etc..
Embodiment 3：
Crude pyroligneous acid is stood at normal temperatures, it is spare；It is accurate to measure 10ml crude pyroligneous acids, it is 1 with 4ml volume ratios:1 second
Ether-methanol extracting mixed extractant crude pyroligneous acid 6 times merges the extract liquor of 6 gained, obtains acetum pyrolignosum rectificatum liquid, with GC-MS points
Analyse the component of acetum pyrolignosum rectificatum liquid.Analysis result is shown：For acid content up to 19.79%, aldehydes matter content is reachable
57.06%.Wherein acid main component is acetic acid, propionic acid, and aldehydes matter main component is phenol, 2- methylphenols, 4-
Methylphenol, 2- metoxyphenols, 4- ethyl -phenols, 2- methoxyl group -4- ethyl -phenols, 2,4- xylenols etc..
Embodiment 4：
Crude pyroligneous acid is stood at normal temperatures, it is spare；It is accurate to measure 10ml crude pyroligneous acids, it is 1 with 5ml volume ratios:1 second
Ether-methanol extracting mixed extractant crude pyroligneous acid 6 times merges the extract liquor of 6 gained, obtains acetum pyrolignosum rectificatum liquid, with GC-MS points
Analyse the component of acetum pyrolignosum rectificatum liquid.Analysis result is shown：For acid content up to 19.71%, aldehydes matter content is reachable
57.40%.Wherein acid main component is acetic acid, propionic acid, and aldehydes matter main component is phenol, 2- methylphenols, 4-
Methylphenol, 2- metoxyphenols, 4- ethyl -phenols, 2- methoxyl group -4- ethyl -phenols, 2,4- xylenols etc..
Embodiment 5：
Crude pyroligneous acid is stood at normal temperatures, it is spare；It is accurate to measure 10ml crude pyroligneous acids, it is 2 with 3ml volume ratios:1 second
Ether-methanol extracting mixed extractant crude pyroligneous acid 6 times merges the extract liquor of 6 gained, obtains acetum pyrolignosum rectificatum liquid, with GC-MS points
Analyse the component of acetum pyrolignosum rectificatum liquid.Analysis result is shown：For acid content up to 19.43%, aldehydes matter content is reachable
59.39%.Wherein acid main component is acetic acid, propionic acid, and aldehydes matter main component is phenol, 2- methylphenols, 4-
Methylphenol, 2- metoxyphenols, 4- ethyl -phenols, 2- methoxyl group -4- ethyl -phenols etc..
Embodiment 6：
Crude pyroligneous acid is stood at normal temperatures, it is spare；It is accurate to measure 10ml crude pyroligneous acids, it is 3 with 3ml volume ratios:1 second
Ether-methanol extracting mixed extractant crude pyroligneous acid 6 times merges the extract liquor of 6 gained, obtains acetum pyrolignosum rectificatum liquid, with GC-MS points
Analyse the component of acetum pyrolignosum rectificatum liquid.Analysis result is shown：For acid content up to 24.37%, aldehydes matter content is reachable
64.14%.Wherein acid main component is acetic acid, propionic acid, and aldehydes matter main component is phenol, 2- methylphenols, 4-
Methylphenol, 2- metoxyphenols, 4- ethyl -phenols, 2- methoxyl group -4- ethyl -phenols, 4- ethyl -2- metoxyphenols etc..
Embodiment 7：
Crude pyroligneous acid is stood at normal temperatures, it is spare；It is accurate to measure 10ml crude pyroligneous acids, it is 4 with 3ml volume ratios:1 second
Ether-methanol extracting mixed extractant crude pyroligneous acid 6 times merges the extract liquor of 6 gained, obtains acetum pyrolignosum rectificatum liquid, with GC-MS points
Analyse the component of acetum pyrolignosum rectificatum liquid.Analysis result is shown：For acid content up to 29.35%, aldehydes matter content is reachable
62.55%.The main component of wherein acid is acetic acid, propionic acid, butyric acid, valeric acid, and aldehydes matter main component is phenol, 2-
Methylphenol, 4- methylphenols, 2- metoxyphenols, 4- ethyl -phenols, 2- methoxyl group -4- ethyl -phenols etc..
Embodiment 8：
Crude pyroligneous acid is stood at normal temperatures, it is spare；It is accurate to measure 10ml crude pyroligneous acids, it is 5 with 3ml volume ratios:1 second
Ether-methanol extracting mixed extractant crude pyroligneous acid 6 times merges the extract liquor of 6 gained, obtains acetum pyrolignosum rectificatum liquid, with GC-MS points
Analyse the component of acetum pyrolignosum rectificatum liquid.Analysis result is shown：For acid content up to 23.81%, aldehydes matter content is reachable
63.37%.The main component of wherein acid is acetic acid, propionic acid, butyric acid, and aldehydes matter main component is phenol, 2- methyl
Phenol, 4- methylphenols, 2- metoxyphenols, 4- ethyl -phenols, 2- methoxyl group -4- ethyl -phenols, 2,4- xylenols etc..
Embodiment 9：
Crude pyroligneous acid is stood at normal temperatures, it is spare；It is accurate to measure 10ml crude pyroligneous acids, it is 3 with 3ml volume ratios:1 second
Ether-methanol extracting mixed extractant crude pyroligneous acid 6 times merges the extract liquor of 6 gained, and the mixed extractant that volatilizees at room temperature obtains
To acetum pyrolignosum rectificatum liquid, the component of acetum pyrolignosum rectificatum liquid is analyzed with GC-MS.Analysis result is shown：Acid content is reachable
25.99%, aldehydes matter content is up to 62.88%.Wherein acid main component is acetic acid, propionic acid, and aldehydes matter is main
Ingredient be phenol, 2- methylphenols, 4- methylphenols, 2- metoxyphenols, 4- ethyl -phenols, 2- methoxyl group -4- ethyl -phenols,
4- ethyl -2- metoxyphenols etc..
Embodiment 10：
Crude pyroligneous acid is stood at normal temperatures, it is spare；It is accurate to measure 10ml crude pyroligneous acids, it is 4 with 3ml volume ratios:1 second
Ether-methanol extracting mixed extractant crude pyroligneous acid 6 times merges the extract liquor of 6 gained, and the mixed extractant that volatilizees at room temperature obtains
To acetum pyrolignosum rectificatum liquid, the component of acetum pyrolignosum rectificatum liquid is analyzed with GC-MS.Analysis result is shown：Acid content is reachable
29.91%, aldehydes matter content is up to 63.18%.The main component of wherein acid is acetic acid, propionic acid, butyric acid, valeric acid,
Aldehydes matter main component is phenol, 2- methylphenols, 4- methylphenols, 2- metoxyphenols, 4- ethyl -phenols, 2- methoxies
Base -4- ethyl -phenols, 4- ethyl -2- metoxyphenols etc..
1 example of table, 10 acetum pyrolignosum rectificatum liquid GC-MS analysis results
Comparative example 1：
Crude pyroligneous acid is stood at normal temperatures, it is spare；It is accurate to measure 10ml crude pyroligneous acids, extract acetum pyrolignosum crudum with 3ml ether
Liquid 6 times merges the extract liquor of 6 gained, and the component of acetum pyrolignosum rectificatum liquid is analyzed with GC-MS.Analysis result is shown：Acid contains
Amount is 16.14%, and aldehydes matter content is up to 52.48%.The main component of wherein acid is acetic acid, propionic acid, butyric acid, phenol
Substance main component is phenol, 2- methylphenols, 4- methylphenols, 2- metoxyphenols, 4- ethyl -phenols, 2- methoxyl groups-
4- ethyl -phenols, 4- ethyl -2- metoxyphenols etc..
2 comparative example of table, 1 acetum pyrolignosum rectificatum liquid GC-MS analysis results
Comparative example 2：
Crude pyroligneous acid is stood at normal temperatures, it is spare；It is accurate to measure 10ml crude pyroligneous acids, it is extracted with 3ml ethyl acetate thick
Wood vinegar 6 times merges the extract liquor of 6 gained, ethyl acetate is steamed at 80 DEG C, and the group of acetum pyrolignosum rectificatum liquid is analyzed with GC-MS
Point.Analysis result is shown：Acid content position 17.04%, aldehydes matter content is up to 53.07%.Wherein acid
Main component is acetic acid, propionic acid, butyric acid, valeric acid, and aldehydes matter main component is phenol, 2- methylphenols, 4- methylphenols, 2-
Metoxyphenol, 4- ethyl -phenols, 2- methoxyl group -4- ethyl -phenols, 2- methoxyl group -5- methylphenols etc..
3 comparative example of table, 2 acetum pyrolignosum rectificatum liquid GC-MS analysis results
Comparative example 3：
Crude pyroligneous acid is stood at normal temperatures, it is spare；It is accurate to measure 10ml crude pyroligneous acids, with 3ml chloroform extraction agent
It extracts crude pyroligneous acid 6 times, merges the extract liquor of 6 gained, the component of acetum pyrolignosum rectificatum liquid is analyzed with GC-MS.Analysis result is shown：
Acid content position 12.39%, aldehydes matter content is up to 46.72%.The main component of wherein acid is acetic acid, phenol
Substance main component is phenol, 2- methylphenols, 4- methylphenols, 2- metoxyphenols, 4- ethyl -phenols, 2- methoxyl groups-
5- methylphenols etc..
4 comparative example of table, 3 acetum pyrolignosum rectificatum liquid GC-MS analysis results
Comparative example 4：
Crude pyroligneous acid is stood at normal temperatures, it is spare；It is accurate to measure 10ml crude pyroligneous acids, it is 3 with 3ml volume ratios:1 second
Ether-ethyl acetate extracting mixed extractant crude pyroligneous acid 6 times merges the extract liquor of 6 gained, and acetum pyrolignosum rectificatum is analyzed with GC-MS
The component of liquid.Analysis result is shown：Acid content position 20.25%, aldehydes matter content is up to 57.99%.Wherein acids
The main component of substance is acetic acid, propionic acid, butyric acid, valeric acid, and aldehydes matter main component is phenol, 2- methylphenols, 4- methyl
Phenol, 2- metoxyphenols, 4- ethyl -phenols, 2- methoxyl group -4- ethyl -phenols, 2- methoxyl group -5- methylphenols, 2,6 diformazans
Oxygroup phenol etc..
5 comparative example of table, 4 acetum pyrolignosum rectificatum liquid GC-MS analysis results
In the research process of the present invention, inventor has selected common extractant such as ether, second to the extraction of crude pyroligneous acid
Acetoacetic ester and chloroform.Result of study shows that three kinds of extractants all have crude pyroligneous acid certain extracting and refining effect.Comparison
Ether extraction, ethyl acetate extracts and chloroform extraction, and the post-processing that ether extracts is by a relatively simple (under room temperature
Volatilization), and ethyl acetate, chloroform (need heating, rotate) post-processing complex, therefore inventor selects ether extraction.
But since its sufficiently complex component of crude pyroligneous acid component is miscible with water, the polarity of water is stronger, causes ether effect of extracting inadequate
It is ideal to be improved.Therefore inventor selects the stronger extractant of polarity to be mixed with mixed extractant with ether, passes through enhancing
The polarity of extractant improves effect of extracting.It is configured after being mixed by certain proportion with ether eventually by research discovery methanol
Mixed extractant has preferable effect of extracting.
Claims (5)
1. the enrichment method of acid and aldehydes matter in a kind of wood vinegar, crude pyroligneous acid are obtained by extraction using extractant
Acetum pyrolignosum rectificatum liquid, which is characterized in that the extractant is the mixed extractant that ether and methanol mix, and described is refined
Acid content ＞ 19%, aldehydes matter content ＞ 58% in wood vinegar.
2. the enrichment method of acid and aldehydes matter in wood vinegar as described in claim 1, which is characterized in that described
Ether is with methanol according to volume ratio 1 ~ 5：1 is mixed.
3. the enrichment method of acid and aldehydes matter in wood vinegar as described in claim 1, which is characterized in that described
The volume ratio of crude pyroligneous acid and ether-methanol mixed extractant is 2 ~ 5:1.
4. the enrichment method of acid and aldehydes matter in wood vinegar as described in claim 1, which is characterized in that when extraction
Hybrid extraction liquid after repeatedly being extracted using mixed extractant.
5. the enrichment method of acid and aldehydes matter in wood vinegar as described in claim 1, which is characterized in that extract liquor
It stands and is volatilized up to acetum pyrolignosum rectificatum liquid under room temperature.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN112602785A (en) * | 2020-11-19 | 2021-04-06 | 江苏利田科技股份有限公司 | Fat-soluble natural antioxidant and preparation method and application thereof |
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| CN105132001A (en) * | 2015-09-11 | 2015-12-09 | 江苏振宇环保科技有限公司 | Method for reducing wood tar in preparation process of wood vinegar |
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| CN105132001A (en) * | 2015-09-11 | 2015-12-09 | 江苏振宇环保科技有限公司 | Method for reducing wood tar in preparation process of wood vinegar |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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Application publication date: 20180824 |