CN109321266A - The preparation method of wood vinegar - Google Patents

The preparation method of wood vinegar Download PDF

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Publication number
CN109321266A
CN109321266A CN201811289293.4A CN201811289293A CN109321266A CN 109321266 A CN109321266 A CN 109321266A CN 201811289293 A CN201811289293 A CN 201811289293A CN 109321266 A CN109321266 A CN 109321266A
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CN
China
Prior art keywords
wood vinegar
liquid
ether
wood
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811289293.4A
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Chinese (zh)
Inventor
王刚
王蕊
吴凤慧
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tangshan Tong Hyuk Biomass Energy Development Co Ltd
Original Assignee
Tangshan Tong Hyuk Biomass Energy Development Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tangshan Tong Hyuk Biomass Energy Development Co Ltd filed Critical Tangshan Tong Hyuk Biomass Energy Development Co Ltd
Priority to CN201811289293.4A priority Critical patent/CN109321266A/en
Publication of CN109321266A publication Critical patent/CN109321266A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10CWORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
    • C10C5/00Production of pyroligneous acid distillation of wood, dry distillation of organic waste
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00Technologies for the production of fuel of non-fossil origin
    • Y02E50/10Biofuels, e.g. bio-diesel

Abstract

The present invention relates to a kind of wood vinegar, especially a kind of preparation method of wood vinegar.Carry out in accordance with the following steps: timber carries out the smoke evacuation generated when charing production by retort or gas retort, and the liquid directly collected after cooling, cohesion obtains crude pyroligneous acid;Crude pyroligneous acid standing 6 months or more, its precipitating is allowed to be divided into three layers, top layer is light oil, and lowest level is that soluble wood tar takes the liquid of middle layer, obtain aging wood vinegar after removing upper layer light oil;Aging wood vinegar is first given into filtering, the active carbon of 3~4% charcoal powder or 2% that account for wood vinegar quality is subsequently poured into, is sufficiently mixed, after placing one day, then filtering is given, becomes acetum pyrolignosum rectificatum liquid;Acetum pyrolignosum rectificatum liquid is taken, is extracted every time with ether, is extracted 6 times, diethyl ether solution is merged, vacuum recycles ether, obtains wood vinegar concentrate.Compared with prior art, the present invention indices are better than similar product.

Description

The preparation method of wood vinegar
Technical field
The present invention relates to a kind of wood vinegar, especially a kind of preparation method of wood vinegar.
Background technique
The yellowish-brown that wood vinegar is emerged when being by the burning of plant raw material of wood-charcoal is simultaneously formed after the cigarette recycling cooling with irritating pungent Liquid.The property of wood vinegar is different and different with the type of raw material of wood-charcoal, the water content of raw material of wood-charcoal and its preparation method.Even identical charcoal The wood vinegar of material, constituent species, content also can different from, with collection technology, the resting period, refining methd difference and It is different.In recent years, occurs the wood vinegar of a variety of different raws material of wood-charcoal in the world, since wood vinegar is with the difference of raw material of wood-charcoal, physics and chemistry Matter is also different, therefore, the preparation method for thering is the bigger market demand to remove to research and develop a kind of new wood vinegar in wood vinegar.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of wood vinegar, the product obtained with the method, indices Better than similar product.
The present invention adopts the following technical scheme:
A kind of preparation method of wood vinegar carries out in accordance with the following steps:
1) timber carries out the smoke evacuation generated when charing production by retort or gas retort, directly receives after cooling, cohesion The liquid of collection, obtains crude pyroligneous acid;
2) crude pyroligneous acid standing 6 months or more, its precipitating is allowed to be divided into three layers, top layer is light oil, and lowest level is solvable Property wood tar, remove upper layer light oil after, take the liquid of middle layer, obtain aging wood vinegar;
3) aging wood vinegar is first given into filtering, is subsequently poured into the work of 3~4% charcoal powder or 2% that account for wood vinegar quality Property charcoal, be sufficiently mixed, after placing one day, then give filtering, become acetum pyrolignosum rectificatum liquid;
4) acetum pyrolignosum rectificatum liquid is taken, is extracted every time with ether, is extracted 6 times, diethyl ether solution is merged, vacuum recycles ether, Obtain wood vinegar concentrate.
By adopting the above technical scheme compared with prior art, the present invention indices be better than similar product.
The present invention adopts the following technical scheme:
In step 4), the proportion of wood vinegar and ether is 100~120g:30~40ml.
In step 4), the proportion of wood vinegar and ether is 100g:30~40ml.
Pour into 4% charcoal powder for accounting for wood vinegar quality.
Specific implementation formula mode
The present invention is described in detail below with reference to embodiment:
Embodiment 1:
A kind of preparation method of wood vinegar carries out in accordance with the following steps:
1, apple tree is selected as timber and carries out the smoke evacuation generated when charing production by retort or gas retort, through cold But, that directly collects after agglomerating arrives with sour liquid as main component, obtains crude pyroligneous acid.
2, crude pyroligneous acid standing 6 months or more, its precipitating is allowed to be divided into three layers, top layer is light oil, and lowest level is solvable Property wood tar, remove upper layer light oil after, take the liquid of middle layer, obtain aging wood vinegar.
3, aging wood vinegar is first given into filtering, is subsequently poured into 4% charcoal powder for accounting for wood vinegar quality, the two is sufficiently mixed It closes, after placing one day, then gives filtering, become acetum pyrolignosum rectificatum liquid.
4, acetum pyrolignosum rectificatum liquid 100g is taken, is extracted every time with 30ml ether, is extracted 6 times, diethyl ether solution is merged, vacuum is returned Ether is received, wood vinegar concentrate is obtained;Wood vinegar and other substances are matched according to actual needs, can produce cosmetics, The products such as the antibacterial disinfectant of deodorization, all indicators are better than similar products.
The physical and chemical index of product should meet the requirement of table 1.
1 physical and chemical index of table
Test method:
Unless otherwise indicated, this experiment reagent used is that analysis is pure, and water should meet wanting for the tertiary effluent in GB/T 6682 It asks.
1, sense organ
The sample for being no less than 20mL is measured, is placed in the flint glass test tube of dried and clean, is carried out in non-direct projection striation part Observation.
2, specific gravity
It is measured under 15 DEG C~25 DEG C of liquid temperature using densimeter.
3, pH value
It is measured using acidometer (pH meter) or pH value test paper.
4, acidity
It is measured using acid-base titration, assumes that the acidity of wood vinegar is provided by acetic acid when calculating.100 are diluted in 1mL Times wood vinegar in few drops of phenolphthalein indicators are added dropwise, be slowly added into 2% or 0.1 specification (i.e. 0.1mol/L) sodium hydroxide it is molten Liquid acquires the point of neutralization.
5, water phase
The ecological wood vinegar percentage of moisture is measured according to GB/T 6283.
6, organic phase, resin coke oil content
7, sample preparation (dehydration concentration method sample preparation)
Acetum pyrolignosum rectificatum liquid 100g is taken, is extracted every time with 30mL ether, is extracted 6 times, diethyl ether solution, vacuum recycling are merged Ether obtains wood vinegar concentrate, is used as GC-MS (gas chromatograph-mass spectrometer, gas chromatography-mass spectrum) sample to be tested.
8, GC-MS method measures ecological wood vinegar chemical component and content
Ecological wood vinegar concentrate ingredient is analyzed with GC-MS method with direct-injection technique.GC conditions: DB- WAX capillary column (30m × 0.25mm × 0.25 μm), 220 DEG C of injector temperature, 60 DEG C of column temperature, after constant temperature 2min, with 6.0 DEG C/ Min speed is warming up to 240 DEG C, constant temperature 8min.Split sampling 80:1.Flow rate of carrier gas 1.0mL/min.Mass Spectrometry Conditions: the source EI, electronics Energy 70eV, 250 DEG C of ion source temperature, mass scan range 35amu~400amu, mass spectrum java standard library: the library NIST.
Inspection rule:
It is executed by the regulation of QB/T 2951.
1, exfactory inspection
Exfactory inspection project is sense organ, specific gravity, pH value, acidity.
2, formal testing
Formal testing is one-hundred-percent inspection project as defined in this standard.During normal production, it carries out every half a year once, there is following feelings Condition for the moment, should also carry out formal testing:
When product approval is gone into operation;
Production technology has larger change, when may influence product quality;
When exfactory inspection result and last time formal testing result have larger difference;
When halt production more than half a year is resumed production;
When national quality superintendent office claims.
Mark, packaging, transport and storage:
1, indicate
Should there are name of product, specifications and models, the product standard of execution number, important technological parameters (skill in 1.1 product packagings Art requirement), date of manufacture, manufacturing enterprise's title, address and phone, points for attention.
Printed words or mark in 1.2 product transportation packages should ensure that more not long and smudgy because lasting, transportation and packing On storage and transportation diagram mark should meet the requirement of GB/T 191.
2, it packs
Packing case, padded coaming answer the material of selector cyclization guaranteed request.User's manual should meet the rule of GB 5296.1 It is fixed.
3, it transports
Answered when Product transport it is with light packs, gently unload, should not be inverted, avoid being exposed to the sun, drench with rain, avoid high temperature or frost, forbid in case On trample and stack weight.
4, it stores
Product should should not be stored in the ring of high temperature or frost in ventilation, drying and not by direct sunlight and the place to drench with rain In border.Stacking should take necessary safeguard procedures, and stacking height should be appropriate, avoid damaging big packaging.
5, the shelf-life
The shelf-life of product product in the case where meeting situation as defined in this standard is 2 years.

Claims (4)

1. a kind of preparation method of wood vinegar carries out in accordance with the following steps:
1) timber carries out the smoke evacuation generated when charing production by retort or gas retort, directly collects after cooling, cohesion Liquid obtains crude pyroligneous acid;
2) crude pyroligneous acid standing 6 months or more, its precipitating is allowed to be divided into three layers, top layer is light oil, and lowest level is soluble wood Tar takes the liquid of middle layer, obtains aging wood vinegar after removing upper layer light oil;
3) aging wood vinegar is first given into filtering, is subsequently poured into the active carbon of 3~4% charcoal powder or 2% that account for wood vinegar quality, It is sufficiently mixed, after placing one day, then gives filtering, become acetum pyrolignosum rectificatum liquid;
4) acetum pyrolignosum rectificatum liquid is taken, is extracted every time with ether, is extracted 6 times, diethyl ether solution is merged, vacuum recycles ether, obtains Wood vinegar concentrate.
2. the preparation method of wood vinegar according to claim 1, it is characterised in that: in step 4), wood vinegar and ether Proportion is 100~120g:30~40ml.
3. the preparation method of wood vinegar according to claim 1, it is characterised in that: in step 4), wood vinegar and ether Proportion is 100g:30ml.
4. the preparation method of wood vinegar according to claim 1, it is characterised in that: pour into and account for the 4% of wood vinegar quality Charcoal powder.
CN201811289293.4A 2018-10-31 2018-10-31 The preparation method of wood vinegar Pending CN109321266A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811289293.4A CN109321266A (en) 2018-10-31 2018-10-31 The preparation method of wood vinegar

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811289293.4A CN109321266A (en) 2018-10-31 2018-10-31 The preparation method of wood vinegar

Publications (1)

Publication Number Publication Date
CN109321266A true CN109321266A (en) 2019-02-12

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111675362A (en) * 2020-06-19 2020-09-18 合肥森愚仁新材料科技有限公司 Harmless treatment method of moso bamboo wet carbonization wastewater, crop growth regulator and use method thereof
CN112136978A (en) * 2020-09-09 2020-12-29 华南农业大学 Application of wood vinegar in alfalfa ensiling

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120167452A1 (en) * 2010-12-30 2012-07-05 Conocophillips Company Absorption and quench method for biomass pyrolysis product
CN105394156A (en) * 2015-12-03 2016-03-16 高大元 Method for preparing antibacterial pest-proof liquid meat-smoking agent
CN107223952A (en) * 2017-08-09 2017-10-03 安徽省启示录餐饮管理有限公司 A kind of high anti-corrosion smoke tartar sauce and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120167452A1 (en) * 2010-12-30 2012-07-05 Conocophillips Company Absorption and quench method for biomass pyrolysis product
CN105394156A (en) * 2015-12-03 2016-03-16 高大元 Method for preparing antibacterial pest-proof liquid meat-smoking agent
CN107223952A (en) * 2017-08-09 2017-10-03 安徽省启示录餐饮管理有限公司 A kind of high anti-corrosion smoke tartar sauce and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
尉芹等: "杨树木醋液的化学成分分析及抑菌试验", 《林业科学》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111675362A (en) * 2020-06-19 2020-09-18 合肥森愚仁新材料科技有限公司 Harmless treatment method of moso bamboo wet carbonization wastewater, crop growth regulator and use method thereof
CN112136978A (en) * 2020-09-09 2020-12-29 华南农业大学 Application of wood vinegar in alfalfa ensiling

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Application publication date: 20190212