CN110437864A - A kind of wood vinegar efficiently separates technique - Google Patents

A kind of wood vinegar efficiently separates technique Download PDF

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Publication number
CN110437864A
CN110437864A CN201910638200.2A CN201910638200A CN110437864A CN 110437864 A CN110437864 A CN 110437864A CN 201910638200 A CN201910638200 A CN 201910638200A CN 110437864 A CN110437864 A CN 110437864A
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CN
China
Prior art keywords
wood vinegar
tower
topping still
acetic acid
component
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CN201910638200.2A
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Chinese (zh)
Inventor
王美聪
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Shenyang University of Chemical Technology
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Shenyang University of Chemical Technology
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Priority to CN201910638200.2A priority Critical patent/CN110437864A/en
Publication of CN110437864A publication Critical patent/CN110437864A/en
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    • 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

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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)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

A kind of wood vinegar efficiently separates technique, is related to a kind of wood vinegar separating technology, and wood vinegar topping still tower top obtains light component by level-one condensation and B-grade condensation, and level-one condensation lower part is equipped with return pipe and heavy constituent is back to topping still;The multicomponent distillate come out in the middle part of wood vinegar topping still tower enters acetic acid lightness-removing column, distillates light component from tower top, the heavy constituent of tower bottom enters acetic acid weight-removing column and further separates each component;The present invention has the rough segmentation rectifying column of a plurality of side take-off mouth using one, and the cutting of wood vinegar stoste is separated into several strands of liquid with entirely different feature with minimum Neng Mao.The regeneration of solvent is realized using solvent regeneration tower and obtains the higher target product of purity, and the present invention can obtain that type is abundant and the higher wood vinegar distillate of quality.

Description

A kind of wood vinegar efficiently separates technique
Technical field
The present invention relates to a kind of wood vinegar separating technologies, efficiently separate technique more particularly to a kind of wood vinegar.
Background technique
By agricultural crop straw, the charing such as fruit stone shell and some branches is to have national grand strategy meaning to produce organic fertilizer The work of justice.But this work is also difficult to smoothly carry out at present, most important reason is exactly in this course must be right Carbonization process sprays a large amount of water, therefore produces a large amount of wood vinegar.And there is presently no practicable means to be subject to benefit With with processing wood vinegar to realize its high efficient resourcing.
Wood vinegar contains the extremely wide organic matter of molecular weight distribution, the carbon atom numbers of these organic matters can be from one to tens not Deng.This, which results in the physical property of these organic matters and chemical property, can be distributed in a very wide range.Meanwhile except minority Organic concentration is slightly higher, and if methanol is up to 2% to 5%, for acetic acid up to 10% to 15%, other most of organic concentrations are all very low, Often less than 1%.Total content of organics can change in a very big range in wood vinegar, such as from 15% to 30% or so, Other are all water.So low concentration containing very eurytopic organic aqueous solution to the technical side of conventional low cost It is very difficult that method, which is separated,.
Wood vinegar has been developed many purposes, is such as used as the insecticide of crops, herbicide, for home poultry raising industry to kill Bacterium, deodorization, etc..However the organic concentration as contained by wood vinegar is too low, and water content is too high, and cause its economic value lower, It promotes and applies difficult.If the place using the place distance production of wood vinegar is slightly remote, the freight charges of that wood vinegar be can easily exceed The value of wood vinegar itself.
Containing there are many extremely valuable organic matter in wood vinegar, these organic matters are often difficult to obtain by normal chemical process .And when these extremely valuable organic matters are present in wood vinegar with very low concentration, but also they at all can not be by It utilizes.
In conclusion to by agricultural crop straw, fruit stone shell and some branches etc. are carbonized to produce organic fertilizer with regard to necessary in large quantities The a large amount of wood vinegar that effectively handle and be generated in the process using this, and to effectively handling and utilizing this process The a large amount of wood vinegar generated, wood vinegar must be just concentrated with very economical means, and extracts and desirable have Machine compound component.And obtained a large amount of water must be able to be effectively purified in the concentration process of wood vinegar, so that it can To be recycled.
Up to the present, many technologies are developed to handle wood vinegar.But most of simply steamed to wood vinegar It evaporates or rectifying, to remove the dirty materials such as the wood glue oil in wood vinegar, to achieve the purpose that purify a kind of wood vinegar (wood vinegar purification Equipment, 104650939 A of application publication number CN;A kind of wood vinegar distilling apparatus, application number 201910128153.7;The wooden vinegar The refining separation device of liquid, 106811225 A of application publication number CN;Wood vinegar distilling apparatus and distillating method, application publication number 106823436 A of CN).It is only a small number of to pre-process wood vinegar for other purposes, if any a kind of patent (high efficiency extraction wood vinegar The method of middle phenols extract, application number: application number 201710543474.4) want to extract from wood vinegar by extracting process Organic phenol.Also patent (a kind of wood vinegar preparing the application in fuel oil, 101962562 B of Authorization Notice No. CN) is intended to Bio-fuel is produced using wood vinegar.Patent (a kind of enzymatic hydrolysis-distillation-absorption joint progress wood vinegar purification, application publication number 105441101 A of CN) then wood vinegar is refined using enzymatic hydrolysis-distillation-absorption integrated processes, to obtain some special liquid Body is to special occasions.These processes are all based on the wooden vinegar very low by simple distillation or the purified organic concentration of rectifying Liquid, efficiency are very low, it is difficult to promote and apply.
Summary of the invention
The purpose of the present invention is to provide a kind of wood vinegar to efficiently separate technique, and the present invention has a plurality of side line using one The rough segmentation rectifying column of mouth is produced, the cutting of wood vinegar stoste is separated into minimum Neng Mao by several strands of liquid with entirely different feature Body.The light component that thick fractionator overhead comes out is collected by level-one condensation and B-grade condensation, in the heavy component logistics of tower bottom Into extraction tower to separate the active principle inside wood vinegar, the regeneration of solvent is realized using solvent regeneration tower and obtains purity Higher target product, the present invention can obtain that type is abundant and the higher wood vinegar distillate of quality.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of wood vinegar efficiently separates technique, and the device of the technique includes that wood vinegar topping still, acetic acid lightness-removing column, acetic acid are de- Weight tower, extraction tower, solvent regeneration tower and topping still condensing unit;
Including following technical process:
Wood vinegar topping still tower top obtains light component by level-one condensation and B-grade condensation, and level-one condenses lower part will equipped with return pipe Heavy constituent is back to topping still;The multicomponent distillate come out in the middle part of wood vinegar topping still tower enters acetic acid lightness-removing column, from tower top Light component is distillated, the heavy constituent of tower bottom enters acetic acid weight-removing column and further separates each component;The top of acetic acid weight-removing column go out be Smart acetic acid, what lower part went out is heavy constituent;Heavy component in wood vinegar topping still goes to extraction tower from tower bottom, wood vinegar topping still with Compared with low energy consumption wood vinegar stoste cutting be separated into several strands have entirely different speciality liquid, the rich solvent containing active principle from Tower top comes out;Heavy component in wood vinegar topping still is walked to tower bottom, obtains most heavy component in tower bottom, tower top obtains most light group Part, and intermediate side line, side line number are more than or equal to 1, then obtain the fraction of different boiling range;The component being ejected from extraction tower into Enter solvent regeneration tower, the separation of useful constituent and solvent is carried out, to obtain fresh solvent and target product.
A kind of wood vinegar efficiently separates technique, and the wood vinegar topping still feed inlet upper and lower side setting side line is adopted Outlet, these side take-off mouths are one or multiple.
A kind of wood vinegar efficiently separates technique, and the wood vinegar topping still operation under negative pressure, or is operated normal Under pressure and micro-positive pressure.
A kind of wood vinegar efficiently separates technique, the wood vinegar topping still operation temperature, i.e. tower top/tower bottom temperature Under the operating pressure of degree and tower, tower top/bottom product is in thermodynamic equilibrium state.
A kind of wood vinegar efficiently separates technique, the wood vinegar crude distillation column temperature 120 degree to 280 degree it Between, depending on the operating pressure of tower and bottom product composition.
The advantages and effects of the present invention are:
The present invention provides a kind of wood vinegar useful constituent of obtaining and efficiently separates technique.Most critical of the invention is exactly the first step The rough segmentation rectifying column of a plurality of side take-off mouth is had using one, and the cutting of wood vinegar stoste is separated into several strands with minimum Neng Mao Liquid with entirely different feature.The tower feed inlet is respectively provided with side take-off mouth up and down, these side take-off mouths can be one It is a, or multiple.After wood vinegar stoste is sent to this tower, heavy component is walked to tower bottom, obtains most heavy component in tower bottom, Tower top obtains most light component, and intermediate side line then obtains the fraction of different boiling range.Come out light group of thick fractionator overhead Lease making crosses level-one condensation and B-grade condensation is collected, and enters extraction tower in the heavy component logistics of tower bottom to separate inside wood vinegar Active principle, realize the regeneration of solvent using solvent regeneration tower and obtain the higher target product of purity, the present invention can be with Acquisition type is enriched and the higher wood vinegar distillate of quality.
Detailed description of the invention
Fig. 1 is overall craft route schematic diagram of the present invention.
Specific embodiment
The present invention is described in detail for illustrated embodiment with reference to the accompanying drawing.
Can on a large scale in order to reach, inexpensive processing wood vinegar, the present invention uses rectifying-suction of a set of continuous operation Attached-extraction process, including including wood vinegar topping still, acetic acid lightness-removing column, acetic acid weight-removing column, extraction tower, solvent regeneration tower five Main tower and the condensation process on topping still top.Wherein most critical is exactly that the first step uses one to have a plurality of side take-off The cutting of wood vinegar stoste is separated into several strands of liquid with entirely different feature with minimum Neng Mao by rectifying column.Herein we It is referred to as thick fractionating column.
Figure one of the present invention is process flow diagram.Wood vinegar topping still C1 feed inlet is respectively provided with side take-off mouth up and down, these Side take-off mouth can be one, or multiple.After wood vinegar stoste is sent to this tower, heavy component is walked to tower bottom, In Tower bottom obtains most heavy component, and tower top obtains most light component, and intermediate side line then obtains the fraction of different boiling range.
Now with an extraction acetic acid, and the process for removing water is illustrated.
In wood vinegar containing 10% or so acetic acid, 80% or so water, other for molecular weight distribution it is extremely wide, boiling point distribution pole Wide various organic compounds.After wood vinegar is sent into thick fractionating column C1, by the operating pressure for suitably controlling thick fractionating column And column bottom temperature, the acetic acid of most (95% or more) can be made to be steamed out from tower bottom.In the stripping section (charging of thick fractionating column Between mouth and tower bottom) one side take-off mouth of setting, so that it may one logistics based on acetic acid is obtained, then this burst of logistics is sent To the refining plant of acetic acid, such as the acetic acid lightness-removing column C2 and acetic acid weight-removing column C3 in figure one of the present invention, so that it may obtain purity very High smart acetic acid.
The boiling point of acetic acid is 117.9 degree.(referred to as stripping section) sets a side acquisition between thick fractionating column feed inlet and tower bottom Mouthful to obtain the material based on acetic acid, the remaining material of the tower bottom necessarily boiling point heavy component higher than acetic acid.And most of water and The organic matter lower than water boiling point is inevitable to more than feed inlet moving.Some organic matters, such as phenol, the very high (phenol of their boiling point It is 182 degree), but they can form the azeotropic mixture of boiling point lower (less than 100 degree) with water.These azeotropic mixtures can be also distilled to slightly It is more than the feed inlet of fractionating column.
Since the heavy component of tower bottom may even happen that decomposition in possible coking, some when the temperature is excessively high.Meanwhile it being recombinated in this stock In part logistics, the concentration of solid impurity is also relatively high.Therefore, if will to tower bottom heavy component logistics further processing separation with Extract required organic compound, it should pay the utmost attention to using liquid/liquid extraction technique, as shown in C4, C5 tower in figure one.
The major part for going to feed inlet or more is water, is partially light component and forms the organic of low-boiling azeotrope with water Object.A side line acquisition outlet is set in feed inlet to the tower top (referred to as rectifying section) of thick fractionating column to be obtained with based on water One component streams of (water content is up to 90% or more).It has been produced completely from stripping section due to measuring bigger acetic acid, this stock Water is already close to neutral (pH value is near 7), and therefore, it can be recycled system utilization completely.
Can continue to go to after mouth is adopted in the side of thick fractionating column rectifying section tower top the mainly boiling point lighter component lower than water and A part of water.This partial material is condensed into liquid phase after steaming tower top with vapour phase, and a part returns rough segmentation and evaporates tower formation reflux, Another part is then used as product to produce.Two-stage or multi-stage condensing device should be arranged in most dense lighter component logistics in order to obtain, tower top.The Logistics under first-stage condenser (A1) is naturally cold based on water.This burst of logistics a part returned rough segmentation evaporate tower formed reflux, one Part is produced as product.It and is then light in the liquid that secondary condenser (or condenser that second level is later, A2) is cooled down The very high aqueous solution of constituents ratio.
In conclusion thick fractionating column feed inlet can set multiple side take-off mouths, rectifying section side up and down (rectifying section and stripping section) Adopt mouth than water, the main fraction produced more than lighter component, stripping section side adopts mouth and mainly produces fraction more than heavy component.These are not Same fraction can be mixed in different proportions to obtain having the concentration wood vinegar of different functions, to adapt to different application field The needs of conjunction.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, Anyone skilled in the art within the technical scope of the present disclosure, according to the technique and scheme of the present invention and its Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.

Claims (5)

1. a kind of wood vinegar efficiently separates technique, which is characterized in that the device of the technique includes wood vinegar topping still, acetic acid Lightness-removing column, acetic acid weight-removing column, extraction tower, solvent regeneration tower and topping still condensing unit;
Including following technical process:
Wood vinegar topping still tower top obtains light component by level-one condensation and B-grade condensation, and level-one condenses lower part will equipped with return pipe Heavy constituent is back to topping still;The multicomponent distillate come out in the middle part of wood vinegar topping still tower enters acetic acid lightness-removing column, from tower top Light component is distillated, the heavy constituent of tower bottom enters acetic acid weight-removing column and further separates each component;The top of acetic acid weight-removing column go out be Smart acetic acid, what lower part went out is heavy constituent;Heavy component in wood vinegar topping still goes to extraction tower from tower bottom, wood vinegar topping still with Compared with low energy consumption wood vinegar stoste cutting be separated into several strands have entirely different speciality liquid, the rich solvent containing active principle from Tower top comes out;Heavy component in wood vinegar topping still is walked to tower bottom, obtains most heavy component in tower bottom, tower top obtains most light group Part, and intermediate side line, side line number are more than or equal to 1, then obtain the fraction of different boiling range;The component being ejected from extraction tower into Enter solvent regeneration tower, the separation of useful constituent and solvent is carried out, to obtain fresh solvent and target product.
2. a kind of wood vinegar according to claim 1 efficiently separates technique, which is characterized in that the wood vinegar topping still into Side take-off mouth is arranged in material mouth upper and lower side, these side take-off mouths are one or multiple.
3. a kind of wood vinegar according to claim 1 efficiently separates technique, which is characterized in that the wood vinegar topping still behaviour Make under negative pressure, or operation is under normal pressure and micro-positive pressure.
4. a kind of wood vinegar according to claim 1 efficiently separates technique, which is characterized in that the wood vinegar topping still behaviour Make temperature, i.e., under the operating pressure of tower top/column bottom temperature and tower, tower top/bottom product is in thermodynamic equilibrium state.
5. a kind of wood vinegar according to claim 4 efficiently separates technique, which is characterized in that the wood vinegar crude distillation column Temperature is between 120 degree to 280 degree, depending on the operating pressure of tower and bottom product composition.
CN201910638200.2A 2019-07-16 2019-07-16 A kind of wood vinegar efficiently separates technique Withdrawn CN110437864A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201077830Y (en) * 2007-03-23 2008-06-25 周泽宇 Biomass heat pyrolytic air dust removing-washing-selective evaporation-decoking purifying-storage facility
CN101353583A (en) * 2008-09-19 2009-01-28 肖进彬 Biomass processing method
CN103124781A (en) * 2010-08-23 2013-05-29 科伊奥股份有限公司 Production of renewable biofuels
CN104232137A (en) * 2014-09-15 2014-12-24 浙江农林大学 Complete apparatus for refining bamboo vinegar by use of multistage multiple combination distillation method
CN106811225A (en) * 2015-11-30 2017-06-09 鹿岩 The refining separation device of pyrolkigneous liquid

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201077830Y (en) * 2007-03-23 2008-06-25 周泽宇 Biomass heat pyrolytic air dust removing-washing-selective evaporation-decoking purifying-storage facility
CN101353583A (en) * 2008-09-19 2009-01-28 肖进彬 Biomass processing method
CN103124781A (en) * 2010-08-23 2013-05-29 科伊奥股份有限公司 Production of renewable biofuels
CN104232137A (en) * 2014-09-15 2014-12-24 浙江农林大学 Complete apparatus for refining bamboo vinegar by use of multistage multiple combination distillation method
CN106811225A (en) * 2015-11-30 2017-06-09 鹿岩 The refining separation device of pyrolkigneous liquid

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
丁忠浩: "《废水资源化综合利用技术》", 31 January 2007, 国防工业出版社 *
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Application publication date: 20191112