CN104327874B - The method preparing pyroligneous liquor - Google Patents

The method preparing pyroligneous liquor Download PDF

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Publication number
CN104327874B
CN104327874B CN201410617932.0A CN201410617932A CN104327874B CN 104327874 B CN104327874 B CN 104327874B CN 201410617932 A CN201410617932 A CN 201410617932A CN 104327874 B CN104327874 B CN 104327874B
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pyroligneous liquor
walnut shell
removal
temperature
pyroligneous
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CN104327874A (en
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华文蔚
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JIANGSU DONGBAO AGROCHEMICAL Co.,Ltd.
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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)
  • Fertilizers (AREA)

Abstract

The invention discloses a kind of method preparing pyroligneous liquor, comprise the steps: 1) removal of impurities: by the Impurity removal in walnut shell;2) hot destructive distillation: the walnut shell after removal of impurities is joined together with charcoal in pyrolysis still, walnut shell and charcoal ratio are 5 8:2 3 be pyrolyzed under temperature is 450 550 DEG C of isolation air 5 10 little time, be then pyrolyzed 24 hours under temperature is 350 380 DEG C of isolation air;3) condensation: condenser condensation is obtained thick pyroligneous liquor by the gas drawn from pyrolysis still;4) stand: by crude pyroligneous acid stratification placed in the vessel together with ethanol;5) distillation: taking the intermediate layer that obtains of layering and carry out rectifying, rectifying condition is: temperature 120 140 DEG C, and condensation obtains refined pyroligneous liquor.The method uses walnut shell to make pyroligneous liquor be easy to layering as raw material, and quality is fine, is particularly well-suited to fertilizer, and the method for employing addition charcoal and two sections of pyrolysis is conducive to the raising of the yield of pyroligneous liquor, adds ethanol solution and is especially beneficial pyroligneous liquor layering.

Description

The method preparing pyroligneous liquor
Technical field
The present invention relates to one and prepare pyroligneous liquor method.
Background technology
Pyroligneous liquor is the product liquid that the condensed cooling of gas phase flue gas during wood materials destructive distillation obtains.It is one Plant pure natural, broad spectrum activity, activated state, planted, by more than 200, the composite biological agent that compositions form, have uniqueness Sootiness fragrance.And owing to pyroligneous liquor is from natural, so the product being made up of it and preparation all can be at natures Decomposing under state, in soil, residual is not it is considered to be green product, more and more each by the world The attention of state.Jealous woman liquid composition obtained by different raw material has certain difference.It is widely used in life Thing agricultural chemicals, biological organic fertilizer, medicine and other fields.Current domestic existing product is with the once sintered one-tenth of timber Raw carbon, then extract wood tar by Electronic Control retort, then separated or water purification filter through smog by wood tar Preparing, its yield is 8-12%, and active constituent content is 22-25%.It is timber owing to preparing raw material, and Yield, active constituent content are the lowest, and application effect is undesirable, and cost is the highest, it is often more important that cause gloomy The consumption of woods resource, is unfavorable for environmental protection.Along with the increasing both production and income of China's agricultural, crops cot, straw Bar aboundresources is easy to get, and its exploitation is delayed, and major part goes out of use, if being used for producing pyroligneous liquor, and can Turn waste into wealth, cleaning ambient, save again the forest reserves, protect environment.
CN200410047562 discloses process for producing pyroligneous liquor and includes raw process and process for refining two step. (1) raw process of pyroligneous liquor, raw material: broad leaf tree such as toothed oak, birch, look, Chinese scholartree etc., coniferous tree such as China fir, cypress, The rossed wood of pine etc., logging residue tree head, tree root, industrial wood waste butt, slab, saw foam.Work Skill: light a fire according to existing charcoal processing technique loading of kiln, using the acidproof porcelain tube of long 1 meter, diameter 20 centimetres as Chimney.The horn mouth of acidproof porcelain tube is down.When raw material carbonize chimney emerge tobacco, cigarette temperature reach 80 DEG C time, The acidproof porcelain tube that 2-5 saves same specification is docked with chimney.2-5 saves acidproof porcelain tube horn mouth upward, depends on Secondary connection.1st, 2 save acidproof porcelain tube junction iron sheet suitable for reading covers, and does not allow cigarette emerge from junction, End opening pad one veneer, forms a gap.Cigarette cools down in above four joint porcelain tubes, and pyroligneous liquor is from the 1st, 2 The gap saving acidproof porcelain tube junction flows out, and typically has wheat straw pipe thick, uses container reception.When receiving pyroligneous liquor, Require that Section 1 chimney cigarette temperature reaches 80-150 DEG C.When cigarette temperature does not reaches 80 DEG C pyroligneous liquor yield poorly and concentration is low, Color is light, and active ingredient is few;When cigarette temperature is more than 150 DEG C, dropping down water and do not become line, pH value reaches 3.5, wood tar Content is high.Condenser porcelain tube is suitable for reading can not be covered with any article or blocking, otherwise can affect the quality of product, Even wholly without using effect.(2) process for refining of pyroligneous liquor, staticly settles 3 by rough pyroligneous liquor More than Yue, remove suspension and the unstability pyroligneous liquor on top layer, account for 10-15%, go the most again to break off the base The sediment in portion and harmful pyroligneous liquor, account for 20-30%, takes middle level pyroligneous liquor and enters as steps described below Row is refined: 1, filtered through gauze;2, film filter filters;3, filtered through gauze;4, inspection, perfusion.Its In, described filtration gauze is medical absorbent cotton;Equipment in whole production technology and packing container requirement Acidproof, porcelain, stainless steel or plastics can be used.
CN03110910 discloses the preparation method of this pyroligneous liquor, and concrete technology step is as follows: (1), select materials: The straw of crops cot or pulverizing through screening and removing impurities, remove old standby;(2), light: first use a small amount of skin The straw of shell or pulverizing is lighted in middle temperature permanent control water cyclic carbon freezing of a furnace;(3), sintering: cot to be lighted or When the straw pulverized plays naked light, start to put into continuously cot or the straw of pulverizing, till not playing naked light, Control furnace temperature 180-260 DEG C to be sintered;(4), collect: the smog that cot sintering produces water circulation in stove System dissolves sedimentation naturally, oozes liquid pyroligneous liquor from gas extraction system after sedimentation, sinters 2-4 hour, wood jealous woman Liquid yield is up to more than 15-23%.Crops cot during process above is mainly: beans shell, rice husk, Husk, sorghum husk, straw is mainly beanstalk, sorghum stalks, corn stalk, wheat straw, and its raw material preferably are selected from agriculture Crop cot, middle temperature permanent control water cyclic carbon freezing of a furnace is to have water circle device, filling with temperature control of mist of not discharging fume The conventional oven put.
Summary of the invention
It is an object of the invention to the method that pyroligneous liquor is prepared in proposition.
For reaching this purpose, the present invention by the following technical solutions:
A kind of method preparing pyroligneous liquor, including:
1) removal of impurities: by the Impurity removal in walnut shell;
2) hot destructive distillation: the walnut shell after removal of impurities is joined together with charcoal in pyrolysis still, walnut shell and charcoal ratio It is pyrolyzed 5-10 hour under temperature is 450-550 DEG C of isolation air for 5-8:2-3, then in temperature is It is pyrolyzed 2-4 hour under 350-380 DEG C of isolation air;
3) condensation: condenser condensation is obtained thick pyroligneous liquor by the gas drawn from pyrolysis still;
4) stand: by crude pyroligneous acid stratification placed in the vessel together with ethanol;
5) distillation: taking the intermediate layer that obtains of layering and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, cold Solidifying obtaining refines pyroligneous liquor.
The method uses walnut shell to make pyroligneous liquor be easy to layering as raw material, and quality is fine, particularly suitable In fertilizer, the method for employing addition charcoal and two sections of pyrolysis is conducive to the raising of the yield of pyroligneous liquor, adds second Alcoholic solution is especially beneficial pyroligneous liquor layering.
Detailed description of the invention
Embodiment 1
1) removal of impurities: by the Impurity removal in walnut shell;
2) hot destructive distillation: being joined together with charcoal by the walnut shell after removal of impurities in pyrolysis still, walnut shell with charcoal ratio is 5-8:2-3 is pyrolyzed 5-10 hour under temperature is 450 DEG C of isolation air, is then 350 DEG C in temperature and completely cuts off sky It is pyrolyzed 2-4 hour under gas;
3) condensation: condenser condensation is obtained thick pyroligneous liquor by the gas drawn from pyrolysis still;
4) stand: by crude pyroligneous acid stratification placed in the vessel together with ethanol;
5) distillation: taking the intermediate layer that obtains of layering and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, cold Solidifying obtaining refines pyroligneous liquor.
Embodiment 2
1) removal of impurities: by the Impurity removal in walnut shell;
2) hot destructive distillation: being joined together with charcoal by the walnut shell after removal of impurities in pyrolysis still, walnut shell with charcoal ratio is 5-8:2-3 is pyrolyzed 5-10 hour under temperature is 480 DEG C of isolation air, is then 350 DEG C in temperature and completely cuts off sky It is pyrolyzed 2-4 hour under gas;
3) condensation: condenser condensation is obtained thick pyroligneous liquor by the gas drawn from pyrolysis still;
4) stand: by crude pyroligneous acid stratification placed in the vessel together with ethanol;
5) distillation: taking the intermediate layer that obtains of layering and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, cold Solidifying obtaining refines pyroligneous liquor.
Embodiment 3
1) removal of impurities: by the Impurity removal in walnut shell;
2) hot destructive distillation: being joined together with charcoal by the walnut shell after removal of impurities in pyrolysis still, walnut shell with charcoal ratio is 5-8:2-3 is pyrolyzed 5-10 hour under temperature is 490 DEG C of isolation air, is then 360 DEG C in temperature and completely cuts off sky It is pyrolyzed 2-4 hour under gas;
3) condensation: condenser condensation is obtained thick pyroligneous liquor by the gas drawn from pyrolysis still;
4) stand: by crude pyroligneous acid stratification placed in the vessel together with ethanol;
5) distillation: taking the intermediate layer that obtains of layering and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, cold Solidifying obtaining refines pyroligneous liquor.
Embodiment 4
1) removal of impurities: by the Impurity removal in walnut shell;
2) hot destructive distillation: being joined together with charcoal by the walnut shell after removal of impurities in pyrolysis still, walnut shell with charcoal ratio is 5-8:2-3 is pyrolyzed 5-10 hour under temperature is 500 DEG C of isolation air, is then 360 DEG C in temperature and completely cuts off sky It is pyrolyzed 2-4 hour under gas;
3) condensation: condenser condensation is obtained thick pyroligneous liquor by the gas drawn from pyrolysis still;
4) stand: by crude pyroligneous acid stratification placed in the vessel together with ethanol;
5) distillation: taking the intermediate layer that obtains of layering and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, cold Solidifying obtaining refines pyroligneous liquor.
Embodiment 5
1) removal of impurities: by the Impurity removal in walnut shell;
2) hot destructive distillation: being joined together with charcoal by the walnut shell after removal of impurities in pyrolysis still, walnut shell with charcoal ratio is 5-8:2-3 is pyrolyzed 5-10 hour under temperature is 520 DEG C of isolation air, is then 370 DEG C in temperature and completely cuts off sky It is pyrolyzed 2-4 hour under gas;
3) condensation: condenser condensation is obtained thick pyroligneous liquor by the gas drawn from pyrolysis still;
4) stand: by crude pyroligneous acid stratification placed in the vessel together with ethanol;
5) distillation: taking the intermediate layer that obtains of layering and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, cold Solidifying obtaining refines pyroligneous liquor.
Embodiment 6
1) removal of impurities: by the Impurity removal in walnut shell;
2) hot destructive distillation: being joined together with charcoal by the walnut shell after removal of impurities in pyrolysis still, walnut shell with charcoal ratio is 5-8:2-3 is pyrolyzed 5-10 hour under temperature is 530 DEG C of isolation air, is then 370 DEG C in temperature and completely cuts off sky It is pyrolyzed 2-4 hour under gas;
3) condensation: condenser condensation is obtained thick pyroligneous liquor by the gas drawn from pyrolysis still;
4) stand: by crude pyroligneous acid stratification placed in the vessel together with ethanol;
5) distillation: taking the intermediate layer that obtains of layering and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, cold Solidifying obtaining refines pyroligneous liquor.
Embodiment 7
1) removal of impurities: by the Impurity removal in walnut shell;
2) hot destructive distillation: being joined together with charcoal by the walnut shell after removal of impurities in pyrolysis still, walnut shell with charcoal ratio is 5-8:2-3 is pyrolyzed 5-10 hour under temperature is 550 DEG C of isolation air, is then 350 DEG C in temperature and completely cuts off sky It is pyrolyzed 2-4 hour under gas;
3) condensation: condenser condensation is obtained thick pyroligneous liquor by the gas drawn from pyrolysis still;
4) stand: by crude pyroligneous acid stratification placed in the vessel together with ethanol;
5) distillation: taking the intermediate layer that obtains of layering and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, cold Solidifying obtaining refines pyroligneous liquor.
Embodiment 8
1) removal of impurities: by the Impurity removal in walnut shell;
2) hot destructive distillation: being joined together with charcoal by the walnut shell after removal of impurities in pyrolysis still, walnut shell with charcoal ratio is 5-8:2-3 is pyrolyzed 5-10 hour under temperature is 530 DEG C of isolation air, is then 350 DEG C in temperature and completely cuts off sky It is pyrolyzed 2-4 hour under gas;
3) condensation: condenser condensation is obtained thick pyroligneous liquor by the gas drawn from pyrolysis still;
4) stand: by crude pyroligneous acid stratification placed in the vessel together with ethanol;
5) distillation: taking the intermediate layer that obtains of layering and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, cold Solidifying obtaining refines pyroligneous liquor.
Embodiment 9
1) removal of impurities: by the Impurity removal in walnut shell;
2) hot destructive distillation: being joined together with charcoal by the walnut shell after removal of impurities in pyrolysis still, walnut shell with charcoal ratio is 5-8:2-3 is pyrolyzed 5-10 hour under temperature is 520 DEG C of isolation air, is then 350 DEG C in temperature and completely cuts off sky It is pyrolyzed 2-4 hour under gas;
3) condensation: condenser condensation is obtained thick pyroligneous liquor by the gas drawn from pyrolysis still;
4) stand: by crude pyroligneous acid stratification placed in the vessel together with ethanol;
5) distillation: taking the intermediate layer that obtains of layering and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, cold Solidifying obtaining refines pyroligneous liquor.

Claims (1)

1. the method preparing pyroligneous liquor, it is characterised in that comprise the steps:
1) removal of impurities: by the Impurity removal in walnut shell;
2) hot destructive distillation: being joined together with charcoal by the walnut shell after removal of impurities in pyrolysis still, walnut shell with charcoal ratio is 5-8:2-3 is pyrolyzed 5-10 hour under temperature is 450-550 DEG C of isolation air, is then 350-380 DEG C in temperature It is pyrolyzed 2-4 hour under isolation air;
3) condensation: condenser condensation is obtained thick pyroligneous liquor by the gas drawn from pyrolysis still;
4) stand: by crude pyroligneous acid stratification placed in the vessel together with ethanol;
5) distillation: taking the intermediate layer that obtains of layering and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, condenses To refined pyroligneous liquor.
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Publication number Priority date Publication date Assignee Title
CN105132001B (en) * 2015-09-11 2017-09-15 绍兴纺织机械集团有限公司 It is a kind of to prepare the method that wood tar is reduced during pyrolkigneous liquid
CN106811225A (en) * 2015-11-30 2017-06-09 鹿岩 The refining separation device of pyrolkigneous liquid
CN105586064A (en) * 2016-01-13 2016-05-18 河北天善生物技术有限公司 Method for preparing refined wood vinegar from crop straw
CN106800943A (en) * 2016-12-13 2017-06-06 中山市世和生物科技有限公司 Preparation method of wood vinegar, feed additive and application thereof
CN106854113A (en) * 2017-01-19 2017-06-16 重庆市中绿农业开发有限责任公司 A kind of walnut organic-inorganic compound fertilizer special
CN112484037A (en) * 2020-11-03 2021-03-12 李洪 Deodorant for compatibility of RDF and application thereof
CN113429228A (en) * 2021-07-23 2021-09-24 菏泽学院 System for preparing pyroligneous through fermentation of ginkgo tree branches

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CN101074382A (en) * 2007-06-25 2007-11-21 辽宁大学 Process for extracting wood-vinegar fluid from almond
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CN101613612A (en) * 2009-07-17 2009-12-30 北京林业大学 Utilize sea-buckthorn limb to prepare the method for charcoal and wood vinegar and the charcoal and the wood vinegar of preparation
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CN101074382A (en) * 2007-06-25 2007-11-21 辽宁大学 Process for extracting wood-vinegar fluid from almond
CN101126028A (en) * 2007-08-03 2008-02-20 浙江省林业科学研究院 Method for preparing bamboo vinegar liquid extract for eliminating fowl influenza virus in environment
CN101613612A (en) * 2009-07-17 2009-12-30 北京林业大学 Utilize sea-buckthorn limb to prepare the method for charcoal and wood vinegar and the charcoal and the wood vinegar of preparation
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