CN104327874A - Method for preparing pyroligneous liquid - Google Patents
Method for preparing pyroligneous liquid Download PDFInfo
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- CN104327874A CN104327874A CN201410617932.0A CN201410617932A CN104327874A CN 104327874 A CN104327874 A CN 104327874A CN 201410617932 A CN201410617932 A CN 201410617932A CN 104327874 A CN104327874 A CN 104327874A
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- pyrolysis
- temperature
- pyroligneous
- impurities
- shell
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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)
- Fertilizers (AREA)
Abstract
The invention discloses a method for preparing pyroligneous liquid. The method comprises the following steps: (1) removing impurities: removing the impurities in walnut shells; (2) carrying out hot dry distillation: adding the walnut shells without the impurities and charcoal into a pyrolysis kettle, wherein the ratio of the walnut shells to the charcoal is (5-8) to (2-3); pyrolyzing for 5-10 hours at a temperature of 450-550 DEG C under the condition of no air; then pyrolyzing for 2-4 hours at a temperature of 350-380 DEG C under the condition of no air; (3) condensing: condensing gas led out from the pyrolysis kettle by a condenser to obtain rough pyroligneous liquid; (4) standing: putting the rough pyroligneous liquid and ethanol into a container, and standing and layering; and (5) distilling: taking a middle layer obtained by layering and rectifying, wherein the rectifying condition is that the temperature is 120-140 DEG C; and condensing to obtain the refined pyroligneous liquid. According to the method, the walnut shells are used as the raw materials so that the pyroligneous liquid is convenient to layer and the quality is very good; the pyroligneous liquid is particularly suitable for being used as a fertilizer; the method adopts the steps of adding the charcoal and carrying out two sections of pyrolysis so that the yield of the pyroligneous liquid is favorably improved; and the ethanol solution is added so that the pyroligneous liquid is especially easy to layer.
Description
Technical field
The present invention relates to one and prepare pyroligneous liquor method.
Background technology
The product liquid that gas phase flue gas when pyroligneous liquor is wood materials destructive distillation obtains through condensing cooling.It is a kind of pure natural, broad spectrum, activated state, plants by more than 200 the composite biological agent that composition forms, and has unique sootiness fragrance.And because pyroligneous liquor is from natural, so it is not the product be made up of it and preparation all can decompose in its natural state, residual in soil, be considered to green product, be more and more subject to the attention of countries in the world.The jealous woman liquid composition that different starting material obtain has certain difference.It is widely used in biological pesticide, biological organic fertilizer, medicine and other fields.Current domestic existing product is with the raw carbon of the once sintered one-tenth of timber, then extracts wood tar oil by electronically controlled charring furnace, then is obtained through smog separation or water purification filter by wood tar oil, and its yield is 8-12%, and active constituent content is 22-25%.Because raw materials is timber, and yield, active constituent content are all low, and effect is undesirable, and cost is also higher, the more important thing is the consumption causing the forest reserves, is unfavorable for environment protection.Along with the increasing both production and income of China's agricultural, farm crop cot, straw aboundresources are easy to get, and its exploitation is delayed, and major part goes out of use, if be used for producing pyroligneous liquor, can turn waste into wealth, cleaning ambient, saves the forest reserves again, protection of the environment.
CN200410047562 discloses process for producing pyroligneous liquor and comprises raw process and process for refining two step.(1) raw process of pyroligneous liquor, raw material: deciduous tree is as toothed oak, birch, look, Chinese scholartree etc., and softwood tree is as the rossed wood of China fir, cypress, pine etc., and logging residue sets head, tree root, industrial wood waste butt, slab, saw foam.Technique: according to existing charcoal processing technique loading of kiln igniting, using the acidproof porcelain tube of length 1 meter, diameter 20 centimetres as chimney.The hydraucone of acidproof porcelain tube down.When raw material carbonize chimney emerge tobacco, cigarette temperature reach 80 DEG C time, acidproof porcelain tube 2-5 being saved same specification docks with chimney.2-5 saves acidproof porcelain tube hydraucone upward, connects successively.1st, the 2 acidproof porcelain tube junction of joint iron sheets suitable for reading cover, and do not allow cigarette emerge from junction, end opening pad one veneer, form a gap.Cigarette cools in four joint porcelain tubes above, and pyroligneous liquor flows out from the gap of the 1st, the 2 acidproof porcelain tube junctions of joint, generally 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 reach 80 DEG C, pyroligneous liquor yields poorly and concentration is low, light, and effective constituent is few; When cigarette temperature is more than 150 DEG C, drop down water and do not become line, pH value reaches 3.5, and wood tar oil content is high.Condenser porcelain tube is suitable for reading can not be covered or blocking with any article, otherwise can affect the quality of product, does not have result of use even completely.(2) process for refining of pyroligneous liquor, rough pyroligneous liquor is staticly settled more than 3 months, remove suspended substance and the destabilization pyroligneous liquor on top layer, account for 10-15%, and then remove the throw out of bottom and harmful pyroligneous liquor, account for 20-30%, get middle level pyroligneous liquor and refine according to following step: 1, filtered through gauze; 2, film filter filters; 3, filtered through gauze; 4, check, perfusion.Wherein, described filtration gauze is medical absorbent cotton; Equipment in whole production technique and packaging vessel require acidproof, can adopt porcelain, stainless steel or plastics.
CN03110910 discloses the preparation method of this pyroligneous liquor, and concrete technology step is as follows: (1), select materials: the straw of farm crop cot or pulverizing through screening and removing impurities, remove old for subsequent use; (2), light: first light in middle temperature perseverance control water cycle carbon freezing of a furnace with the straw of a small amount of cot or pulverizing; (3), sintering: when the straw of the cot lighted or pulverizing plays naked light, start the straw dropping into cot or pulverizing continuously, till not playing naked light, control furnace temperature 180-260 DEG C and sinter; (4), collect: the water circulation system of smog in stove that cot sintering produces dissolves sedimentation naturally, oozes liquid pyroligneous liquor after sedimentation from exhaust system, sintering 2-4 hour, pyroligneous liquor yield can reach more than 15-23%.Farm crop cot in above technological process is mainly: beans shell, rice husk, husk, sorghum husk, straw is beanstalk, sorghum stalks, corn stalk, wheat straw mainly, its optimal seeking of raw and processed materials is from farm crop cot, middle temperature perseverance control water cycle carbon freezing of a furnace has water circle device, the conventional oven with temperature control unit of mist of not discharging fume.
Summary of the invention
The object of the invention is to the method proposing to prepare pyroligneous liquor.
For reaching this object, the present invention by the following technical solutions:
Prepare a method for pyroligneous liquor, comprising:
1) removal of impurities: by the Impurity removal in nut-shell;
2) hot destructive distillation: the nut-shell after removal of impurities is joined together with charcoal in pyrolysis still, nut-shell and charcoal ratio are 5-8:2-3 is when under 450-550 DEG C of isolated air, pyrolysis 5-10 is little in temperature, then pyrolysis 2-4 hour under temperature is 350-380 DEG C of isolated air;
3) condensation: condenser condenses is obtained thick pyroligneous liquor by the gas of drawing from pyrolysis still;
4) leave standstill: crude pyroligneous acid is put stratification in a reservoir together with ethanol;
5) distill: get the middle layer that layering obtains and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, and condensation obtains refining pyroligneous liquor.
This method adopts nut-shell to make pyroligneous liquor be convenient to layering as raw material, and quality is fine, is specially adapted to fertilizer, adopts the method adding charcoal and two sections of pyrolysis to be conducive to the raising of the output of pyroligneous liquor, adds ethanolic soln and be beneficial to pyroligneous liquor layering especially.
Embodiment
Embodiment 1
1) removal of impurities: by the Impurity removal in nut-shell;
2) hot destructive distillation: the nut-shell after removal of impurities is joined together with charcoal in pyrolysis still, nut-shell and charcoal ratio are 5-8:2-3 is when under 450 DEG C of isolated air, pyrolysis 5-10 is little in temperature, then pyrolysis 2-4 hour under temperature is 350 DEG C of isolated air;
3) condensation: condenser condenses is obtained thick pyroligneous liquor by the gas of drawing from pyrolysis still;
4) leave standstill: crude pyroligneous acid is put stratification in a reservoir together with ethanol;
5) distill: get the middle layer that layering obtains and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, and condensation obtains refining pyroligneous liquor.
Embodiment 2
1) removal of impurities: by the Impurity removal in nut-shell;
2) hot destructive distillation: the nut-shell after removal of impurities is joined together with charcoal in pyrolysis still, nut-shell and charcoal ratio are 5-8:2-3 is when under 480 DEG C of isolated air, pyrolysis 5-10 is little in temperature, then pyrolysis 2-4 hour under temperature is 350 DEG C of isolated air;
3) condensation: condenser condenses is obtained thick pyroligneous liquor by the gas of drawing from pyrolysis still;
4) leave standstill: crude pyroligneous acid is put stratification in a reservoir together with ethanol;
5) distill: get the middle layer that layering obtains and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, and condensation obtains refining pyroligneous liquor.
Embodiment 3
1) removal of impurities: by the Impurity removal in nut-shell;
2) hot destructive distillation: the nut-shell after removal of impurities is joined together with charcoal in pyrolysis still, nut-shell and charcoal ratio are 5-8:2-3 is when under 490 DEG C of isolated air, pyrolysis 5-10 is little in temperature, then pyrolysis 2-4 hour under temperature is 360 DEG C of isolated air;
3) condensation: condenser condenses is obtained thick pyroligneous liquor by the gas of drawing from pyrolysis still;
4) leave standstill: crude pyroligneous acid is put stratification in a reservoir together with ethanol;
5) distill: get the middle layer that layering obtains and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, and condensation obtains refining pyroligneous liquor.
Embodiment 4
1) removal of impurities: by the Impurity removal in nut-shell;
2) hot destructive distillation: the nut-shell after removal of impurities is joined together with charcoal in pyrolysis still, nut-shell and charcoal ratio are 5-8:2-3 is when under 500 DEG C of isolated air, pyrolysis 5-10 is little in temperature, then pyrolysis 2-4 hour under temperature is 360 DEG C of isolated air;
3) condensation: condenser condenses is obtained thick pyroligneous liquor by the gas of drawing from pyrolysis still;
4) leave standstill: crude pyroligneous acid is put stratification in a reservoir together with ethanol;
5) distill: get the middle layer that layering obtains and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, and condensation obtains refining pyroligneous liquor.
Embodiment 5
1) removal of impurities: by the Impurity removal in nut-shell;
2) hot destructive distillation: the nut-shell after removal of impurities is joined together with charcoal in pyrolysis still, nut-shell and charcoal ratio are 5-8:2-3 is when under 520 DEG C of isolated air, pyrolysis 5-10 is little in temperature, then pyrolysis 2-4 hour under temperature is 370 DEG C of isolated air;
3) condensation: condenser condenses is obtained thick pyroligneous liquor by the gas of drawing from pyrolysis still;
4) leave standstill: crude pyroligneous acid is put stratification in a reservoir together with ethanol;
5) distill: get the middle layer that layering obtains and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, and condensation obtains refining pyroligneous liquor.
Embodiment 6
1) removal of impurities: by the Impurity removal in nut-shell;
2) hot destructive distillation: the nut-shell after removal of impurities is joined together with charcoal in pyrolysis still, nut-shell and charcoal ratio are 5-8:2-3 is when under 530 DEG C of isolated air, pyrolysis 5-10 is little in temperature, then pyrolysis 2-4 hour under temperature is 370 DEG C of isolated air;
3) condensation: condenser condenses is obtained thick pyroligneous liquor by the gas of drawing from pyrolysis still;
4) leave standstill: crude pyroligneous acid is put stratification in a reservoir together with ethanol;
5) distill: get the middle layer that layering obtains and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, and condensation obtains refining pyroligneous liquor.
Embodiment 7
1) removal of impurities: by the Impurity removal in nut-shell;
2) hot destructive distillation: the nut-shell after removal of impurities is joined together with charcoal in pyrolysis still, nut-shell and charcoal ratio are 5-8:2-3 is when under 550 DEG C of isolated air, pyrolysis 5-10 is little in temperature, then pyrolysis 2-4 hour under temperature is 350 DEG C of isolated air;
3) condensation: condenser condenses is obtained thick pyroligneous liquor by the gas of drawing from pyrolysis still;
4) leave standstill: crude pyroligneous acid is put stratification in a reservoir together with ethanol;
5) distill: get the middle layer that layering obtains and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, and condensation obtains refining pyroligneous liquor.
Embodiment 8
1) removal of impurities: by the Impurity removal in nut-shell;
2) hot destructive distillation: the nut-shell after removal of impurities is joined together with charcoal in pyrolysis still, nut-shell and charcoal ratio are 5-8:2-3 is when under 530 DEG C of isolated air, pyrolysis 5-10 is little in temperature, then pyrolysis 2-4 hour under temperature is 350 DEG C of isolated air;
3) condensation: condenser condenses is obtained thick pyroligneous liquor by the gas of drawing from pyrolysis still;
4) leave standstill: crude pyroligneous acid is put stratification in a reservoir together with ethanol;
5) distill: get the middle layer that layering obtains and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, and condensation obtains refining pyroligneous liquor.
Embodiment 9
1) removal of impurities: by the Impurity removal in nut-shell;
2) hot destructive distillation: the nut-shell after removal of impurities is joined together with charcoal in pyrolysis still, nut-shell and charcoal ratio are 5-8:2-3 is when under 520 DEG C of isolated air, pyrolysis 5-10 is little in temperature, then pyrolysis 2-4 hour under temperature is 350 DEG C of isolated air;
3) condensation: condenser condenses is obtained thick pyroligneous liquor by the gas of drawing from pyrolysis still;
4) leave standstill: crude pyroligneous acid is put stratification in a reservoir together with ethanol;
5) distill: get the middle layer that layering obtains and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, and condensation obtains refining pyroligneous liquor.
Claims (1)
1. prepare a method for pyroligneous liquor, it is characterized in that comprising the steps:
1) removal of impurities: by the Impurity removal in nut-shell;
2) hot destructive distillation: the nut-shell after removal of impurities is joined together with charcoal in pyrolysis still, nut-shell and charcoal ratio are 5-8:2-3 is when under 450-550 DEG C of isolated air, pyrolysis 5-10 is little in temperature, then pyrolysis 2-4 hour under temperature is 350-380 DEG C of isolated air;
3) condensation: condenser condenses is obtained thick pyroligneous liquor by the gas of drawing from pyrolysis still;
4) leave standstill: crude pyroligneous acid is put stratification in a reservoir together with ethanol;
5) distill: get the middle layer that layering obtains and carry out rectifying, rectifying condition is: temperature 120-140 DEG C, and condensation obtains refining pyroligneous liquor.
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| CN201410617932.0A CN104327874B (en) | 2014-11-05 | 2014-11-05 | The method preparing pyroligneous liquor |
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| CN104327874B CN104327874B (en) | 2016-08-17 |
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Cited By (7)
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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 |
| 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 |
| CN106811225A (en) * | 2015-11-30 | 2017-06-09 | 鹿岩 | The refining separation device of pyrolkigneous liquid |
| 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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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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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