CN112480955A - Method for separating wood vinegar and wood tar - Google Patents
Method for separating wood vinegar and wood tar Download PDFInfo
- Publication number
- CN112480955A CN112480955A CN202011131914.3A CN202011131914A CN112480955A CN 112480955 A CN112480955 A CN 112480955A CN 202011131914 A CN202011131914 A CN 202011131914A CN 112480955 A CN112480955 A CN 112480955A
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- CN
- China
- Prior art keywords
- wood
- wood tar
- separating
- tar
- wood vinegar
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- 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.)
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Classifications
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0217—Separation of non-miscible liquids by centrifugal force
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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)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
- Compounds Of Unknown Constitution (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for separating wood vinegar and wood tar. The method follows the following key steps in sequence: firstly, preliminarily and quickly separating the pyroligneous liquor from the insoluble wood tar by using high-speed centrifugal operation; the key step two, using chromatographic separation operation to finely separate the wood vinegar liquid and the soluble wood tar. Compared with the traditional method for separating the wood vinegar from the wood tar, the technical route provided by the patent has the advantages of high efficiency, low cost and good separation effect, and is beneficial to the development of the wood vinegar industry.
Description
Technical Field
The present invention belongs to the field of three-waste treating and comprehensive utilizing technology.
Background
The wood vinegar liquid system condenses pyrolysis gas generated by slowly pyrolyzing biomass to obtain mixed liquid of wood vinegar liquid and wood tar, and then separates the mixed liquid to obtain clear reddish brown liquid. The application field of the wood vinegar is wide. At present, the method is applied to the fields of agricultural production (soil disinfectants, compost fermentation promoters, plant growth regulators and pesticide auxiliaries) and chemical industry (basic raw materials for organic synthesis are available on the market as basic raw materials of a plurality of organic fertilizers), and the refined pyroligneous liquor can be applied to the fields of food, medical treatment and health (antibacterial agents, insect-proof agents, anti-inflammatory agents, antipruritic agents and sewage treatment).
At present, the common methods for separating the mixed liquid of the pyroligneous liquor and the wood tar at home and abroad to obtain the pyroligneous liquor product comprise a standing separation method, an activated carbon adsorption method, an extraction method, a low-temperature freezing method and a distillation method. The standing separation method has simple equipment and easy operation, but the standing time of the method is short, namely several months, and is more than half a year, and the time is long. The activated carbon adsorption method has high cost and the activated carbon is difficult to regenerate. The extraction method has the defects that a third component needs to be introduced into a system, and the pyroligneous component and an extracting agent need to be separated after extraction, so that the operation is complicated. The low-temperature freezing method has large energy consumption and high cost and is only suitable for laboratory operation. The distillation method is convenient to operate, the equipment is relatively simple, but many components of the pyroligneous liquor cannot be collected in the distillation process, and meanwhile, the energy consumption of the distillation operation is large.
The invention provides a method for separating pyroligneous liquor and wood tar mixed liquor by adopting a high-speed centrifugation-chromatographic separation method, aiming at the defects of the prior method for preparing the pyroligneous liquor product by separating the pyroligneous liquor and the wood tar mixed liquor at home and abroad. The high-speed centrifugation is to generate a strong centrifugal field by means of high-speed rotation, and firstly, the pyroligneous liquor and insoluble wood tar contained in the wood tar are centrifugally separated. The operation of the step adopts simple equipment, does not need additional reagent, has short operation process and high efficiency; and then carrying out chromatographic separation on the mixed solution from which the insoluble wood tar is removed, and adsorbing and removing the soluble wood tar in the mixed solution. The method has the advantages of simple equipment, easy regeneration of chromatographic column, repeated use, and improved separation efficiency and effect. The method provided by the invention is convenient to operate, can effectively reduce the separation cost of the wood vinegar liquid and the wood tar mixed liquid, and has higher efficiency.
Disclosure of Invention
Firstly, performing high-speed centrifugal operation on a mixed solution of pyroligneous liquor and wood tar, wherein the separation factor during the high-speed centrifugal operation is not lower than 20000, the centrifugal speed during the high-speed centrifugal operation is not lower than 5000r/min, and the mixed solution is layered into a light phase (the pyroligneous liquor and the soluble wood tar) and a heavy phase (insoluble wood tar) through the high-speed centrifugal operation, so that the insoluble wood tar is removed from the mixed solution.
And then performing chromatographic separation on the mixed solution without the insoluble wood tar, wherein the stationary phase used in the chromatographic separation is macroporous adsorption resin formed by polymerizing and crosslinking a compound with aromatic groups by using a stationary phase, and the crosslinking degree of the resin is 5-9%. The stationary phase adsorbs the soluble wood tar in the mixed solution, thereby realizing the removal of the soluble wood tar from the wood vinegar and obtaining the wood vinegar product.
Detailed Description
The first embodiment is as follows:
[1] taking the pyrolysis mixed solution obtained by separating slow pyrolysis birch and condensing as an example, the mixed solution of pyroligneous liquor and wood tar is firstly subjected to high-speed centrifugal operation, the separation factor when the high-speed centrifugal operation is carried out is 22000, the centrifugal rotation speed when the high-speed centrifugal operation is carried out is 6000r/min, and the mixed solution is separated into a light phase (pyroligneous liquor and soluble wood tar, which account for 92 wt% of the pyrolysis mixed solution) and a heavy phase (which accounts for 8 wt% of the pyrolysis mixed solution) through the high-speed centrifugal operation, so that the insoluble wood tar is removed from the mixed solution.
[2] And then carrying out chromatographic separation on the mixed solution from which the insoluble wood tar is removed, wherein a stationary phase used in the chromatographic separation adopts macroporous adsorption resin formed by styrene-divinylbenzene copolymer with the crosslinking degree of 7%, and the stationary phase adsorbs the soluble wood tar in the mixed solution (accounting for 22 wt% of the pyrolysis mixed solution), so that the soluble wood tar is removed from the pyroligneous liquor, and the pyroligneous liquor product (accounting for 70%) is obtained.
Example two:
[1] taking pyrolysis mixed liquor obtained by separating slow pyrolysis pine and condensing as an example, firstly performing high-speed centrifugal operation on the mixed liquor of the wood vinegar liquor and the wood tar, wherein the separation factor during the high-speed centrifugal operation is 30000, the centrifugal speed during the high-speed centrifugal operation is 6500r/min, and through the high-speed centrifugal operation, the mixed liquor is layered into a light phase (the wood vinegar liquor and the soluble wood tar, which account for 76 wt% of the pyrolysis mixed liquor) and a heavy phase (which accounts for 24 wt% of the pyrolysis mixed liquor), so that the insoluble wood tar is removed from the mixed liquor.
[2] And then carrying out chromatographic separation on the mixed solution from which the insoluble wood tar is removed, wherein a stationary phase used in the chromatographic separation adopts macroporous adsorption resin formed by styrene-divinylbenzene copolymer with the crosslinking degree of 8%, and the stationary phase adsorbs the soluble wood tar (accounting for 22 wt% of the pyrolysis mixed solution) in the mixed solution, so that the soluble wood tar is removed from the pyroligneous liquor, and the pyroligneous liquor product (accounting for 70%) is obtained.
Example three:
[1] taking the pyrolysis mixed solution obtained by separating the slow-speed pyrolysis spruce and condensing as an example, the mixed solution of the wood vinegar solution and the wood tar is firstly subjected to high-speed centrifugation, the separation factor when the high-speed centrifugation is carried out is 28000, the centrifugation speed when the high-speed centrifugation is carried out is 7000r/min, and the mixed solution is separated into a light phase (the wood vinegar solution and the soluble wood tar which account for 77 wt% of the pyrolysis mixed solution) and a heavy phase (the pyrolysis mixed solution which accounts for 23 wt%) through the high-speed centrifugation operation, so that the insoluble wood tar is removed from the mixed solution.
[2] And then carrying out chromatographic separation on the mixed solution from which the insoluble wood tar is removed, wherein a stationary phase used in the chromatographic separation adopts macroporous adsorption resin formed by styrene-divinyl copolymer with the crosslinking degree of 6%, and the stationary phase adsorbs the soluble wood tar in the mixed solution (accounting for 11 wt% of the pyrolysis mixed solution), so that the soluble wood tar is removed from the pyroligneous liquor, and the pyroligneous liquor product (accounting for 66%) is obtained.
Claims (2)
1. A method for separating wood vinegar and wood tar is characterized in that: the method follows the following key steps in sequence: firstly, preliminarily and quickly separating the pyroligneous liquor from the insoluble wood tar by using high-speed centrifugal operation; the key step two, using chromatographic separation operation to finely separate the wood vinegar liquid and the soluble wood tar.
2. The method of separating wood vinegar from wood tar according to claim 1, wherein: the key steps are that the separation factor of the high-speed centrifugal operation is not lower than 20000, and the centrifugal speed is not lower than 5000 r/min; the stationary phase used in the chromatographic separation operation of the key step II is macroporous adsorption resin formed by polymerizing and crosslinking compounds with aromatic groups, and the crosslinking degree of the resin is 5-9%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011131914.3A CN112480955A (en) | 2020-10-21 | 2020-10-21 | Method for separating wood vinegar and wood tar |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011131914.3A CN112480955A (en) | 2020-10-21 | 2020-10-21 | Method for separating wood vinegar and wood tar |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112480955A true CN112480955A (en) | 2021-03-12 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011131914.3A Pending CN112480955A (en) | 2020-10-21 | 2020-10-21 | Method for separating wood vinegar and wood tar |
Country Status (1)
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| CN (1) | CN112480955A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000313885A (en) * | 1999-04-27 | 2000-11-14 | Gamano Kensetsu Kk | Method for clarifying pyroligneous acid by freezing and thawing |
| WO2018009052A1 (en) * | 2016-07-05 | 2018-01-11 | Saw Gee Shyang | A method of producing bio-fertiliser |
| CN108285804A (en) * | 2018-01-18 | 2018-07-17 | 浙江农林大学 | A kind of method that wood vinegar removes water concentration and separating tar |
| CN108707481A (en) * | 2018-06-08 | 2018-10-26 | 农业部规划设计研究院 | Grease continuous separation device in a kind of pyrolysis gas |
| CN110180215A (en) * | 2019-05-31 | 2019-08-30 | 南京三聚生物质新材料科技有限公司 | Application, chromatographic column and separation method of the walnut shell in wood vinegar separating-purifying |
-
2020
- 2020-10-21 CN CN202011131914.3A patent/CN112480955A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000313885A (en) * | 1999-04-27 | 2000-11-14 | Gamano Kensetsu Kk | Method for clarifying pyroligneous acid by freezing and thawing |
| WO2018009052A1 (en) * | 2016-07-05 | 2018-01-11 | Saw Gee Shyang | A method of producing bio-fertiliser |
| CN108285804A (en) * | 2018-01-18 | 2018-07-17 | 浙江农林大学 | A kind of method that wood vinegar removes water concentration and separating tar |
| CN108707481A (en) * | 2018-06-08 | 2018-10-26 | 农业部规划设计研究院 | Grease continuous separation device in a kind of pyrolysis gas |
| CN110180215A (en) * | 2019-05-31 | 2019-08-30 | 南京三聚生物质新材料科技有限公司 | Application, chromatographic column and separation method of the walnut shell in wood vinegar separating-purifying |
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