CN101368106A - Purifying process for solution of wood vinegar - Google Patents

Purifying process for solution of wood vinegar Download PDF

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Publication number
CN101368106A
CN101368106A CNA2008101413504A CN200810141350A CN101368106A CN 101368106 A CN101368106 A CN 101368106A CN A2008101413504 A CNA2008101413504 A CN A2008101413504A CN 200810141350 A CN200810141350 A CN 200810141350A CN 101368106 A CN101368106 A CN 101368106A
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membrane
wood vinegar
water tank
water
membrane separation
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CN101368106B (en
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王宏力
林振衡
李敏
陈平
刘兴
王柏楠
梁伟刚
王启翰
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HENAN CHEMICAL INDUSTRY RESEARCH INSTITUTE CO LTD
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HENAN CHEMICAL INDUSTRY RESEARCH INSTITUTE CO LTD
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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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Abstract

The invention relates to a method of the purification technology of pyracetic acid. The method is characterized in that the method comprises the following steps: firstly, the stock solution in a stock solution bath is fed into a two stage pre-filtration system and a two stage secondary precision filtration system which are connected in series to be filtered; secondly, the filtered solution obtained in the first step is fed into multistage membrane separating systems which are connected in series at intervals in sequence and are composed of at least three stage membrane separating devices and three water washing boxes to be separated; wherein, the concentrated water separated through the primary stage membrane separating device is respectively fed into the stock solution bath and a concentrated water tank; the concentrated water separated through the secondary stage membrane separating device is fed into the concentrated water tank through a pipeline; the concentrated water separated through the tertiary stage membrane separating device is respectively fed into the first water washing box and the second water washing box through a pipeline; finally the concentrated pyracetic acid with 50 percent of content is obtained in the concentrated water tank, and the separated fresh water is discharged after being metered through the third water washing box.

Description

The purification technique of wood vinegar
Technical field
The present invention designs chemistry (chemical industry) technology, relates to a kind of purification technique of wood vinegar specifically.
Background technology
Wood vinegar is the precious material that extracts from natural phant pyrolysis charring process, contains 200 kinds of organism, is a kind of component complexity, diverse in function and metastable system material.Because the natural overall equilbrium mechanism of action of numerous micro substance factors shows mysterious usefulness in actual applications in the wood vinegar.To the further investigation of wood vinegar, every performance of wood vinegar is familiar with day by day with effect and is obtained paying attention to along with both at home and abroad, begins to be widely used in agricultural, forestry, livestock industry, food-processing industry, medical and health industry and light industry industry.Especially wood vinegar has multiple effects such as promoting plant-growth, antibiotic, diseases prevention, is good green fertilizer and agricultural chemicals, and the application on agricultural more and more widely.
Wood vinegar is filbert to the dark brown translucent liquid, and unique sootiness fragrance is arranged, flavor acid, and pH value 1.5-3.7, proportion about 1.0025 contains more than 200 kind of organic components such as acids, alcohols, phenols, aldehydes, ketone, wherein organic content 7-15%.
Because above-mentioned wood vinegar organic concentration is lower, the development and application of derived product brought a lot of inconvenience, be unusual difficulty especially as commodity selling, can cause severe contamination to environment and underground water simultaneously.It can only be carried out purifying and concentrate, the wood vinegar organic concentration be reached more than 50% just can have commercial value preferably.The purifying concentration method that was in the past adopted all is to carry out heating method, boils off part moisture content by the method for evaporating, and the wood vinegar organic content is improved, but the processing method of above-mentioned this heating evaporation exists following weak point:
(1) it is bigger to be used to heat the distillatory energy consumption, and every processing purifying concentrates one ton of wood vinegar (organic content 50%), and expense is at 200 yuans.
(2) be entrained with the organic substance of part in the moisture content that distills, make the biomass composition of the wood vinegar after concentrating that variation take place, can't guarantee the primordial condition of crude substance, use to derived product to produce detrimentally affect.
(3) wood vinegar after distillation heating owing to through 100 ℃ high-temperature technology situation, make the chemical transformation that has produced part between the each component, makes the biomass body of wood vinegar suffer destruction.
Summary of the invention
Purpose of the present invention provides a kind of purification technique of wood vinegar just at existing weak point in the above-mentioned prior art.Method of the present invention is important to be to adopt multistage membrane separation process technology wood vinegar to be carried out the purifying process of cold concentration, the series connection of the membrane module by a plurality of different apertures, finally obtain, maintain the concentrated wood vinegar of 50% organic content of wood vinegar biomass substance.
Processing method of the present invention comprises the steps: a, at first the stoste in the former liquid pool is sent in the two-stage pre-filtering that is connected with series system, the smart filtering system of two-stage and filtered; B, the filtered liquid of step a gained is sent into separating that series system is provided with at interval successively again by at least three grades of membrane separation units and the multistage film separating system that three water tanks are formed; Wherein, sent into former liquid pool and dense water tank through the isolated dense water liquid of one-level membrane separation unit respectively via pipeline; Be admitted to dense water tank through the isolated dense water liquid of secondary membrane separation unit via pipeline; Sent into first water tank and second water tank through three grades of isolated dense water liquid of membrane separation unit respectively via pipeline; Finally obtain the concentrated wood vinegar of 50% content, the discharging after the metering of the 3rd water tank of isolated fresh water at dense water tank.
Principle of work of the present invention is as follows:
One) pretreatment technology
1, pre-filtering treatment system
The purpose one that pre-filtering is handled is to remove the turbidity of excess and suspended solids, colloidalmaterial; The 2nd, suppress or control the formation of compound, prevent the passage of their precipitation obstruction water or form coating on the film surface; The 3rd, prevent the pollution of particulate material and microorganism to film and assembly.
In a word, when the pre-filtering of membrane separation unit feed water is handled, need to consider two aspects: the one, prevent pollution and the obstruction of suspended substance, colloid and microorganism to film and pipe interior; Be the precipitation fouling that will prevent difficulty soluble salt on the other hand.When the result of two aspects can both reach requirement, could guarantee the normal operation of film device.
2, the smart filter of one-level
The effect of the smart filter of one-level is to remove large granular impurities such as suspended matter and flocculent substance.Its filtering accuracy is 5 μ m, and it also belongs to the pretreatment technology device of film separating system, can remove the above granule foreign of 5 μ m, alleviates the operating load of subsequent technique film effectively.
3, the smart filter of secondary
The smart filter of secondary is the same with the principle of the smart filter of one-level, but the smart filter of secondary is meticulousr than the smart filter of one-level, and the filter element filtering precision that it adopts is 1 μ m, and the material of being removed is more, and is thinner, and the two combination more can guarantee carrying out smoothly of subsequent film treating processes.
Two) film separating system
1. ultrafiltration (being called for short UF): one-level membrane separation unit
(1) principle of work
Ultrafiltration is a kind of water purification, solution separating, concentrated of being widely used in.And recover useful materials from waste water, purification of waste water utilizes the new and high technology in field again.The core parts of ultra-filtration equipment are hollow fiber ultrafiltration membrane.Hollow fiber ultrafiltration membrane is an important branch in the ultra-filtration technique, is the most ripe and advanced in the ultra-filtration technique.
In the membrane separation technique category, its separation accuracy is reflexive to be infiltrated in the micro-filtration filter area, and ultrafiltration is (MF＜UF＜NF＜R0) between nanofiltration and micro-filtration.The field of definition of ultrafiltration is a molecular weight cut-off about 500～500000, and the approximation of corresponding membrane pore size is 0.002 μ～0.1 μ.Ultra-filtration membrane is as sieve, (under 0.1～0.6MPa), allows solvent and sees through less than the solute of membrane pore size, and stop the solute greater than the aperture to pass through, with purification, the separation of finishing solution with concentrate at certain pressure.
Because the singularity of its structure, film does not have supporting mass, and moulding process continuity, homogeneity are good, simple in structure, and ultrafiltrated is easy to keep advantage such as pure, has accounted for space of top prominence in the ultrafiltration Application for Field.
(2) technical characterstic
1. ultra-filtration process does not have the variation of phase border, can separate under normal temperature and low pressure, thereby energy consumption is low, is about 1/2～1/5 of method of evaporation and cold method;
2. equipment volume is little, and is simple in structure, and working temperature is at 5～45 ℃, and working pressure requires 0.05～0.15MPa, need not heat, and low pressure operation, energy conservation, so it is investment cost is low, easy to implement;
3. the ultra-filtration and separation process is simple positive delivery liquid, and technical process is simple, the easy handling management;
4. the variation of matter does not take place in solution in separation, concentration process, thereby is suitable for protecting the processing of flavor and thermosensitive solution;
5. be suitable for Separation and Recovery valuable macromolecular substance of trace and lower concentration macromolecular substance from dilute solution;
6. can be with the material fractional separation of different molecular weight;
7. ultra-filtration membrane is the even continuum of being made by high molecular polymer, does not in use have coming off of any impurity, guarantees the pure of processed solution.
2, nanofiltration (being called for short NF): secondary membrane separation unit
(1) principle of work
Nanofiltration membrane and reverse osmosis membrane do not have obvious limit.Reverse osmosis membrane and nanofiltration membrane must link together just meaningfully with having semi-permeable membranes that permission solvent (water molecules) sees through, R0 phenomenon and UF phenomenon just can occur.Nanofiltration membrane (NF) is one of four big membrane separation techniques, nanofiltration membrane is a kind of functional semi-permeable membranes that allows solvent molecule or some low molecular weight solutes or low price ion to see through, it because of the size that can hold back material be 1nm (nanometer) promptly 0.001 μ m gain the name, the filtering accuracy of nanofiltration membrane is between ultra-filtration membrane (UF) and reverse osmosis membrane (R0).
(2) characteristics and function
The core parts of nano-filtration membrane equipment are nanofiltration membrane, its very big feature is that membrane body has electric charge, the major reason of this to be it still have under low pressure very higher desalting performance generally can be removed the organism of relative molecular mass about 200～400, the ability of holding back dissolved salt is between 20%～98%, decreasing ratio to the monovalent anion salts solution is lower than high price anion salt solution, as NaC1 and CaCL 2Decreasing ratio be 20%～80%, and MgSO 4And Na 2SO 4Decreasing ratio be 90%～98%.
Nanofiltration membrane generally is used to remove the organism and the colourity on the face of land, remove the hardness and the radiation radium of well water, part is removed solvability salt, useful matter in enriching food and the separation medicine etc., the operation pressure reduction of nanofiltration membrane both sides is generally 0.35～1.6MPa, and this programme employing nanofiltration membrane energy molecular weight cut-off is the organism more than 300.Its standard decreasing ratio is 60～80%.This series membranes can be operated under ultralow pressure, reduces the pressure of back order processing apparatus, thereby realizes energy-conservation, as to reduce facility investment and process cost purpose.
3, reverse osmosis (being called for short R0): three grades of membrane separation units
(1) reverse osmosis membrane principle
The aperture of reverse osmosis mostly≤10 * 10 -10M, its separate object is to be in the inorganics of ionic condition and the organism (molecular weight is more than 50) of the overwhelming majority in the solution.
Reverse osmosis is to utilize this physical phenomenon of infiltration to realize isolating.To two kinds of water that contain different concns salt, separate with a film with semipermeability matter, can find that the water on one side that salt concentration is low can see through membrane permeation to the high one side of salt concentration, but the salinity that it contained and impermeable.So little by little merge till the salt concentration on both sides equates.The process of osmosis of nature is very long.In order to accelerate this fusion process, can increase a pressure in high water one side of saltiness, allow infiltration stop, the seepage water pressure of Here it is film.Pressure is strengthened, water just can inverse osmosis again, and then salinity stays, and this has just formed the desalination principle of reverse osmosis membrane.I.e. in water salty (as seawater), in addition bigger than naturally osmotic pressure pressure carries out infiltration round about, and the water molecules in the water of source is pressed onto the other side of film, becomes clean water, thereby reaches the purpose of removing salinity in the water.
(2) technical characterstic
Adopt the method for reverse osmosis membrane separation to purify water to be the side to film to apply external pressure, small-molecule substances such as water, methyl alcohol can see through the dilute side that the film surface enters film, and macromolecular organism has just been stayed the dense water side of film.Realize separating of larger molecular organics and small organic molecule and water with this, also just reduced COD and the ammonia nitrogen in the fresh water naturally.
The low pressure reverse osmosis film can be removed larger molecular organics, COD and ammonia nitrogen effectively under lower operating pressure.Its working process is exactly that the centrifugation of membrane sepn-by film is separated into dense water and fresh water two portions with the water inlet of film system; The high pressure reverse osmosis membrane is to remove larger molecular organics, COD and ammonia nitrogen under elevated pressures effectively, adopts high-pressure membrane to handle in this technology earlier, adopts low-pressure membrane further to purify water then, makes last water outlet reach requirement.
Beneficial effect of the present invention is as follows:
(1) from separation, separablely in the crude pyroligneous acid per ton go out 50% fresh water, reached substantially that membrane sepn concentrates.
(2), do not change by the organic body in the wood vinegar of cold concentration from organic composition.
(3) from being processed into originally, processing costs per ton is calculated by 100 degree electricity, is about 70 yuans, is about 200 yuans (wherein also having the organic loss of part) and concentrate the energy consumption of using with heat.
(4) from environment protection treating, the water technology expense is per ton routinely is about 50 yuans, that is to say that you do not utilize wood vinegar will spend 50 yuans yet and handle waste water.
(5) wood vinegar of resulting 50% content in processing back has good commercial value, about about 10000 yuan of price per ton.
Its advantage is as follows:
(1) adopted and taken off isolation technique, can make wood vinegar be in the deepfreeze enrichment stage.
(2) preserved the biological body in the wood vinegar and provide guarantee for the derived product use.
(3) a large amount of energy consumptions required in the concentrated and purified process have been saved.
(4) produced high density symphysis material wood vinegar with higher commercial value.
(5) caused environmental pollution to carry out thorough improvement to wood vinegar, saved pollution abatement costs, and it has been turned waste into wealth produced favorable economic benefit, social benefit and environmental benefit, for applying of renewable energy source item provides favourable support.
Description of drawings
Accompanying drawing is a process flow sheet of the present invention.
Embodiment
The present invention is further described below with reference to embodiment:
As shown in the figure, processing method of the present invention comprises the steps: a, at first will send into by pipeline in the smart filtering system of two-stage pre-filtering, two-stage that is connected with series system through the stoste after former liquid pool precipitation, the cooling and filter; B, the filtered liquid of step a gained is sent in the multistage film separating system that three grades of membrane separation units being provided with at interval successively with series system and three water tanks form by pipeline separated again; Wherein, sent into former liquid pool and dense water tank through the isolated dense water liquid of one-level membrane separation unit respectively via pipeline; Be admitted to dense water tank through the isolated dense water liquid of secondary membrane separation unit via pipeline; Sent into first water tank and second water tank through three grades of isolated dense water liquid of membrane separation unit respectively via pipeline; Finally obtain the concentrated wood vinegar of 50% content, the discharging after the metering of the 3rd water tank of isolated fresh water at dense water tank.
Filter membrane in the membrane separation unit of one-level described in the present invention is a hollow fiber ultrafiltration membrane, the molecular weight cut-off about 500～500000 of this ultra-filtration membrane, and the approximation of corresponding membrane pore size is 0.002 μ～0.1 μ.Filter membrane in the described secondary membrane separation unit is a nanofiltration membrane, this nanofiltration membrane is a kind of functional semi-permeable membranes that allows solvent molecule or some low molecular weight solutes or low price ion to see through, its size of holding back material is 1nm, i.e. 0.001 μ m, molecular weight is more than 300, and filtering accuracy is between ultra-filtration membrane and reverse osmosis membrane.Filter membrane in described three grades of membrane separation units is a reverse osmosis membrane, the aperture of this reverse osmosis membrane≤10 * 10 -10M, its separate object is to be in the inorganics of ionic condition and the organism (molecular weight is more than 50) of the overwhelming majority in the solution.

Claims (4)

1. the purification technique of a wood vinegar is characterized in that: this method comprises the steps: a, at first the stoste in the former liquid pool is sent in the smart filtering system of two-stage pre-filtering, two-stage that is connected with series system and filtered; B, the filtered liquid of step a gained is sent into separating that series system is provided with at interval successively again by at least three grades of membrane separation units and the multistage film separating system that three water tanks are formed; Wherein, sent into former liquid pool and dense water tank through the isolated dense water liquid of one-level membrane separation unit respectively via pipeline; Be admitted to dense water tank through the isolated dense water liquid of secondary membrane separation unit via pipeline; Sent into first water tank and second water tank through three grades of isolated dense water liquid of membrane separation unit respectively via pipeline; Finally obtain the concentrated wood vinegar of 50% content, the discharging after the metering of the 3rd water tank of isolated fresh water at dense water tank.
2. the purification technique of wood vinegar according to claim 1, it is characterized in that: the filter membrane in the described one-level membrane separation unit is a hollow fiber ultrafiltration membrane, the molecular weight cut-off about 500～500000 of this ultra-filtration membrane, the approximation of corresponding membrane pore size are 0.002 μ～0.1 μ.
3. the purification technique of wood vinegar according to claim 1, it is characterized in that: the filter membrane in the described secondary membrane separation unit is a nanofiltration membrane, this nanofiltration membrane is a kind of functional semi-permeable membranes that allows solvent molecule or some low molecular weight solutes or low price ion to see through, its size of holding back material is 1nm, i.e. 0.001 μ m, molecular weight is more than 300, and filtering accuracy is between ultra-filtration membrane and reverse osmosis membrane.
4. the purification technique of wood vinegar according to claim 1, it is characterized in that: the filter membrane in described three grades of membrane separation units is a reverse osmosis membrane, the aperture of this reverse osmosis membrane≤10 * 10 -10M, its separate object is to be in the inorganics of ionic condition and the organism of the overwhelming majority in the solution, molecular weight is more than 50.
CN200810141350A 2008-09-12 2008-09-12 Purifying process for solution of wood vinegar Expired - Fee Related CN101368106B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101697738B (en) * 2009-10-27 2011-11-30 西北农林科技大学 Method for continuously extracting antibactial substances and antioxidant substances from pyrolignucs acid
CN102512961A (en) * 2011-10-28 2012-06-27 商丘三利新能源有限公司 Technology for purifying wood vinegar
CN112011355A (en) * 2020-09-21 2020-12-01 阜阳师范大学 Wood vinegar refining and purifying method

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101697738B (en) * 2009-10-27 2011-11-30 西北农林科技大学 Method for continuously extracting antibactial substances and antioxidant substances from pyrolignucs acid
CN102512961A (en) * 2011-10-28 2012-06-27 商丘三利新能源有限公司 Technology for purifying wood vinegar
CN112011355A (en) * 2020-09-21 2020-12-01 阜阳师范大学 Wood vinegar refining and purifying method

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Free format text: CORRECT: INVENTOR; FROM: WANG HONGLI LIN ZHENHENG LI MIN CHEN PING LIU XING WANG BAINAN LIANG WEIGANG WANG QIHAN ZHANG HELIN ZHU DONGFANG BAO XINDANG MAO JIE ZHANG YUE WANG XINXIANG YANG XIAOGANG CHAI YONGLI MENG WEI GU ZHONGMING LIU YULIN LI YANGUO WU ZHEN ZHAO YILI LIU XIUWEI HU MEI LU CHAO KUANG WENHUI XIA CHENGHAO ZHANG HUIMIN CHEN JIE WANG XIAOYI LIU JIHUA GUO GE FENG YUJUN ZHAO SHENGYONG LIU YI TO: WANG HONGLI LIN ZHENHENG ZHUANG XINSHENG CHEN PING LIU XING WANG BAINAN QU JIANHAI WANG QIHAN LIU GUOLIANG ZHAO LIXIN WANG LEI MAO JIE ZHANG YUE WANG XINXIANG YANG XIAOGANG CHAI YONGLI MENG WEI GU ZHONGMING LIU YULIN LI YANGUO WU ZHEN ZHAO YILI LIU XIUWEI HU MEI LU CHAO KUANG WENHUI XIA CHEN

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