CN108285803A - A kind of method that bamboo vinegar removes water concentration and separating tar - Google Patents
A kind of method that bamboo vinegar removes water concentration and separating tar Download PDFInfo
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- CN108285803A CN108285803A CN201810070673.2A CN201810070673A CN108285803A CN 108285803 A CN108285803 A CN 108285803A CN 201810070673 A CN201810070673 A CN 201810070673A CN 108285803 A CN108285803 A CN 108285803A
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- bamboo vinegar
- organic solvent
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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
-
- 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
- C10C1/00—Working-up tar
-
- 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
- C10C1/00—Working-up tar
- C10C1/04—Working-up tar by distillation
-
- 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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- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of bamboo vinegar water removal concentration and the methods of separating tar.Belong to natural products deep stirring stake field.Bamboo vinegar includes the organic acid and tar, 90% or more moisture less than 10%, and because packing 10 times of increases with logistics cost, it is zero or negative price status to lead to price.In addition bamboo tar niff makes one to detest, be had adverse effect to safety of human and livestock and ecological environment security.The present invention solves the technical barrier of this technical bottleneck and water removal concentration.The method of the present invention is simply at low cost.The present invention is directed to solve the above market-oriented problem with technological means, it is characterised in that 6 techniqueflows are technological package circuit, are successively respectively：Closed inorganic salts drying, closed organic solvent are dissolved, are separated by filtration, alternating temperature distillation, recycling organic solvent is recycled, the water removal of inorganic salts drier recycles.
Description
Technical field
The present invention relates to a kind of bamboo vinegar water removal concentration and the methods of separating tar, are used for refined bamboo vinegar, belong to natural
The method of product manufacture field, specifically a kind of bamboo vinegar water removal concentration and separating tar.
Background technology
Bamboo charcoal especially bamboo absorbent charcoal price is up to 12000 yuan per ton or more, has good profit and market development empty
Between, therefore, the industry of bamboo charcoal is increasing, but the application development of bamboo vinegar is very slowly, as environmental protection verification is more and more tighter
Lattice greatly constrain the sustainable development of bamboo charcoal.The ingredient of bamboo vinegar has hundreds of, and main includes the organic matter less than 10%
(organic matter is organic acid and tar), 90% or more moisture, large quantity of moisture is due to packing and 10 times of logistics cost
It is added above, make its organic substance value well below packaging logistics cost, it is zero or negative price status, bamboo vinegar to lead to price
Have become nugatory waste.However bamboo vinegar belongs to natural products, has in terms of health care and agricultural extensive
Application value however, bamboo tar niff not only makes one to detest, but also has safety of human and livestock and ecological environment security
Adverse effect, therefore, whether the technical barrier how bamboo vinegar removes bamboo tar can widely applied bottleneck as bamboo vinegar.This
Invention not only solves this technical bottleneck, also solves the technical barrier of bamboo vinegar water removal concentration, to make packaging and logistics
90% or more cost savings provide technical support for its extensive use with the marketization.The method of the present invention is simply at low cost, mainly
It is distilled using the extra thermal energy of bamboo charcoal processing factory, drier used can be recycled with organic solvent and be recycled, not only reduce
Production cost also protects ecological environment, production process not to have pollutant emission.
In the compositions, method of chromatography bamboo vinegar, most important sample treatment be exactly remove it is big in bamboo vinegar
Moisture is measured, there are some document reports, mainly uses freeze-drying, organic solvent extractionprocess etc., wherein freeze-drying
Due to expensive, do not have market-oriented prospects for commercial application, organic solvent extractionprocess is not suitable for industry also due to price is too high
Metaplasia is produced.Bamboo vinegar ingredient hundreds of, the selection to organic solvent is difficult, it is ensured that organic solvent can dissolve more bamboo vinegars
Liquid organic matter, while organic solvent being needed easily to be detached with the organic mass-energy of bamboo vinegar.In addition, being also when selecting drier
Limited by various conditions, it is desirable to be able to absorb moisture, not with bamboo vinegar organic matter generate chemical reaction, cannot be dissolved in
Solvent is easily separated etc. the condition requirement met simultaneously with organic solvent.And the organic solvent extractionprocess reported is difficult
Meet conditions above simultaneously, cause dehydration is not clean, miss some bamboo vinegar organic matters, missing inspection bamboo vinegar organic matter it is many at
Grade problem.The present invention has well solved the above technical barrier in selection drier and organic solvents in particular matched combined.
Invention content
It is an object of the invention to overcome defect of the existing technology, a kind of bamboo vinegar water removal concentration is provided and separation is burnt
The method of oil, makes the moisture removal rate of bamboo vinegar reach 99% and 99.5% or more, not only can be directly as chromatographic sample point
The ingredient for analysing bamboo vinegar and bamboo tar, can be used for industrialized production high-concentration bamboo vinegar and bamboo tar.
Number is the percentage number of quality in present specification.
A kind of method of the bamboo vinegar water removal concentration and separating tar, it is characterised in that following technical route is used,
It is specifically divided into following 6 techniqueflows：
1) closed inorganic salts drying.A certain amount of bamboo vinegar is taken, a certain amount of inorganic salts drier (certain measurer is added
Body is the bamboo vinegar that inorganic salts crystallization water quality is equal portions mass fraction), it is closed to stir evenly, stand a period of time.
2) closed organic solvent dissolving.Be added the organic solvent of 1-20 times of bamboo vinegar mass fraction, it is closed be sufficiently stirred after
Dissolving；
3) it is separated by filtration.Filter residue is spare with filtrate；
4) alternating temperature distills.Filtrate is after alternating temperature distills, 40-100 DEG C of 40-190 DEG C of vapo(u)rizing temperature or vacuum distillation temperature
Obtain high-concentration bamboo vinegar and bamboo tar final products and organic solvent；
5) recycling organic solvent is recycled.The organic solvent that techniqueflow 4 recycles, can recycle in techniqueflow
In 2；
6) inorganic salts drier water removal recycles.Filter residue in techniqueflow 3 is heated to 100-260 DEG C, removes the crystallization water,
It recycles in techniqueflow 1.
The method of a kind of bamboo vinegar water removal concentration and separating tar, it is characterised in that the techniqueflow 1
Closed inorganic salts drying, takes the bamboo vinegar of 100 mass units, (a is specially inorganic salts to the inorganic salts drier of a kilograms of addition
Crystallization water quality is 100 mass units), it is closed to stir evenly, stand 30-120 minutes.Inorganic salts drier is specially：Nothing
Brochanite, anhydrous calcium chloride, anhydrous magnesium sulfate, anhydrous sodium sulfate, one or more kinds of mixing of dead plaster.
The method of a kind of bamboo vinegar water removal concentration and separating tar, it is characterised in that the techniqueflow 2
The dissolving of closed organic solvent, is added the organic solvent of 1-20 times of bamboo vinegar mass fraction, it is closed be sufficiently stirred after dissolve, You Jirong
Agent specifically includes：Ethyl alcohol, methanol, formic acid, acetic acid, ethyl acetate, dichloromethane, dimethyl sulfoxide (DMSO) (DMSO), dimethyl formyl
One or more kinds of double solvents of amine (DMF).
The method of a kind of bamboo vinegar water removal concentration and separating tar, it is characterised in that the techniqueflow 3
It is separated by filtration, solid is detached with liquid, it is spare with filtrate to obtain filter residue；
The method of a kind of bamboo vinegar water removal concentration and separating tar, it is characterised in that the techniqueflow 4
Alternating temperature distills, and filtrate is after alternating temperature distills, 40-100 DEG C of 40-190 DEG C of vapo(u)rizing temperature or vacuum distillation temperature, according to having used
The difference of solvent first uses low temperature distillation to collect one kind of organic solvent and high-concentration bamboo vinegar, reuses high temperature distillation receipts
Collect another, obtains high-concentration bamboo vinegar and bamboo tar final products and organic solvent.
The method of a kind of bamboo vinegar water removal concentration and separating tar, it is characterised in that the techniqueflow 5
Recycling organic solvent is recycled, and is referred to the organic solvent of the recycling of techniqueflow 4, can be recycled in techniqueflow 2.
The method of a kind of bamboo vinegar water removal concentration and separating tar, it is characterised in that the techniqueflow 6
The water removal of inorganic salts drier recycles, and refers to that the filter residue in techniqueflow 3 is heated to 100-260 DEG C, removes the crystallization water, repeatedly sharp
In techniqueflow 1.Optimum heating temperature is different according to the type for selecting drier.
The method of a kind of bamboo vinegar water removal concentration and separating tar, it is characterised in that 6 techniqueflows
For technological package circuit, 6 techniqueflow sequences are 123456 or 123645.
The method of a kind of bamboo vinegar water removal concentration and separating tar, it is characterised in that the technical route and side
Method is applied not only to industrial production high-concentration bamboo vinegar and bamboo tar final products, and it is former to can be used for lab analysis bamboo vinegar
The sample preparation of liquid chromatography constituent analysis, the environmental protection that bamboo vinegar can also be produced as bamboo charcoal waste are handled.
Description of the drawings
Fig. 1 is techniqueflow chart
Specific implementation mode
It below will just present invention be described in more detail by example.
Example 1
1) closed inorganic salts drying.The bamboo vinegar of 90kg is taken, 160kg drier anhydrous cupric sulfates are added, closed stirring is equal
It is even, stand 30 minutes；
2) closed organic solvent dissolving.The organic solvent ethyl alcohol of bamboo vinegar mass fraction 450kg is added, it is closed to be sufficiently stirred
Dissolving；
3) it is separated by filtration.Filter residue is spare with filtrate；
4) alternating temperature distills.It is organic solvent second that filtrate obtains distillate by 40 DEG C of 78 DEG C of distillations or vacuum distillation temperature
Alcohol is heated to 60 DEG C of 118 DEG C of distillations or vacuum distillation temperature after distillation completely, and distillate obtains high-concentration bamboo vinegar, remaining
Substance is bamboo tar；
5) recycling organic solvent is recycled.The organic solvent ethyl alcohol that techniqueflow 4 recycles, can recycle in technology
In flow 2；
6) inorganic salts drier water removal recycles.Filter residue cupric sulfate pentahydrate in techniqueflow 3 is heated to 258 DEG C, removal
The crystallization water is recycled in techniqueflow 1.
Example 2
1) closed inorganic salts drying.The bamboo vinegar of 108kg is taken, 111kg drier anhydrous calcium chlorides are added, closed stirring is equal
It is even, stand 45 minutes；
2) closed organic solvent dissolving.The organic solvent dimethylformamide (DMF) of 216kg is added, it is closed to be sufficiently stirred
Dissolving；
3) it is separated by filtration.Filter residue is spare with filtrate；
4) inorganic salts drier water removal recycles.Filter residue calcium chloride hexahydrate in techniqueflow 3 is heated to 260 DEG C, removal
The crystallization water is recycled in techniqueflow 1；
5) alternating temperature distills.It is high concentration bamboo vinegar that filtrate obtains distillate by 60 DEG C of 118 DEG C of distillations or vacuum distillation temperature
Liquid is heated to 153 DEG C of distillations or 78 DEG C of vacuum distillation temperature, distillate obtains organic solvent DMF after distillation completely, remaining
Substance is bamboo tar；
6) recycling organic solvent is recycled.The organic solvent DMF that techniqueflow 5 recycles, can recycle in technology
In flow 2.
Example 3
1) closed inorganic salts drying.The bamboo vinegar of 126kg is taken, 120kg drier anhydrous magnesium sulfates are added, closed stirring is equal
It is even, stand 120 minutes；
2) closed organic solvent dissolving.The organic solvent methanol of bamboo vinegar mass fraction 126kg is added, it is closed to be sufficiently stirred
Dissolving；
3) it is separated by filtration.Filter residue is spare with filtrate；
4) alternating temperature distills.It is organic solvent first that filtrate obtains distillate by 35 DEG C of 65 DEG C of distillations or vacuum distillation temperature
Alcohol is heated to 60 DEG C of 118 DEG C of distillations or vacuum distillation temperature after distillation completely, and distillate obtains high-concentration bamboo vinegar, remaining
Substance is bamboo tar；
5) recycling organic solvent is recycled.The organic solvent methanol that techniqueflow 4 recycles, can recycle in technology
In flow 2；
6) inorganic salts drier water removal recycles.Five water magnesium sulfate of filter residue in techniqueflow 3 is heated to 200 DEG C, removal
The crystallization water is recycled in techniqueflow 1.
Example 4
1) closed inorganic salts drying.The bamboo vinegar of 180kg is taken, 142kg drier anhydrous sodium sulfates are added, closed stirring is equal
It is even, stand 60 minutes；
2) closed organic solvent dissolving.The organic solvent formic acid of bamboo vinegar mass fraction 360kg is added, it is closed to be sufficiently stirred
Dissolving；
3) it is separated by filtration.Filter residue is spare with filtrate；
4) alternating temperature distills.It is organic solvent first that filtrate obtains distillate by 52 DEG C of 101 DEG C of distillations or vacuum distillation temperature
Acid is heated to 60 DEG C of 118 DEG C of distillations or vacuum distillation temperature after distillation completely, and distillate obtains high-concentration bamboo vinegar, remaining
Substance is bamboo tar；
5) recycling organic solvent is recycled.The organic solvent formic acid that techniqueflow 4 recycles, can recycle in technology
In flow 2；
6) inorganic salts drier water removal recycles.Five aqueous sodium persulfate of filter residue in techniqueflow 3 is heated to 100 DEG C, removal
The crystallization water is recycled in techniqueflow 1.
Example 5
1) closed inorganic salts drying.The bamboo vinegar of 180kg is taken, 142kg drier anhydrous sodium sulfates are added, closed stirring is equal
It is even, stand 60 minutes；
2) closed organic solvent dissolving.The organic solvent acetic acid of bamboo vinegar mass fraction 540kg is added, it is closed to be sufficiently stirred
Dissolving；
3) it is separated by filtration.Filter residue is spare with filtrate；
4) alternating temperature distills.It is high concentration bamboo vinegar that filtrate obtains distillate by 52 DEG C of 100 DEG C of distillations or vacuum distillation temperature
Liquid is heated to 118 DEG C of distillations or 60 DEG C of vacuum distillation temperature, distillate obtains organic solvent acetic acid after distillation completely, remaining
Substance is bamboo tar；
5) recycling organic solvent is recycled.The organic solvent formic acid that techniqueflow 4 recycles, can recycle in technology
In flow 2；
6) inorganic salts drier water removal recycles.Filter residue sal glauberi in techniqueflow 3 is heated to 100 DEG C, removal
The crystallization water is recycled in techniqueflow 1.
Example 6
1) closed inorganic salts drying.The bamboo vinegar of 36kg is taken, 136kg drier dead plasters are added, closed stirring is equal
It is even, stand 60 minutes；
2) closed organic solvent dissolving.The organic solvent dimethyl sulfoxide (DMSO) (DMSO) of bamboo vinegar mass fraction 360kg is added,
It is closed to be sufficiently stirred dissolving；
3) it is separated by filtration.Filter residue is spare with filtrate；
4) alternating temperature distills.It is that organic solvent is high that filtrate obtains distillate by 60 DEG C of 118 DEG C of distillations or vacuum distillation temperature
Concentration bamboo vinegar is heated to 90 DEG C of 190 DEG C of distillations or vacuum distillation temperature, distillate obtains organic solvent after distillation completely
DMSO, surplus materials are bamboo tar；
5) recycling organic solvent is recycled.The organic solvent DMSO that techniqueflow 4 recycles, can recycle in technology
In flow 2；
6) inorganic salts drier water removal recycles.Five aqueous sodium persulfate of filter residue in techniqueflow 3 is heated to 163 DEG C, removal
The crystallization water is recycled in techniqueflow 1.
Example 7
1) closed inorganic salts drying.The bamboo vinegar of 180kg is taken, 142kg drier anhydrous sodium sulfates are added, closed stirring is equal
It is even, stand 45 minutes；
2) closed organic solvent dissolving.The organic solvent ethyl acetate of bamboo vinegar mass fraction 900kg is added, it is closed abundant
Stirring and dissolving；
3) it is separated by filtration.Filter residue is spare with filtrate；
4) alternating temperature distills.It is organic solvent acetic acid that filtrate obtains distillate by 40 DEG C of 77 DEG C of distillations or vacuum distillation temperature
Ethyl ester is heated to 60 DEG C of 118 DEG C of distillations or vacuum distillation temperature after distillation completely, and distillate obtains high-concentration bamboo vinegar, remains
Excess matter is bamboo tar；
5) recycling organic solvent is recycled.The organic solvent that techniqueflow 4 recycles, can recycle in techniqueflow
In 2；
6) inorganic salts drier water removal recycles.Filter residue sal glauberi in techniqueflow 3 is heated to 100 DEG C, removal
The crystallization water is recycled in techniqueflow 1.
Example 8
1) closed inorganic salts drying.The bamboo vinegar of 108kg is taken, 111kg drier anhydrous calcium chlorides are added, closed stirring is equal
It is even, stand 60 minutes；
2) closed organic solvent dissolving.The organic solvent dichloromethane of 216kg is added, it is closed to be sufficiently stirred dissolving；
3) it is separated by filtration.Filter residue is spare with filtrate；
4) inorganic salts drier water removal recycles.Filter residue calcium chloride hexahydrate in techniqueflow 3 is heated to 260 DEG C, removal
The crystallization water is recycled in techniqueflow 1；
5) alternating temperature distills.It is that organic solvent is heated to after distillation completely that filtrate obtains distillate by 40 DEG C of distillations
60 DEG C of 117 DEG C of distillations or vacuum distillation temperature, distillate obtain high-concentration bamboo vinegar, and surplus materials is bamboo tar；
6) recycling organic solvent is recycled.The organic solvent that techniqueflow 5 recycles, can recycle in techniqueflow
In 2.
Example 9
1) closed inorganic salts drying.The bamboo vinegar of 180kg is taken, drier is added, and (160kg anhydrous cupric sulfates+71kg is anhydrous
Sodium sulphate), it is closed to stir evenly, stand 90 minutes；
2) closed organic solvent dissolving.Organic solvent (180kg ethyl alcohol+the 180kg of bamboo vinegar mass fraction 360kg is added
Methanol), it is closed to be sufficiently stirred dissolving；
3) it is separated by filtration.Filter residue is spare with filtrate；
4) alternating temperature distills.It is organic solvent that filtrate obtains distillate by 40 DEG C of 78 DEG C of distillations or vacuum distillation temperature,
After distillation completely, it is heated to 60 DEG C of 118 DEG C of distillations or vacuum distillation temperature, distillate obtains high-concentration bamboo vinegar, surplus materials
For bamboo tar；
5) recycling organic solvent is recycled.The organic solvent that techniqueflow 4 recycles, can recycle in techniqueflow
In 2；
6) inorganic salts drier water removal recycles.Filter residue (sal glauberi and cupric sulfate pentahydrate) in techniqueflow 3 adds
Heat removes the crystallization water, recycles in techniqueflow 1 to 258 DEG C.
Example 10
1) closed inorganic salts drying.The bamboo vinegar of 180kg is taken, drier is added, and (160kg anhydrous cupric sulfates+71kg is anhydrous
Sodium sulphate), it is closed to stir evenly, stand 75 minutes；
2) closed organic solvent dissolving.Organic solvent (the 270kgDMF+ of 3 times of bamboo vinegar mass fraction is added
270kgDMSO), closed to be sufficiently stirred dissolving；
3) it is separated by filtration.Filter residue is spare with filtrate；
4) alternating temperature distills.It is high concentration bamboo vinegar that filtrate obtains distillate by 60 DEG C of 117 DEG C of distillations or vacuum distillation temperature
Liquid is heated to 100 DEG C of 190 DEG C of distillations or vacuum distillation temperature, distillate obtains organic solvent, residue after distillation completely
Matter is bamboo tar；
5) recycling organic solvent is recycled.The organic solvent that techniqueflow 4 recycles, can recycle in techniqueflow
In 2；
6) inorganic salts drier water removal recycles.Filter residue (sal glauberi and cupric sulfate pentahydrate) in techniqueflow 3 adds
Heat removes the crystallization water, recycles in techniqueflow 1 to 258 DEG C.
Example 11
1) closed inorganic salts drying.The bamboo vinegar of 180kg is taken, drier is added, and (160kg anhydrous cupric sulfates+71kg is anhydrous
Sodium sulphate), it is closed to stir evenly, stand 75 minutes；
2) closed organic solvent dissolving.Be added 2 times of bamboo vinegar mass fraction compounded organic solvent (120kg ethyl alcohol+
120kg methanol+120kg formic acid), it is closed to be sufficiently stirred dissolving；
3) it is separated by filtration.Filter residue is spare with filtrate；
4) alternating temperature distills.It is organic solvent that filtrate obtains distillate by 52 DEG C of 101 DEG C of distillations or vacuum distillation temperature,
After distillation completely, it is heated to 60 DEG C of 118 DEG C of distillations or vacuum distillation temperature, distillate obtains high-concentration bamboo vinegar, surplus materials
For bamboo tar；
5) recycling organic solvent is recycled.The organic solvent that techniqueflow 4 recycles, can recycle in techniqueflow
In 2；
6) inorganic salts drier water removal recycles.Filter residue (sal glauberi and cupric sulfate pentahydrate) in techniqueflow 3 adds
Heat removes the crystallization water, recycles in techniqueflow 1 to 258 DEG C.
Example 12
1) closed inorganic salts drying.The bamboo vinegar of 180kg is taken, drier (the anhydrous sulphur of 16kg anhydrous cupric sulfates+71kg is added
Sour sodium+63kg anhydrous magnesium sulfates), it is closed to stir evenly, stand 75 minutes；
2) closed organic solvent dissolving.4 times of compounded organic solvents of addition bamboo vinegar mass fraction (360kg ethyl acetate+
360kg dichloromethane), it is closed to be sufficiently stirred dissolving；
3) it is separated by filtration.Filter residue is spare with filtrate；
4) alternating temperature distills.It is organic solvent that filtrate obtains distillate by 40 DEG C of 77 DEG C of distillations or vacuum distillation temperature,
After distillation completely, it is heated to 60 DEG C of 118 DEG C of distillations or vacuum distillation temperature, distillate obtains high-concentration bamboo vinegar, surplus materials
For bamboo tar；
5) recycling organic solvent is recycled.The organic solvent that techniqueflow 4 recycles, can recycle in techniqueflow
In 2；
6) inorganic salts drier water removal recycles.Filter residue (sal glauberi and cupric sulfate pentahydrate) in techniqueflow 3 adds
Heat removes the crystallization water, recycles in techniqueflow 1 to 258 DEG C.
Illustrate the water removal effect of foregoing invention product below by way of experiment.
1. embodiment 1-12 bamboo vinegar moisture removals effect (95% fiducial range) of table
Table 1 statistics indicate that, embodiment 1-12 is to the moisture removal rate of the bamboo vinegar of different organic matter contents from 98.72-
99.78%, wherein embodiment 1-10 reach moisture removal rate and reach 99% or more, water of the embodiment 1-2 and 5-6 to bamboo vinegar
Divide removal rate to reach 99.5% or more, the ingredient of bamboo vinegar and bamboo tar can be not only analyzed directly as chromatographic sample, also may be used
For industrialized production high-concentration bamboo vinegar and bamboo tar, packing charge and 90% or more physical distribution expenses are reduced, you can reach market
Change and requires.
Claims (9)
1. a kind of method of bamboo vinegar water removal concentration and separating tar, it is characterised in that use following technical route, be specifically divided into
6 techniqueflows below：
1) closed inorganic salts drying.A certain amount of bamboo vinegar is taken, it is (a certain amount of to be specially that a certain amount of inorganic salts drier is added
Inorganic salts crystallize the bamboo vinegar that water quality is equal portions mass fraction), it is closed to stir evenly, stand a period of time.
2) closed organic solvent dissolving.Be added the organic solvent of 1-20 times of bamboo vinegar mass fraction, it is closed be sufficiently stirred after dissolve；
3) it is separated by filtration.Filter residue is spare with filtrate；
4) alternating temperature distills.After alternating temperature distills, 40-100 DEG C of 40-190 DEG C of vapo(u)rizing temperature or vacuum distillation temperature obtain filtrate
High-concentration bamboo vinegar and bamboo tar final products and organic solvent；
5) recycling organic solvent is recycled.The organic solvent that techniqueflow 4 recycles, can recycle in techniqueflow 2：
6) inorganic salts drier water removal recycles.Filter residue in techniqueflow 3 is heated to 100-260 DEG C, removes the crystallization water, repeatedly
Using in techniqueflow 1.
2. the method for a kind of bamboo vinegar water removal concentration according to claim 1 and separating tar, it is characterised in that described
The closed inorganic salts of techniqueflow 1 are dried, and the bamboo vinegar of 100 mass units is taken, and a kilograms of inorganic salts drier (a tools are added
Body is that inorganic salts crystallization water quality is 100 mass units), it is closed to stir evenly, stand 30-120 minutes.Inorganic salts drier
Specially：The one or more of anhydrous cupric sulfate, anhydrous calcium chloride, anhydrous magnesium sulfate, anhydrous sodium sulfate, dead plaster are mixed
It closes.
3. the method for a kind of bamboo vinegar water removal concentration according to claim 1 and separating tar, it is characterised in that described
The closed organic solvent of techniqueflow 2 dissolves, and is added the organic solvent of 1-20 times of bamboo vinegar mass fraction, it is closed be sufficiently stirred after
Dissolving, organic solvent specifically include：Ethyl alcohol, methanol, formic acid, acetic acid, ethyl acetate, dichloromethane, dimethyl sulfoxide (DMSO) (DMSO),
One or more kinds of double solvents of dimethylformamide (DMF).
4. the method for a kind of bamboo vinegar water removal concentration according to claim 1 and separating tar, it is characterised in that described
Techniqueflow 3 is separated by filtration, and solid is detached with liquid, it is spare with filtrate to obtain filter residue.
5. the method for a kind of bamboo vinegar water removal concentration according to claim 1 and separating tar, it is characterised in that described
The alternating temperature of techniqueflow 4 distills, and filtrate is after alternating temperature distills, 40-190 DEG C of vapo(u)rizing temperature or vacuum distillation temperature 40-100
DEG C, according to the difference for using organic solvent, first use low temperature distillation to collect one kind of organic solvent and high-concentration bamboo vinegar, then make
Another is collected with high temperature distillation, obtains high-concentration bamboo vinegar and bamboo tar final products and organic solvent.
6. the method for a kind of bamboo vinegar water removal concentration according to claim 1 and separating tar, it is characterised in that described
The recycling organic solvent of techniqueflow 5 is recycled, and is referred to the organic solvent of the recycling of techniqueflow 4, can be recycled in technology
In flow 2.
7. the method for a kind of bamboo vinegar water removal concentration according to claim 1 and separating tar, it is characterised in that described
The inorganic salts drier water removal of techniqueflow 6 recycles, and refers to that the filter residue in techniqueflow 3 is heated to 100-260 DEG C, removal knot
Brilliant water is recycled in techniqueflow 1.Optimum heating temperature is different according to the type for selecting drier.
8. the method for a kind of bamboo vinegar water removal concentration and separating tar according to claim 1-7, it is characterised in that described
6 techniqueflows be technological package circuit, 6 techniqueflows sequence is 123456 or 123645.
9. the method for a kind of bamboo vinegar water removal concentration and separating tar according to claim 1-8, it is characterised in that described
Technical route and method, be applied not only to industrial production high-concentration bamboo vinegar and bamboo tar final products, can be used for testing
The sample preparation of raw liquid of bamboo vinegar chromatography component analysis is analyzed in room, bamboo vinegar can also be produced as bamboo charcoal the environmental protection of waste
Processing.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810070673.2A CN108285803A (en) | 2018-01-18 | 2018-01-18 | A kind of method that bamboo vinegar removes water concentration and separating tar |
| CN201910027997.2A CN109609169B (en) | 2018-01-18 | 2019-01-11 | Method for dewatering, concentrating and separating tar from plant vinegar |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810070673.2A CN108285803A (en) | 2018-01-18 | 2018-01-18 | A kind of method that bamboo vinegar removes water concentration and separating tar |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108285803A true CN108285803A (en) | 2018-07-17 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111264302A (en) * | 2020-03-09 | 2020-06-12 | 中国林业科学研究院林产化学工业研究所 | Edible fungus growth promoter and preparation method and application thereof |
| CN113996078A (en) * | 2021-11-10 | 2022-02-01 | 浙江农林大学 | Simple processing method for concentrated natural organic acid by using biomass dry distillation acid as raw material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111264302A (en) * | 2020-03-09 | 2020-06-12 | 中国林业科学研究院林产化学工业研究所 | Edible fungus growth promoter and preparation method and application thereof |
| CN113996078A (en) * | 2021-11-10 | 2022-02-01 | 浙江农林大学 | Simple processing method for concentrated natural organic acid by using biomass dry distillation acid as raw material |
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Application publication date: 20180717 |