CN107880922A - One kind is without phenol bamboo vinegar and preparation method thereof - Google Patents

One kind is without phenol bamboo vinegar and preparation method thereof Download PDF

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Publication number
CN107880922A
CN107880922A CN201711189566.3A CN201711189566A CN107880922A CN 107880922 A CN107880922 A CN 107880922A CN 201711189566 A CN201711189566 A CN 201711189566A CN 107880922 A CN107880922 A CN 107880922A
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China
Prior art keywords
bamboo
vinegar
phenol
charcoal
bamboo vinegar
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CN201711189566.3A
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Chinese (zh)
Inventor
操铖
高煜
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Huayi Pharmaceutical Anhui Co Ltd
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Huayi Pharmaceutical Anhui Co Ltd
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Priority to CN201711189566.3A priority Critical patent/CN107880922A/en
Publication of CN107880922A publication Critical patent/CN107880922A/en
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10CWORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
    • C10C5/00Production of pyroligneous acid distillation of wood, dry distillation of organic waste
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10BDESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B53/00Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
    • C10B53/02Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10BDESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B57/00Other carbonising or coking processes; Features of destructive distillation processes in general
    • C10B57/08Non-mechanical pretreatment of the charge, e.g. desulfurization
    • C10B57/10Drying
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00Technologies for the production of fuel of non-fossil origin
    • Y02E50/10Biofuels, e.g. bio-diesel

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Coke Industry (AREA)

Abstract

The invention discloses one kind without phenol bamboo vinegar and preparation method thereof, bamboo-vinegar includes phenol, and phenol is in yellowish-brown in acidic liquid, is the harmful substance for forbidding picking in China's food, medicine, cosmetics, articles for washing.The country is due to bamboo vinegar purification technique backwardness at present, and bamboo vinegar liquid product is in brown color or bronzing, and phenol content severe overweight, this just constrains application of the bamboo vinegar in fields such as food, medicine, cosmetics, articless for washing.The present invention uses pure physical purification method, succeeds in developing a kind of colourless, transparent, smoke smell free, avirulent no phenol bamboo vinegar.Bamboo charcoal bamboo vinegar industry authoritative sources unanimously thinks:Comprehensive replacement is currently used in the coloured bamboo vinegar in the fields such as food, medicine, cosmetics, articles for washing without phenol bamboo vinegar.This method preparation method is simple to operate, relatively low without special installation, short preparation period, cost.

Description

One kind is without phenol bamboo vinegar and preparation method thereof
Technical field
The invention belongs to pharmaceutical synthesis field, and in particular to one kind is without phenol bamboo vinegar and preparation method thereof.
Background technology
Bamboo vinegar is the product liquid that bamboo wood is pyrolyzed to obtain, and it is a kind of considerably complicated liquid mixture of constituent, Its main component is the materials such as water, organic acid, phenols, ketone, alcohols, and its forming process is very complicated.Bamboo vinegar output of fluid then with The species of bamboo wood, the moisture content of bamboo wood and pyrolytic process it is different and different, its composition is more with collection method, pyrolysis temperature, storage Deposit the different of condition etc. and constantly change.
Bamboo vinegar has many functions, and its tissue to plant and animal has good permeability and absorbability, to domestic animal Excrement and garbage stench also have eliminate effect.In terms of bamboo vinegar can also play a part of plant hormone, give Crop adds micro bamboo vinegar, then can play and promote plant establishment, germination, growth, the effect for making the taste of fruit improve. In a word, it can be widely applied to each fields such as agricultural, medical treatment, health care.
Japan is bamboo vinegar liquid research in the world, application level highest country.Bamboo jealous woman fertilizer is carried out in organic agriculture production The production of material, character analysis and experiment to agriculture and forestry production etc., it has also become it is indispensable natural to be engaged in no agricultural chemicals cultivation The organic agriculture means of production of plant source.There are a large amount of uses in prevention and preventing and treating bird flu, aftosa etc., obtain preferable Effect.Particularly in recent years, the mechanism for exploring bamboo jealous woman as synergist synergy in Chinese medicine Chinese prescription is increased, has delivered and has been permitted It is more to prevent the application example and paper of " three high ", gout etc. about bamboo jealous woman.
South Korea is research, the up-and-coming youngster using bamboo vinegar liquid.It is mainly used in preventing and treating pest and disease damage, subtracts agricultural chemicals, improves soil Environment, reduce secondary pollution etc..There are a large amount of uses in bird flu, aftosa etc. prevention and preventing and treating, obtain preferable Effect.In recent years, accelerate bamboo jealous woman to apply in beverage, food, medicine, daily use chemicals etc., make great progress, exist at present The status being in a leading position in the world.The product of bamboo vinegar drug type, the country there is no report.
The production method of bamboo vinegar has 3 kinds:One kind is the direct firing process of earth kiln, and equipment cost is low, to bamboo charcoal, bamboo after improvement The quality and the rate of recovery of vinegar liquid all increase;It is retort pyrolysismethod in second, point fixed destructive distillation and moving bed are continuously done Two classes are evaporated, waste gas caused by some type of furnaces and technique can be used as fuel, and bamboo vinegar quality and yield are better than the former;The third is Method is prepared with special equipment, the type of furnace is small, can be to the accurate control of links.
The content of the invention
The purpose of the present invention is precisely in order to solve each manufacturer's raw material sources of tradition, production equipment, technology etc. no Together, product quality is uneven, and some also infiltrates the pyrolkigneous liquid composition such as wood tar, into a kind of mixed type bamboo vinegar, shadow Ring its application field.In order to improve and stablize the quality of bamboo vinegar, it is ensured that it is safe to use, expand application field, this research from Bamboo vinegar raw materials for production, production equipment, collection process, storage method and process for purification etc. are explored, and make every effort to acquisition one The production of kind high-purity bamboo vinegar and processing technology.
The invention provides one kind without phenol bamboo vinegar and preparation method thereof, 5~6 tons of fresh feed is taken to be obtained through initial gross separation To 1 ton of bamboo charcoal and 300~600kg bamboo vinegar, general bamboo vinegar is divided into three classes according to temperature is collected:It is low temperature less than 90 DEG C Bamboo vinegar, the medium temperature bamboo vinegar for being, it is high temperature bamboo vinegar higher than 120 DEG C between 90~120 DEG C.The first bamboo vinegar obtained is palm fibre Color, after standing, upper strata is clarification bamboo vinegar, and lower sediment be bamboo tar, then clarified solution substep is refined.Initial gross separation frequently with Settled process, organic solvent extractionprocess, conventional bamboo charcoal is further refined, Activated Carbon Adsorption Separation, reuses distillation, rectification process carries It is pure.
As preferred means, preparation method comprises the following steps:1) the crooked termination precision pulling that will be formed when felling bamboo Bench saw is clipped, and using port as locating surface, raw bamboo is cut into fixed length thick bamboo tube, broken thick bamboo tube with broken bamboo machine, then will be cut with slicer It is 1-4mm into thickness, a width of 10-25mm bamboo chip, while remove that bamboo is blue or green and tabasheer, bamboo green grass or young crops thickness are processed in 1-3mm Bamboo scraps caused by process;2) bamboo charcoal is dry, bamboo wood carbonizes in advance, bamboo wood carbonized, bamboo charcoal are calcined and five stages of cooling;3) using quiet Put method, organic solvent extractionprocess carries out initial gross separation to bamboo-vinegar;4) simple distillation:Mixture to be separated is loaded into distillation In kettle, heating and part are evaporated.The steam released by distillation still is imported in condenser, due to cooling effect steam within the condenser It is changed into liquid, the distillate of generation flows into collector.5) rectification and purification:Utilize the steam generated in distillation equipment and previously steaming The steam gone out, partial condensation obtain phegma, remove phenol with charcoal absorption, that is, obtain no phenol bamboo vinegar liquid product.
As further preferred means, the concrete technology of the step 2) is:
Bamboo wood is dried:Fumigation drying is carried out using red-hot flue gas caused by fuel combustion, typically needs one week or so time.This When, the temperature in charcoal kiln is generally less than 150 DEG C, mainly removes the moisture in bamboo wood, makes the geomery of bamboo wood be not easy to change Become.If the drying of bamboo wood is separately carried out, it is necessary to separately build bamboo wood smoke kiln with the process made charcoal.
Bamboo wood carbonizes in advance:At this moment 150 DEG C~270 DEG C of the temperature in charcoal kiln, bamboo wood by thermally decompose it is obvious, start to produce Raw acetic acid and tar.
Bamboo wood carbonized:Very fast thermal decomposition occurs at this moment 270 DEG C~360 DEG C of the temperature in charcoal kiln, bamboo wood, produces a large amount of Catabolite, be the natural polymer product such as acetic acid, tar Main Stage.Within this stage, because bamboo wood is very fast Thermal decomposition, release substantial amounts of heat.
Bamboo charcoal is calcined:At this moment more than 360 DEG C of the temperature in charcoal kiln.In this stage, with the lasting progress of high temperature, residual The exclusion that the material that can be volatilized in bamboo charcoal obtains, but caused gas-condensate liquid --- bamboo vinegar is seldom.
Embodiment
Embodiment 1
One kind comprises the following steps without phenol bamboo vinegar and preparation method thereof:
1) the crooked termination formed when felling bamboo is clipped with precision pulling bench saw, using port as locating surface, raw bamboo be cut into Fixed length thick bamboo tube, thick bamboo tube is broken with broken bamboo machine, then it is 1-4mm that will be cut into thickness with slicer, a width of 10-25mm bamboo chip, together When remove that bamboo is blue or green and tabasheer, bamboo green grass or young crops thickness obtain bamboo scraps caused by process in 1-3mm;
2) bamboo charcoal is dry, bamboo wood carbonizes in advance, bamboo wood carbonized, bamboo charcoal are calcined and five stages of cooling;
Bamboo wood is dried:Fumigation drying is carried out using red-hot flue gas caused by fuel combustion, typically needs one week or so time.This When, the temperature in charcoal kiln is generally less than 150 DEG C, mainly removes the moisture in bamboo wood, makes the geomery of bamboo wood be not easy to change Become.If the drying of bamboo wood is separately carried out, it is necessary to separately build bamboo wood smoke kiln with the process made charcoal.
Bamboo wood carbonizes in advance:At this moment 150 DEG C of the temperature in charcoal kiln, bamboo wood by thermally decompose it is obvious, start produce acetic acid And tar.
Bamboo wood carbonized:Very fast thermal decomposition occurs at this moment 270 DEG C of the temperature in charcoal kiln, bamboo wood, produces substantial amounts of decompose Product, it is the Main Stage of the natural polymer product such as acetic acid, tar.Within this stage, due to bamboo wood very fast heat point Solution, releases substantial amounts of heat.
Bamboo charcoal is calcined:At this moment more than 360 DEG C of the temperature in charcoal kiln.In this stage, with the lasting progress of high temperature, residual The exclusion that the material that can be volatilized in bamboo charcoal obtains, but caused gas-condensate liquid --- bamboo vinegar is seldom.
3) initial gross separation is carried out to bamboo-vinegar using settled process, organic solvent extractionprocess;
4) simple distillation:Mixture to be separated is loaded in distillation still, heating and part are evaporated.Released by distillation still Steam is imported in condenser, and because cooling effect steam is changed into liquid within the condenser, the distillate of generation flows into collector;
5) rectification and purification:Using the steam generated in distillation equipment and the steam previously steamed, partial condensation is flowed back Liquid, phenol is removed with charcoal absorption, that is, obtains no phenol bamboo vinegar liquid product.
Using made from the method without phenol bamboo vinegar physical and chemical index:
First, proportion:1.010g/ml;pH:3.0;
2nd, form:Water white transparency;Smoke smell free, stable performance;See that light, long-term storage are non-discolouring.
Without phenol bamboo vinegar component:Survey is picked up through Shanghai Chinese Medicine Creation Research Center's mass spectrograph, no phenol bamboo vinegar component is as follows:Second Acid 88.341%;Propionic acid 2.391%;Butyric acid 0.177%;Formic acid 0.370%;The grade composition of butyrolactone 0.852;It is burnt that dissolving is not picked Oil, phenol, formaldehyde.
Without phenol bamboo vinegar toxicity:Picked up through Zhejiang Center for Disease Control 200701207# and observe and predict announcement:Without phenol bamboo vinegar.
Tested material chmice acute LD50 of passing through mouth is more than 10g/kg body weight, according to acute toxicity grading criteria, its chmice acute Oral toxicity belongs to actual nontoxic level.
The present invention is using settled process, organic solvent extractionprocess initial gross separation bamboo-vinegar, with bamboo charcoal, charcoal absorption point From, reuse distillation, rectification process purification, be further refining to obtain natural high-quality without phenol bamboo vinegar.The preparation method operates Simply, it is relatively low without special installation, short preparation period, cost.
The description to embodiment the invention is not restricted to more than, those skilled in the art according to disclosure of the present invention, The creative work improvement and modification that be carried out need not be passed through on the basis of the present invention, all should protection scope of the present invention it It is interior.

Claims (3)

1. one kind is without phenol bamboo vinegar and preparation method thereof, it is characterised in that takes 5~6 tons of fresh feed to obtain 1 through initial gross separation The bamboo vinegar of ton bamboo charcoal and 300~600kg, general bamboo vinegar are divided into three classes according to temperature is collected:It is low temperature bamboo less than 90 DEG C Vinegar liquid, the medium temperature bamboo vinegar for being, it is high temperature bamboo vinegar higher than 120 DEG C between 90~120 DEG C.The first bamboo vinegar obtained is palm fibre Color, after standing, upper strata is clarification bamboo vinegar, and lower sediment be bamboo tar, then clarified solution substep is refined.Initial gross separation frequently with Settled process, organic solvent extractionprocess, conventional bamboo charcoal is further refined, Activated Carbon Adsorption Separation, reuses distillation, rectification process carries It is pure.
2. it is according to claim 1 one kind without phenol bamboo vinegar and preparation method thereof, it is characterised in that preparation method include with Lower step:1) the crooked termination formed when felling bamboo is clipped with precision pulling bench saw, using port as locating surface, it is fixed that raw bamboo is cut into Long thick bamboo tube, thick bamboo tube is broken with broken bamboo machine, then it is 1-4mm that will be cut into thickness with slicer, a width of 10-25mm bamboo chip, simultaneously Remove bamboo green grass or young crops and tabasheer, bamboo green grass or young crops thickness obtain bamboo scraps caused by process in 1-3mm;2) bamboo charcoal is dry, the pre- charcoal of bamboo wood Change, bamboo wood carbonized, bamboo charcoal calcination and five stages of cooling;3) bamboo-vinegar is carried out using settled process, organic solvent extractionprocess Initial gross separation;4) simple distillation:Mixture to be separated is loaded in distillation still, heating and part are evaporated;Released by distillation still Steam import in condenser, because cooling effect steam is changed into liquid within the condenser, the distillate of generation, which flows into, to be collected Device.5) rectification and purification:Using the steam generated in distillation equipment and the steam previously steamed, partial condensation obtains phegma, uses Charcoal absorption removes phenol, that is, obtains no phenol bamboo vinegar liquid product.
3. one kind according to claim 2 is without phenol bamboo vinegar and preparation method thereof, it is characterised in that the tool of the step 2) Body technology is:
Bamboo wood is dried:Fumigation drying is carried out using red-hot flue gas caused by fuel combustion, typically needs one week or so time.At this moment, Temperature in charcoal kiln is generally less than 150 DEG C, mainly removes the moisture in bamboo wood, the geomery of bamboo wood is not allowed malleable. If the drying of bamboo wood is separately carried out, it is necessary to separately build bamboo wood smoke kiln with the process made charcoal;
Bamboo wood carbonizes in advance:At this moment 150 DEG C~270 DEG C of the temperature in charcoal kiln, bamboo wood by thermally decompose it is obvious, start produce vinegar Acid and tar;
Bamboo wood carbonized:Very fast thermal decomposition occurs at this moment 270 DEG C~360 DEG C of the temperature in charcoal kiln, bamboo wood, produces substantial amounts of point Product is solved, is the Main Stage of the natural polymer product such as acetic acid, tar.Within this stage, due to the very fast heat of bamboo wood Decompose, release substantial amounts of heat;
Bamboo charcoal is calcined:At this moment more than 360 DEG C of the temperature in charcoal kiln.In this stage, with the lasting progress of high temperature, bamboo is remained in The exclusion that the material that can be volatilized in charcoal obtains, but caused gas-condensate liquid --- bamboo vinegar is seldom.
CN201711189566.3A 2017-11-24 2017-11-24 One kind is without phenol bamboo vinegar and preparation method thereof Pending CN107880922A (en)

Priority Applications (1)

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Application Number Priority Date Filing Date Title
CN201711189566.3A CN107880922A (en) 2017-11-24 2017-11-24 One kind is without phenol bamboo vinegar and preparation method thereof

Publications (1)

Publication Number Publication Date
CN107880922A true CN107880922A (en) 2018-04-06

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108888995A (en) * 2018-06-25 2018-11-27 浙江农林大学 A kind of method of bamboo vinegar orientation extracting
CN113975212A (en) * 2021-11-10 2022-01-28 浙江御风新材料科技有限公司 Processing method for removing harmful substances in bamboo wood vinegar liquid and wet tissue liquid and mouthwash prepared by processing method
CN114933913A (en) * 2022-05-09 2022-08-23 湘潭大学 Preparation method of refined bamboo vinegar

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108888995A (en) * 2018-06-25 2018-11-27 浙江农林大学 A kind of method of bamboo vinegar orientation extracting
CN108888995B (en) * 2018-06-25 2021-02-12 浙江农林大学 Bamboo vinegar directional extraction method
CN113975212A (en) * 2021-11-10 2022-01-28 浙江御风新材料科技有限公司 Processing method for removing harmful substances in bamboo wood vinegar liquid and wet tissue liquid and mouthwash prepared by processing method
CN113975212B (en) * 2021-11-10 2023-12-12 浙江银帆生物科技有限公司 Processing method for removing harmful substances in bamboo-wood vinegar, wet tissue liquid and mouthwash prepared by processing method
CN114933913A (en) * 2022-05-09 2022-08-23 湘潭大学 Preparation method of refined bamboo vinegar
CN114933913B (en) * 2022-05-09 2023-05-05 湘潭大学 Preparation method of refined bamboo vinegar

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Application publication date: 20180406

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