CN100497525C - Preparation process of refined bamboo vinegar liquid - Google Patents

Preparation process of refined bamboo vinegar liquid Download PDF

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Publication number
CN100497525C
CN100497525C CNB2006100537905A CN200610053790A CN100497525C CN 100497525 C CN100497525 C CN 100497525C CN B2006100537905 A CNB2006100537905 A CN B2006100537905A CN 200610053790 A CN200610053790 A CN 200610053790A CN 100497525 C CN100497525 C CN 100497525C
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China
Prior art keywords
bamboo vinegar
refined
bamboo
vinegar liquid
preparation technology
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Expired - Fee Related
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CNB2006100537905A
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Chinese (zh)
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CN1931960A (en
Inventor
涂志龙
叶永胜
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Suichang Biyan Bamboo Charcoal Co., Ltd.
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TU ZHILONG YE YONGSHENG
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    • 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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  • Treatment Of Liquids With Adsorbents In General (AREA)

Abstract

The present invention relates to bamboo pyrolysis technology, and is especially process of refining bamboo vinegar liquid as the liquid product of bamboo carbonizing process. The purifying process includes the following steps: 1. adding active carbon or bamboo charcoal in 1-2 wt% into crude bamboo vinegar liquid, heating while stirring for 3-4, stilling and filtering to eliminate dregs; 2. purifying the filtrate in ion exchange resin column to obtain refined bamboo vinegar liquid; and 3. storing the refined bamboo vinegar liquid in lightproof tank. The process of the present invention is simple, time saving, low in power consumption and low in cost, and the refined bamboo vinegar liquid has less organic acid loss, low tar content and no smoky smell.

Description

A kind of preparation technology of refined bamboo vinegar
Technical field
The present invention relates to the bamboo wood pyrolysis art, is the method for the product liquid bamboo vinegar liquid purification that produces in the dry distillation charring process about bamboo.
Background technology
Bamboo vinegar liquid is a byproduct of firing bamboo charcoal, is a kind of volatile, dark red brown water soluble mixt that the bamboo wood pyrolytic process produces, is to collect by the emission gases cooling when firing bamboo charcoal to form.Its main component is nearly 300 kinds of materials such as water, organic acid, alcohols, ketone and phenols, can be used as the basic raw material of chemical industry refinement and organic synthesis.
Bamboo vinegar after refining can be used as food spice, fumigant, can be used as sanitas, antiseptic-germicide, insect-proof agent again, or is used for beauty treatment, treatment acne and beriberi.The process for purification of bamboo vinegar liquid generally has following 3 kinds of treatment processs: 1, standing separation method (directly settled process, add the settled process of medicine), standing separation method are simple to operate, and cost is low, but separating effect is not good, and required time is longer.2, distillation method: the boiling point that utilizes each composition in the bamboo vinegar stoste is different and carry out isolating a kind of method, and 2 kinds of simple distillation (atmospheric distillation) and distillation under vacuum are often arranged.Simple distillation can only be used for the rough segmentation mixture, though simple to operate, energy consumption is big; The distillation under vacuum separation degree is high slightly, but investment is big, complicated operation, and energy consumption is also big, and the loss of total organic acids amount is also high.3, combined techniques: be about to a kind of method of purification that above-mentioned two kinds of methods combine and propose as patent application 02136544, elder generation's simple distillation is left standstill and is deposited some months, can cause the production time to prolong like this, production efficiency reduces, and the discoloring agent S-WAT that adds belongs to the chemical ingredients that is limited by strictness in medicine and food index.Patent 200310116218.6 has proposed a kind of process for purification, adding 0.1%~20% superoxol before distillation leaves standstill, be easy to cause the content overproof of hydrogen peroxide in refined bamboo vinegar like this, thereby limited its application in medicine, field of food.And the bamboo tar content of the bamboo vinegar liquid that above-mentioned these method for purification make is still very high, has one strong tangy flavour, has influenced the quality of product greatly.
Summary of the invention
The objective of the invention is to, at time-consuming, the problem such as energy consumption big, the total organic acids loss is high, sootiness is highly seasoned that exist in the existing method for purification, a kind of preparation technology of refined bamboo vinegar is provided, adopt ion exchange resin, can be easy, save time, energy consumption is low, with low cost produce that the total organic acids loss is low, tar content is low, the refined bamboo vinegar of smokeless smoke flavour.
The objective of the invention is to be achieved by following proposal.
A kind of preparation technology of refined bamboo vinegar comprises the steps:
1, adds in bamboo vinegar stoste that to account for bamboo vinegar stoste weight percent be 1%~2% gac or bamboo charcoal, heat to stir after 3~4 hours and leave standstill, filter, remove residue;
The bamboo vinegar liquid supernatant liquor that 2, will obtain is after filtration crossed the new resin column of handling that ion exchange resin is housed, and after the purified separation, gained liquid is refined bamboo vinegar;
3, the refined bamboo vinegar that makes being put into immediately the good finished product jar of opacifying property (for example black, brown jar) stores.
Gac in the described step 1 or bamboo charcoal contain the fine duct greater than 1.6 nanometers, 80% aperture at least.
Heating in the described step 1 is that temperature is risen to 50 ℃~60 ℃.
Filtration in the described step 1 is to adopt plate-and-frame filter press to carry out filter operation.
As an alternative, the filtration in the described step 1 is to adopt whizzer to carry out filter operation.
Ion exchange resin in the described step 2 is macroporous adsorbent resin.
As an alternative, the ion exchange resin in the described step 2 is ion exchange resin.
The invention has the beneficial effects as follows:
1, the refined bamboo vinegar that makes of the present invention, wherein particularly acetic acid content is very high for the total organic acids that the bamboo vinegar liquid effect is played a decisive role, and analyzes after testing to be 76% of organism total content in the bamboo vinegar liquid; Compare with raw liquid of bamboo vinegar in extractive process, total organic acids loses seldom, only loses 2%, then loses 30%~40% in the traditional technology;
2, bamboo tar content harmful in the refined bamboo vinegar that makes is low;
3, filter the refined bamboo vinegar that makes through ion exchange resin and removed tangy flavour;
4, the refined bamboo vinegar that makes is as clear as crystal, makes its color and luster with natural botanical extraction liquid and characteristic, is easy to be accepted by people;
5, preparation technology of the present invention save that cost, energy consumption are low, environmental protection, save time, equipment is simple, throughput is high.The present invention adopts gac or bamboo charcoal and ion exchange resin that bamboo vinegar stoste is handled, and gac or bamboo charcoal are with low cost, and gac after handling well or bamboo charcoal and ion exchange resin can pass through the regeneration step restorability, and cost has been saved in recycling; Preparation process need not to expend the too much energy, and can not produce the pollution to environment; Used equipment is simple, and several hrs can make refined bamboo vinegar, is applicable to large-scale commercial production.
Embodiment
The invention will be further described below in conjunction with embodiment, but therefore do not limit the present invention among the described scope of embodiments.
Embodiment 1 (preparation method one of refined bamboo vinegar)
1, add in bamboo vinegar stoste that to account for bamboo vinegar stoste weight percent be 1%~2% gac or bamboo charcoal, heat to 50 ℃~60 ℃, stirs and leave standstill a few hours after 3~4 hours, the employing plate-and-frame filter press filters, and removes residue;
The bamboo vinegar liquid supernatant liquor that 2, will obtain is after filtration crossed the new D101 macroporous adsorptive resins of handling, and after purification with macroreticular resin separated, the gained weak yellow liquid was refined bamboo vinegar;
3, the refined bamboo vinegar that makes being put into immediately the good finished product jar of opacifying property (for example black, brown jar) stores.
Wherein gac or bamboo charcoal are selected for use and are contained 80% aperture gac or the bamboo charcoal greater than the fine duct of 1.6 nanometers at least, help next step separation and purification.
Embodiment 2 (preparation method two of refined bamboo vinegar)
1, add in bamboo vinegar stoste that to account for bamboo vinegar stoste weight percent be 1%~2% gac or bamboo charcoal, heat to 50 ℃~60 ℃, stirs and leave standstill a few hours after 3~4 hours, the employing whizzer carries out centrifuging, removes residue;
The bamboo vinegar liquid supernatant liquor that 2, will obtain is after filtration crossed the new ion exchange resin column of handling (wherein ion exchange resin is that D208 is resin dedicated) after ion-exchange resin purification separates, and the gained weak yellow liquid is refined bamboo vinegar;
3, the refined bamboo vinegar that makes being put into immediately the good finished product jar of opacifying property (for example black, brown jar) stores.
Wherein gac or bamboo charcoal are selected for use and are contained 80% aperture gac or the bamboo charcoal greater than the fine duct of 1.6 nanometers at least, help next step separation and purification.
Because gac or bamboo charcoal have superpower adsorption function, can remove the most of tangy flavour in the bamboo vinegar stoste, and can adsorb toxic heavy metal unnecessary in the bamboo vinegar stoste and impurity, and bamboo vinegar stoste is purified.Macroporous adsorbent resin or ion exchange resin can adsorb some main components of tangy flavour in the bamboo vinegar stoste, bamboo vinegar stoste are heard up almost do not allow the unconformable pungent tangy flavour of people.This method is simple to operate, is suitable for industrial production.During industrial production, the model of resin column and scale can select determine according to practical situation, and the content of the bamboo vinegar stoste that the content of polymer polymeric adsorbent can need be purified according to reality adds, and weight is about 20% of bamboo vinegar stoste weight.
Prepared refined bamboo vinegar can be used for medical treatment, diet, beauty treatment aspect, especially is applied to sterilization and disinfection, and as the additive of beverage, food, aspects such as beauty and skin care can be diluted to different concentration preparation or interpolation according to the difference of purposes during use.
Test example 1 (the dissolved tar content detection of refined bamboo vinegar)
The refined bamboo vinegar that the present invention makes is put into furnace pot, obtain black residue with the fire burns heating, residue is weighed, the ratio that calculates its weight and former bamboo vinegar liquid weight is bamboo vinegar liquid dissolved tar content, numerical value is less than 3% explanation bamboo vinegar liquid quality better, purity height.The present invention makes refined bamboo vinegar burning gained black residue and cannot see substantially through visual inspection, therefore, can determine that tar content is very low.
Test example 2 (organic content of refined bamboo vinegar detects)
Refined bamboo vinegar with the present invention makes adopts gas-chromatography---GC-MS through Zhejiang University
(GC-MS) check and analysis, in 176 kinds of organism being tested, main organic content is as follows:
1, organic acid 83% (wherein acetate 76%);
2, phenols 2%;
3, ketone 2.5%;
4, aldehydes 1.5%;
5, alcohols 6%;
6, the ester class 2%;
7, other 3%.
The composition of tangy flavour is very complicated, often form by tens kinds even hundreds of kind material, mainly contain this a few class materials as tar, phenols, alcohols, carbonyl compound, hydro carbons, the content of these materials reduces greatly in the prepared refined bamboo vinegar of the present invention, so tangy flavour produces seldom naturally.
Test example 3 (contrast experiment of refined bamboo vinegar and stoste production technique)
Method The total organic acids yield Tar content Color and luster Energy consumption Burnt smoke Equipment and technology Throughput
The tradition distillation method 60~70% Few Yellowish High Very big Complicated Low
The inventive method 98% Seldom Yellowish Very low Seldom Simply High

Claims (5)

1. the preparation technology of a refined bamboo vinegar is characterized in that comprising the steps:
1. add in bamboo vinegar stoste that to account for bamboo vinegar stoste weight percent be 1%~2% gac or bamboo charcoal, heat to stir after 3~4 hours and leave standstill, filter, remove residue;
The bamboo vinegar liquid supernatant liquor that 2. will obtain is after filtration crossed the new resin column of handling that ion exchange resin or macroporous adsorbent resin are housed, and after the purified separation, gained liquid is refined bamboo vinegar;
3. the refined bamboo vinegar that makes being put into immediately the good finished product jar of opacifying property stores.
2. the preparation technology of a kind of refined bamboo vinegar according to claim 1 is characterized in that: gac or the bamboo charcoal of described step in 1. contains the fine duct greater than 1.6 nanometers, 80% aperture at least.
3. the preparation technology of a kind of refined bamboo vinegar according to claim 1 is characterized in that: described step heating in 1. is that temperature is risen to 50 ℃~60 ℃.
4. the preparation technology of a kind of refined bamboo vinegar according to claim 1 is characterized in that: the filtration of described step in 1. is to adopt plate-and-frame filter press to carry out filter operation.
5. the preparation technology of a kind of refined bamboo vinegar according to claim 1 is characterized in that: the filtration of described step in 1. is to adopt whizzer to carry out filter operation.
CNB2006100537905A 2006-10-11 2006-10-11 Preparation process of refined bamboo vinegar liquid Expired - Fee Related CN100497525C (en)

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Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
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CN100497525C true CN100497525C (en) 2009-06-10

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Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101185527B (en) * 2007-08-03 2011-05-11 浙江省林业科学研究院 Anti-oxidant containing wood and bamboo vinegar liquid extract and preparing method and application thereof
CN101696378B (en) * 2009-11-02 2014-09-03 涂志龙 Bamboo charcoal wine yeasts, bamboo charcoal wine and preparation method thereof
CN101935537A (en) * 2010-08-31 2011-01-05 中国科学院上海生命科学研究院湖州现代农业生物技术产业创新中心 High-concentration bamboo vinegar and preparation method thereof
CN102008071B (en) * 2010-10-07 2013-03-20 吴子平 Fresh bamboo juice extraction process
CN102021012B (en) * 2010-12-15 2013-09-11 安徽省石台县牯牛降竹炭制品有限责任公司 Preparation method of bamboo vinegar
CN103893216B (en) * 2014-03-13 2016-09-28 沈阳化工大学 A kind of extracting and developing method of antioxidant composition in rough wood vinegar
CN104164248A (en) * 2014-08-28 2014-11-26 桂林市艾康科技有限公司 Preparation method of refined bamboo vinegar
CN106497592A (en) * 2016-11-28 2017-03-15 茂名市浩源环保科技有限公司 A kind of industrial preparation method of bamboo vinegar
CN107129822A (en) * 2017-06-20 2017-09-05 博莱维(厦门)生物科技有限公司 A kind of preparation method of refined bamboo vinegar
CN108841408A (en) * 2018-06-11 2018-11-20 张金辉 A kind of crude wood vinegar removing impurities process for upgrading and application thereof
CN108728148A (en) * 2018-06-11 2018-11-02 吉林农业大学 The production technology and application method of wood vinegar
CN108893129A (en) * 2018-09-04 2018-11-27 蔡信弟 Coproduction prepares the production method and equipment of bamboo charcoal and bamboo vinegar
CN109158092A (en) * 2018-10-11 2019-01-08 成都其其小数科技有限公司 A kind of multifunctional air cleaning agent and preparation method

Non-Patent Citations (2)

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用竹炭精制竹醋液的研究. 翁益明,王伟龙,张文标,洪游游.竹子研究汇刊,第24卷第2期. 2005
用竹炭精制竹醋液的研究. 翁益明,王伟龙,张文标,洪游游.竹子研究汇刊,第24卷第2期. 2005 *

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Owner name: SUICHANG BIYAN BAMBOO CHARCOAL CO., LTD.

Free format text: FORMER OWNER: TU ZHILONG

Effective date: 20111031

Free format text: FORMER OWNER: YE YONGSHENG

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Effective date of registration: 20111031

Address after: 323300 Zhejiang Lishui Suichang County High Town Industrial Zone, Suichang River Miao

Patentee after: Suichang Biyan Bamboo Charcoal Co., Ltd.

Address before: 323300 No. 276, West Street, Suichang County, Zhejiang

Co-patentee before: Ye Yongsheng

Patentee before: Tu Zhilong

CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20090610

Termination date: 20161011