CN103882160A - Method for purifying Valonia tannin extract - Google Patents
Method for purifying Valonia tannin extract Download PDFInfo
- Publication number
- CN103882160A CN103882160A CN201410138042.1A CN201410138042A CN103882160A CN 103882160 A CN103882160 A CN 103882160A CN 201410138042 A CN201410138042 A CN 201410138042A CN 103882160 A CN103882160 A CN 103882160A
- Authority
- CN
- China
- Prior art keywords
- solution
- valonex
- add
- dry
- acetone
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Extraction Or Liquid Replacement (AREA)
- Compounds Of Unknown Constitution (AREA)
Abstract
The invention discloses a method for purifying Valonia tannin extract. The method adopts Valonia or Valonia tannin extract as a main raw material, and comprises the following main process routes of adding water in the Valonia and heating for extraction or adding water in the Valonia tannin extract and heating to dissolve the Valonia tannin extract, flocculating and settling by using a chemical reagent polyacrylamide, treating by using an organic solvent (performing the treatment on acetone solutions with low concentration and high concentration in two times), passing through a chromatography column and drying, thereby obtaining a finished product. By adopting the method, such impurities as non tannin in the Valonia tannin extract can be effectively removed, the tannin content of the obtained purified finished product of Valonia tannin extract is high than 80% and the yield is higher than 80% as well.
Description
Technical field
The invention belongs to valonex deep process technology field, relate in particular to a kind of purification process of valonex.
Background technology
Rubber Bowl is that the kind of oak class fruit shell claims, it is rich in tannin, as the wild tanning plant of one, is distributed widely in China most areas.Valonex obtains taking rubber Bowl as raw material production exactly, and rubber Bowl can gather use every year, does not affect growth and the use of trees, and output is large, aboundresources is renewable, for a long time the main tannin extract raw material of Dou Shi China.The contained tannin of valonex belongs to hydrolysable tannins, mainly be made up of castalagin, the Tian Li peaceful acid of florigen, the peaceful acid of chestnut Bowl, sweet chestnut Bowl, rubber Bowl tan florigen acid and the sweet Li Su etc. of florigen acid, different rubber Bowl that tan that tan, non-tannis is containing Flavonol, gallic acid and carbohydrate etc.Valonex is mainly used in the ore floatation agent of Wet-type oxidation sweetening agent, Anticrustator for descaling boiler, metallurgical industry of leather retanning agent, industrial sulfurous gas and inhibitor, oil and gas well drilling slurry thinner, ceramic industry dispergator, metal antirusting agent, waste water flocculant etc.
Although valonex is of many uses, because of the character of itself, be all subject to certain limitation at many-sided consumption, cause the output of valonex to be a greater impact, more rubber Bowl resource is still underutilized.As aspect leather tanning, because valonex color is dark, seepage velocity is slow, leather color and luster that tanning goes out is dark, plate firmly, not water-fastness etc., be only suitable for tanning heavy leather; Aspect ore floatation, in the time extracting some rare noble metals, because valonex tannin content only has 66%-70%, than Chinese gallotanninic acid tannin content, 78%-81% is low, so have certain influence in extraction yield and purity especially.Therefore, improve valonex tannin content and be market in the urgent need to, be the important channel of improving the demand of market to valonex.
Summary of the invention
The technical problem to be solved in the present invention is to provide the purification process of the valonex that a kind of tannin content is higher.
For solving the problems of the technologies described above, the present invention by the following technical solutions: the purification process of valonex, in rubber Bowl vat liquor or the valonex aqueous solution, add chemical reagent polyacrylamide, make the impurity flocculation sediments such as part non-tannis and remove; In solution, add organic solvent-acetone again, remove and be insoluble to the impurity such as the part non-tannis of organic solvent-acetone; Subsequently solution is analysed to post by resinbed, the further impurity such as remove portion non-tannis, gained solution is after drying and get final product.
Add organic solvent-acetone to process totally twice, add for the first time the acetone soln of mass concentration 60%, add for the second time the acetone soln of mass concentration 85%.
The purification process of above-mentioned valonex, in comprising the following steps:
<1> rubber Bowl heating lixiviate or the valonex heating for dissolving that adds water that adds water
Rubber Bowl raw material is added water at 60-90 DEG C through extracted many times, and vat liquor merges; Or be made into the valonex aqueous solution by the powdery valonex heating for dissolving that adds water;
<2> chemical reagent polyacrylamide flocculation sediment
In the rubber Bowl vat liquor of step <1> or the valonex aqueous solution, add chemical reagent polyacrylamide to stir evenly, add-on be in solution dry biomass 0.8%, leave standstill 12-24h, make the impurity flocculation sediments such as part non-tannis and remove the certain density dense glue of remaining solution evaporation simmer down to;
The processing of <3> organic solvent
According to the quality of dry-matter in the dense glue of step <2>, add the acetone soln of mass concentration 60% to stir evenly by solid-liquid mass ratio 1:0.5, after putting into whizzer centrifugation, remove lower sediment (part non-tannis etc.), upper solution is again by the former solid-to-liquid ratio of solid-liquid mass ratio 1:0.5() add the acetone soln of mass concentration 85% to stir evenly, ditto carry out centrifugation, remove precipitation (non-tannis etc.) part, mixing solutions is put to heating recovery organic solvent-acetone on rotatory evaporator;
<4> chromatography column is crossed post
After step <3> remaining solution after treatment is cooling, on the chromatography column that ion exchange resin is housed, cross post;
<5> is dry
The solution of gained after post, when evaporation concentration to solution contains dry-matter 50% left and right on rotatory evaporator, puts into vacuum drying oven 70-75 DEG C reduced vacuum dry, obtains meal after grinding; Or when solution evaporation is concentrated into containing dry-matter 20%-30%, the dry meal that to obtain of spraying.
For the lower problem of current valonex product tannin content, contriver has carried out large quantity research to the purifying of valonex, thereby set up purification process of the present invention, this method is taking rubber Bowl or valonex as main raw material, and its operational path is: rubber Bowl heating lixiviate or valonex heating for dissolving → chemical reagent polyacrylamide flocculation sediment → organic solvent processing (acetone soln low, high density carries out the at twice) → chromatography column that adds water that adds water is crossed post → dry → finished product.Application the present invention can effectively remove the impurity such as the non-tannis in valonex, and its tannin content of valonex finished product of the purifying of acquisition reaches more than 80%, and yield is also more than 80%.
Embodiment
Embodiment 1
Take through broken rubber Bowl raw material 200g, put into 1000ml beaker, by solid: liquor ratio 1:2.5 adds clear water (tap water), be placed in water-bath and heat lixiviate, every 2h fluid once, total immersion is carried six times (first, secondary extraction temperature is 60-70 DEG C, the 3rd, four extraction temperatures are 70-80 DEG C, the 5th, six extraction temperatures are 80-90 DEG C), six leach liquors merging are placed in a plastic tank, obtain leach liquor 2600g(containing dry-matter 2.2%), add 0.46g polyacrylamide to stir evenly, disgorging after standing 18h, solution is placed in reduction vaporization on rotatory evaporator and is concentrated into containing dry 14.3%.
Take cooled concentrated solution 200g and put into beaker, after adding the acetone soln of 14.3g mass concentration 60% to stir evenly, pour centrifuge tube into and build, then be placed in whizzer, setting speed is 3000r/min, centrifugation 12min, upper solution is refunded in beaker and (discarded precipitation), after adding again the acetone soln of 14.3g mass concentration 85% to stir evenly, pour in centrifuge tube, be placed in whizzer by former setting speed centrifugation 12min, incline and upper solution and be placed on rotatory evaporator after heating recovery organic solvent, be cooled to room temperature, solution is poured into chromatography column (domestic simple glass core chromatography column, specification: 30mm*500mm, in-built AB-8 macroporous adsorbent resin, descend same) mistake post, when subsequently solution being put on rotatory evaporator to reduction vaporization and being concentrated into solution containing dry-matter 50% left and right, pour in a little porcelain dish, put it in vacuum drying oven and dry in 70-75 DEG C, after grinding, taking-up obtains meal 25.8g(water content 11.30%), yield (by over dry thing) 80.02%.
Finished product detects by LY/T1082-2008 tannin extract analytical test method, and tannin content is 80.9%.
Embodiment 2
Take through broken rubber Bowl raw material 400g, put into 2000ml large beaker, carry out lixiviate processing by embodiment 1.Six leach liquors merging are placed in a plastic tank, add 1.1g polyacrylamide to stir evenly, disgorging after standing 18h, and solution is placed in reduction vaporization on rotatory evaporator and is concentrated into containing dry 13.8%.
Take cooled concentrated solution 300g and put into beaker, after adding the acetone soln of 20.7g mass concentration 60% to stir evenly, pour centrifuge tube into and build, then be placed in whizzer, setting speed is 3000r/min, centrifugation 12min, upper solution is refunded in beaker and (discarded precipitation), after adding again the acetone soln of 20.7g mass concentration 85% to stir evenly, pour in centrifuge tube, be placed in whizzer by former setting speed centrifugation 12min, incline and upper solution and be placed on rotatory evaporator after heating recovery organic solvent, be cooled to room temperature, solution is poured into chromatography column (domestic simple glass core chromatography column, specification: 40mm*500mm) mistake post, when subsequently solution being put on rotatory evaporator to reduction vaporization and being concentrated into solution containing dry-matter 20% left and right, take that on mini spray dryer, to carry out spray dried dry, obtain powdery finished product 36.4g(water content 9.0%), yield (by over dry thing) 80.01%.
Finished product detects by LY/T1082-2008 tannin extract analytical test method, and tannin content is 81.3%.
Embodiment 3
(Baise of Guangxi Lin Hua factory produces to take powdery valonex, tannin content 70.6%) 50g is in beaker, add clear water 500ml, be placed in water-bath and be heated to 60-70 DEG C and stirring and dissolving, after being cooled to room temperature, add 0.4g polyacrylamide to stir evenly, after leaving standstill 24h, remove precipitation, in solution, add the acetone soln of 25g mass concentration 60% to stir evenly, then pour in centrifuge tube and build, put into whizzer, press rotating speed 3000r/min centrifugation 12min, incline and upper solution, in mixing solutions, add the acetone soln of 25g mass concentration 85% to stir evenly again, mixing solutions is poured in centrifuge tube, be placed in whizzer by former rotating speed centrifugation 12min, incline and upper solution and put on rotatory evaporator after heating recovery acetone, be cooled to room temperature, pour solution into chromatography column (model, specification is with embodiment 2) the middle post of crossing, crossing solution after post puts on rotatory evaporator when reduction vaporization is concentrated into solution containing dry-matter 50% left and right, put it in vacuum drying oven and dry in 70-75 DEG C, after grinding, taking-up obtains meal 40.1g (water content 9.5%), yield 80.2%.
Finished product detects by LY/T1082-2008 tannin extract analytical test method, and its tannin mass fraction is 81.7%.
Embodiment 4
(Baise of Guangxi Lin Hua factory produces to take powdery valonex, tannin content 70.6%) 100g is in beaker, add clear water 1000ml, be placed in water-bath and be heated to 60-70 DEG C and stirring and dissolving, after being cooled to room temperature, add 0.8g polyacrylamide to stir evenly, after leaving standstill 24h, remove precipitation, in solution, add the acetone soln of 50g mass concentration 60% to stir evenly, then pour in centrifuge tube and build, put into whizzer, press rotating speed 3000r/min centrifugation 12min, incline and upper solution, in mixing solutions, add the acetone soln of 50g mass concentration 85% to stir evenly again, mixing solutions is poured in centrifuge tube, be placed in whizzer by former rotating speed centrifugation 12min, incline and upper solution and put on rotatory evaporator after heating recovery acetone, be cooled to room temperature, pour solution into chromatography column (model, specification is with embodiment 2) the middle post of crossing, crossing solution after post puts on rotatory evaporator when reduction vaporization is concentrated into solution containing dry-matter 20% left and right, it is carried out on mini spray dryer to spray dried dry, obtain meal 80.6g (water content 9.3%), yield 80.6%.
Finished product detects by LY/T1082-2008 tannin extract analytical test method, and its tannin mass fraction is 81.6%.
Claims (3)
1. a purification process for valonex, is characterized in that: in rubber Bowl vat liquor or the valonex aqueous solution, add chemical reagent polyacrylamide, make the impurity flocculation sediments such as part non-tannis and remove; In solution, add organic solvent-acetone again, remove and be insoluble to the impurity such as the part non-tannis of organic solvent-acetone; Subsequently solution is analysed to post by resinbed, the further impurity such as remove portion non-tannis, gained solution is after drying and get final product.
2. the purification process of valonex according to claim 1, is characterized in that: described in add organic solvent-acetone to process totally twice, add for the first time the acetone soln of mass concentration 60%, add for the second time the acetone soln of mass concentration 85%.
3. the purification process of valonex according to claim 2, is characterized in that comprising the following steps:
<1> rubber Bowl heating lixiviate or the valonex heating for dissolving that adds water that adds water
Rubber Bowl raw material is added water at 60-90 DEG C through extracted many times, and vat liquor merges; Or be made into the valonex aqueous solution by the powdery valonex heating for dissolving that adds water;
<2> chemical reagent polyacrylamide flocculation sediment
In the rubber Bowl vat liquor of step <1> or the valonex aqueous solution, add chemical reagent polyacrylamide to stir evenly, add-on be in solution dry biomass 0.8%, leave standstill 12-24h, make the impurity flocculation sediments such as part non-tannis and remove the dense glue of remaining solution evaporation simmer down to;
The processing of <3> organic solvent
According to the quality of dry-matter in the dense glue of step <2>, add the acetone soln of mass concentration 60% to stir evenly by solid-liquid mass ratio 1:0.5, after putting into whizzer centrifugation, remove lower sediment, upper solution adds the acetone soln of mass concentration 85% to stir evenly by solid-liquid mass ratio 1:0.5 again, ditto carry out centrifugation, remove precipitation part, mixing solutions is put to heating recovery organic solvent-acetone on rotatory evaporator;
<4> chromatography column is crossed post
After step <3> remaining solution after treatment is cooling, on the chromatography column that ion exchange resin is housed, cross post;
<5> is dry
The solution of gained after post, when evaporation concentration to solution contains dry-matter 50% on rotatory evaporator, puts into vacuum drying oven 70-75 DEG C reduced vacuum dry, obtains meal after grinding; Or when solution evaporation is concentrated into containing dry-matter 20%-30%, the dry meal that to obtain of spraying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410138042.1A CN103882160B (en) | 2014-04-08 | 2014-04-08 | The purification process of valonex |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410138042.1A CN103882160B (en) | 2014-04-08 | 2014-04-08 | The purification process of valonex |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103882160A true CN103882160A (en) | 2014-06-25 |
| CN103882160B CN103882160B (en) | 2016-02-17 |
Family
ID=50951277
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410138042.1A Expired - Fee Related CN103882160B (en) | 2014-04-08 | 2014-04-08 | The purification process of valonex |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103882160B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111134245A (en) * | 2020-01-19 | 2020-05-12 | 中国林业科学研究院林产化学工业研究所 | Valonea extract feed additive for broiler chickens and application thereof |
| CN116535977A (en) * | 2023-05-05 | 2023-08-04 | 广西林业集团有限公司 | Method for efficiently extracting tannin extract by compound co-leaching |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381420A (en) * | 2008-10-30 | 2009-03-11 | 河北科技大学 | Continuous extraction method of pectin, tannin and pigment from persimmon exocarp |
| EP2044848A1 (en) * | 2007-10-01 | 2009-04-08 | STC S.r.l. Science Technology & Consulting | Process for the treatment and the recovery of humid pomace produced by two-phase oil mills |
| CN102688613A (en) * | 2012-05-24 | 2012-09-26 | 杭州利群环保纸业有限公司 | Extract deep purification and edulcoration process in manufacturing technology of papermaking tobacco sheets |
| CN103265892A (en) * | 2013-05-27 | 2013-08-28 | 广西壮族自治区林业科学研究院 | Method for purifying eucalyptus tannin |
| CN103524571A (en) * | 2013-10-08 | 2014-01-22 | 河北科技大学 | Recycling method for preparing tannic acid from walnut residues |
-
2014
- 2014-04-08 CN CN201410138042.1A patent/CN103882160B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2044848A1 (en) * | 2007-10-01 | 2009-04-08 | STC S.r.l. Science Technology & Consulting | Process for the treatment and the recovery of humid pomace produced by two-phase oil mills |
| CN101381420A (en) * | 2008-10-30 | 2009-03-11 | 河北科技大学 | Continuous extraction method of pectin, tannin and pigment from persimmon exocarp |
| CN102688613A (en) * | 2012-05-24 | 2012-09-26 | 杭州利群环保纸业有限公司 | Extract deep purification and edulcoration process in manufacturing technology of papermaking tobacco sheets |
| CN103265892A (en) * | 2013-05-27 | 2013-08-28 | 广西壮族自治区林业科学研究院 | Method for purifying eucalyptus tannin |
| CN103524571A (en) * | 2013-10-08 | 2014-01-22 | 河北科技大学 | Recycling method for preparing tannic acid from walnut residues |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111134245A (en) * | 2020-01-19 | 2020-05-12 | 中国林业科学研究院林产化学工业研究所 | Valonea extract feed additive for broiler chickens and application thereof |
| CN116535977A (en) * | 2023-05-05 | 2023-08-04 | 广西林业集团有限公司 | Method for efficiently extracting tannin extract by compound co-leaching |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103882160B (en) | 2016-02-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106432368A (en) | Method of efficiently extracting fulvic acid from papermaking black liquid | |
| CN106348273A (en) | Extraction agent for preparing industrial phosphoric acid through hydrochloric acid method and extraction method thereof | |
| CN103665195B (en) | A kind of method utilizing agar in Enzymatic Extraction fragrant plant mentioned in ancient texts | |
| CN103882160B (en) | The purification process of valonex | |
| CN102583916A (en) | Method for removing heavy metal from sludge | |
| CN105461778A (en) | Method for extracting tea saponin from sasangua cake | |
| CN101565438B (en) | Purification method for Tylosin | |
| CN105985315A (en) | Method for extracting nicotine from tobacco waste | |
| CN102746354B (en) | Method for extracting tylosin by tylosin fermentation broth | |
| CN101260129A (en) | Method of purifying tannic acid | |
| CN102924969A (en) | Method for refining paprika red pigment | |
| CN101885494B (en) | Purification technology for producing salt in waste water by thiofide | |
| CN102464898B (en) | Method for recovering yellow ginger pigment from yellow ginger hydrolysate saponin extraction waste liquid | |
| CN101491319B (en) | Method for producing dried old orange peel and anti-scaling anti-corrosive detergent using orange peel | |
| CN106268693A (en) | A kind of filtering material for sewage disposal and preparation method thereof | |
| CN101759152A (en) | Method for removing impurities in process of extracting iodine by using iodine-contained phosphate ore as raw materials | |
| CN105193880A (en) | Extraction method for actinidia arguta flavones | |
| CN105152142A (en) | Method for recovering sulfuric acid from waste acid produced by anthraquinone production | |
| CN102964355B (en) | Preparation method of penicillin G sulfoxide | |
| CN101830591A (en) | Water recycling method for use in extraction process of vanadium pentoxide | |
| CN101708830A (en) | Method for purifying raffinate | |
| CN101250141B (en) | Method for preparing tobias acid by effective components extracted from waste water of tobias acid production | |
| CN103864868A (en) | Green extraction process of natural active flavone-rutin | |
| CN113402987A (en) | Extraction method of bayberry tannin extract | |
| CN102976279B (en) | Method for extracting sulfur and inorganic salt from wet-desulfurization waste sulfur paste |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160217 Termination date: 20170408 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |