CN102250155A - Method for extracting concentrated tannin from grape pomace - Google Patents
Method for extracting concentrated tannin from grape pomace Download PDFInfo
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- CN102250155A CN102250155A CN2011101961430A CN201110196143A CN102250155A CN 102250155 A CN102250155 A CN 102250155A CN 2011101961430 A CN2011101961430 A CN 2011101961430A CN 201110196143 A CN201110196143 A CN 201110196143A CN 102250155 A CN102250155 A CN 102250155A
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- grape skin
- tannin
- cooking liquor
- grape pomace
- extracting
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Abstract
The invention discloses a method for extracting concentrated tannin from grape pomace, which comprises the following steps of: screening the grape pomace, removing impurities, and drying to control the water content to be 5-10 percent; adding the dried grape pomace into a round bottomed flask, adding mixed alkali of sodium hydrogensulfite and sodium carbonate which is 5 percent based on the absolute dry weight of the grape pomace material and serves as an extracting agent, adding distilled water, controlling a liquid-solid ratio to be 8:1, cooking and refluxing at 100DEG C for 60 to 180 minutes, and cooling to normal temperature; pouring out cooking liquid, adding distilled water for diluting and washing, and filtering; and distilling the separated cooking liquid under reduced pressure by using a rotary evaporator and freeze-drying the cooking liquid to obtain the concentrated tannin, wherein the tannin yield is 20 to 25 percent and the effective tannin content is 45 to 50 percent. The method has the advantages of rich raw material sources and simple process, waste in the food processing industry is efficiently recycled, and the production cost of a tannin adhesive is reduced.
Description
Technical field
What the present invention relates to is a kind of method of extracting condensed tannins from grape skin, is raw material with the grape skin, is extraction agent with the mixed base.The tannin that is extracted can be used for tanning industry and tannin sill worker tackiness agent, belongs to the technical field of macromolecule adhesive.
Background technology
Grape and converted products thereof are the bigger products of the volume of world trade and the volume of trade.And in the vinify and the course of processing, unavoidably can produce a large amount of trester residuums.The grape waste residue is mainly used in fertilizer, feed and refuse treatment at present, and added value is very low.Show that after deliberation the grape waste residue contains abundant condensing class tannin, can cause certain potentially contaminated to soil in a short time with its direct landfill and compost.Therefore if grape skin is used to extract condensed tannins.Both solve the high efficiente callback utilization of the waste of food-processing industry, turned waste into wealth, met the recycle of current renewable resources, preserved the ecological environment, set up the themes of the times of the green earth.Can save production cost again, improve the power of striving unexpectedly of product.
Summary of the invention:
What the present invention proposed is a kind of method of extracting condensed tannins from grape skin, is raw material with the grape skin, is extraction agent with the mixed base.By being that raw material extracts condensed tannins with grape skin, solve the high efficiente callback utilization of the waste of food-processing industry, turn waste into wealth; Reduce the production cost of tannin again.
With with in some barks (as hard wood, pines etc.) extracting tannin compares, grape skin used in the present invention is the residuum after grape squeezes through wine brewing, in the wine brewing squeezing process in the grape some are easily molten, the tannin of low polymerization degree has been extracted by squeezing and has entered in the grape wine, remain in the grape skin mainly is that some are poorly soluble, the condensing class tannin of high-polymerization degree, therefore if adopt and the identical extraction process of extraction tannin from some barks, sodium hydroxide or yellow soda ash with the aqueous solution or lower concentration (0.5-1%) are extracting solution, and the condensed tannins yield is low; And if alkali charge is too high, again some non-tannis compositions in the grape skin are also extracted in a large number such as some polymer carbohydrates and derivative thereof, condensed tannins content reduces though the tannin yield improves effectively.Because the These characteristics of this raw material, it is extraction agent that the present invention adopts mixed base, introduces sulfonic group to improve the solubleness and the reactive behavior of grape skin tannin in the tannin structure by sulphite, improves the yield of condensed tannins when reducing the alkali consumption relatively.
Technical solution of the present invention: a kind of method of extracting condensed tannins from grape skin comprises following processing step:
(1) raw material screening and drying: grape skin is screened, remove impurity wherein, carry out drying then, dried water ratio is controlled at 5-10%;
(2) boiling extracting: get the dried grape skin of 20g and place the 250mL round-bottomed flask and add extraction agent, this extraction agent is by sodium bisulfite (NaHSO
3) add yellow soda ash (Na
2CO
3) the mixed base composition, the S-WAT (NaHSO in this mixed base
3) account for 2.5% of grape skin gross weight, yellow soda ash (Na
2CO
3) account for 2.5% of grape skin gross weight, add distilled water, the liquid-solid ratio of control alkali lye and grape skin is 8: 1, connects prolong, is heated to 100 ℃ and picks up counting, and behind the boiling backflow 60-180min, closes heating unit, is cooled to normal temperature;
(3) washing and filtering: cooking liquor is poured out, added 3 times of distilled water diluting washings, filter then, cooking liquor is isolated to the boiling liquid measure;
(4) underpressure distillation and lyophilize: isolated cooking liquor is carried out underpressure distillation with BUCHI R II type Rotary Evaporators, the control distillation temperature is at 50-60 ℃, cooking liquor moisture concentration after concentrating is controlled at 10-20%, carries out lyophilize and obtain condensed tannins; Extracting the tannin yield is 20-25%, obtains the condensed tannins over dry in extraction and heavily accounts for the heavy per-cent of raw material over dry; Effectively condensed tannins content is 45-50%, heavily accounts for alkaline extraction in the tannin over dry with formaldehyde reaction and obtains the heavy per-cent of condensed tannins over dry.
BUCHI R II type Rotary Evaporators is used in described underpressure distillation, does not have concrete decompression numerical value on the instrument, is as the criterion with the temperature of setting, and the applying pressure pump is evacuated down to and distills out water vapor be as the criterion under design temperature.
Advantage of the present invention: the waste-grape skin with food-processing industry is a raw material, and sufficient raw is the solvent extraction condensed tannins with the mixed base, and technology is easy, and tannin can be used for tanning industry and tannin sill worker tackiness agent.Therefore the high efficiente callback utilization that had both solved the waste of food-processing industry reduces the production cost of tannin again.
Embodiment
Embodiment 1:
Grape skin is screened, remove impurity wherein, carry out drying then, dried water ratio is controlled at 5-10%.Get 20g exsiccant grape skin and place round-bottomed flask, add 5% (with grape skin raw material over dry restatement) mixed base extracting solution, wherein 2.5% is sodium bisulfite (NaHSO
3) about 1g, 2.5% is yellow soda ash (Na
2CO
3) about 1g, adding distilled water, the liquid-solid ratio of control alkali lye and grape skin is 8: 1, connects prolong.Be heated to 100 ℃ and pick up counting, behind the boiling backflow 60min, close heating unit, be cooled to normal temperature.Cooking liquor is poured out, added 3 times of cold water dilution washings, filter then, cooking liquor is isolated to the boiling liquid measure.Isolated cooking liquor is carried out underpressure distillation with BUCHI R II type Rotary Evaporators, and the control distillation temperature is carried out lyophilize with the cooking liquor after concentrating (moisture concentration is controlled in the 10-20% scope) and is obtained condensed tannins at 50-60 ℃.The tannin yield is 20%, and effectively condensed tannins content is 45%.
Embodiment 2:
Grape skin is screened, remove impurity wherein, carry out drying then, dried water ratio is controlled in 10%.Get 20g exsiccant grape skin and place round-bottomed flask, add 5% (with grape skin raw material over dry restatement) mixed base extracting solution, wherein 2.5% is sodium bisulfite (NaHSO
3) about 1g, 2.5% is yellow soda ash (Na
2CO
3) about 1g, adding distilled water, the liquid-solid ratio of control alkali lye and grape skin is 8: 1, connects prolong.Be heated to 100 ℃ and pick up counting, behind the boiling backflow 120min, close heating unit, be cooled to normal temperature.Cooking liquor is poured out, added 3 times of distilled water diluting washings, filter then, cooking liquor is isolated to the boiling liquid measure.Isolated cooking liquor is carried out underpressure distillation with BUCHI R II type Rotary Evaporators, and the control distillation temperature is carried out lyophilize with the cooking liquor after concentrating (moisture concentration is controlled in the 10-20% scope) and is obtained condensed tannins at 50-60 ℃.The tannin yield is 22%, and effectively condensed tannins content is 48%.
Embodiment 3:
Grape skin is screened, remove impurity wherein, carry out drying then, dried water ratio is controlled in 10%.Get 20g exsiccant grape skin and place round-bottomed flask, add 5% (with grape skin raw material over dry restatement) mixed base extracting solution, wherein 2.5% is sodium bisulfite (NaHSO
3) about 1g, 2.5% is yellow soda ash (Na
2CO
3) about 1g, adding distilled water, the liquid-solid ratio of control alkali lye and grape skin is 8: 1, connects prolong.Be heated to 100 ℃ and pick up counting, behind the boiling backflow 120min, close heating unit, be cooled to normal temperature.Cooking liquor is poured out, added 3 times of distilled water diluting washings, filter then, cooking liquor is isolated to the boiling liquid measure.Isolated cooking liquor is carried out underpressure distillation with BUCHI R II type Rotary Evaporators, and the control distillation temperature is carried out lyophilize with the cooking liquor after concentrating (moisture concentration is controlled in the 10-20% scope) and is obtained condensed tannins at 50-60 ℃.The tannin yield is 25%, and effectively condensed tannins content is 50%.
Claims (1)
1. method of extracting condensed tannins from grape skin is characterized in that this method comprises following processing step:
(1) raw material screening and drying: grape skin is screened, remove impurity wherein, carry out drying then, dried water ratio is controlled at 5-10%;
(2) boiling extracting: get the dried grape skin of 20g and place the 250mL round-bottomed flask and add extraction agent, this extraction agent is by sodium bisulfite (NaHSO
3) add yellow soda ash (Na
2CO
3) the mixed base composition, the S-WAT (NaHSO in this mixed base
3) account for 2.5% of grape skin gross weight, yellow soda ash (Na
2CO
3) account for 2.5% of grape skin gross weight, add distilled water, the liquid-solid ratio of control alkali lye and grape skin is 8: 1, connects prolong, is heated to 100 ℃ and picks up counting, and behind the boiling backflow 60-180min, closes heating unit, is cooled to normal temperature;
(3) washing and filtering: cooking liquor is poured out, added 3 times of distilled water diluting washings, filter then, cooking liquor is isolated to the boiling liquid measure;
(4) underpressure distillation and lyophilize: isolated cooking liquor is carried out underpressure distillation with BUCHI R II type Rotary Evaporators, the control distillation temperature is at 50-60 ℃, cooking liquor moisture concentration after concentrating is controlled at 10-20%, carries out lyophilize and obtain condensed tannins.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101961430A CN102250155A (en) | 2011-07-14 | 2011-07-14 | Method for extracting concentrated tannin from grape pomace |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101961430A CN102250155A (en) | 2011-07-14 | 2011-07-14 | Method for extracting concentrated tannin from grape pomace |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102250155A true CN102250155A (en) | 2011-11-23 |
Family
ID=44977760
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011101961430A Pending CN102250155A (en) | 2011-07-14 | 2011-07-14 | Method for extracting concentrated tannin from grape pomace |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107841268A (en) * | 2017-11-28 | 2018-03-27 | 南京林业大学 | A kind of preparation method of Grape Skin tannin modified phenolic resin adhesive |
| CN111233554A (en) * | 2020-03-19 | 2020-06-05 | 广西壮族自治区林业科学研究院 | Organic fertilizer prepared by resource utilization of forestry processing residues and method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020028259A1 (en) * | 1997-12-30 | 2002-03-07 | Marc Feries | Method for obtaining grape tannin, resulting tannin and uses |
-
2011
- 2011-07-14 CN CN2011101961430A patent/CN102250155A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020028259A1 (en) * | 1997-12-30 | 2002-03-07 | Marc Feries | Method for obtaining grape tannin, resulting tannin and uses |
Non-Patent Citations (3)
| Title |
|---|
| 赵文杰，等: "葡萄皮渣中单宁的提取纯化及含量测定", 《中国酿造》 * |
| 郭珊珊: "石榴中单宁的分离纯化、结构及活性研究", 《华中农业大学硕士学位论文》 * |
| 陈栓虎，等: "水溶法从石榴皮中提取单宁研究简报", 《陕西农业科学》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107841268A (en) * | 2017-11-28 | 2018-03-27 | 南京林业大学 | A kind of preparation method of Grape Skin tannin modified phenolic resin adhesive |
| CN107841268B (en) * | 2017-11-28 | 2020-06-09 | 南京林业大学 | Preparation method of grape skin tannin modified phenolic resin adhesive |
| CN111233554A (en) * | 2020-03-19 | 2020-06-05 | 广西壮族自治区林业科学研究院 | Organic fertilizer prepared by resource utilization of forestry processing residues and method thereof |
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Application publication date: 20111123 |