CN105969527A - Comprehensive utilization method of ginger leaves - Google Patents
Comprehensive utilization method of ginger leaves Download PDFInfo
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Abstract
The invention discloses a comprehensive utilization method of ginger leaves. The method comprises the following steps: (1) extracting ginger leaves by supercritical CO2 extraction to obtain ginger leaf raw oil; (2) carrying out molecular distillation on the ginger leaf raw oil to obtain ginger leaf essential oil; (3) reextracting the ginger leaf raw material extracted by supercritical CO2 extraction by using alcohol, filtering, and carrying out vacuum concentration on the obtained filtrate to obtain ginger leaf total flavones; (4) separating the ginger leaf total flavones by column chromatography to obtain ginger leaf phenolic acid and ginger leaf flavones; and (5) carrying out water extraction and filtration on the filter residue obtained by the alcohol extraction, and carrying out vacuum concentration and drying on the obtained filtrate to obtain ginger leaf polysaccharides. The method can simultaneously extract multiple components (ginger leaf essential oil, ginger leaf phenolic acid, ginger leaf flavones, ginger leaf polysaccharide and the like) in the ginger leaves, thereby obviously enhancing the comprehensive utilization ratio of the ginger leaves, changing wastes into valuable substances, and implementing the economic value. The method can implement no waste generation in the production process, and is green and environment-friendly.
Description
Technical field
The present invention relates to comprehensive plant and utilize field, particularly relate to the method for comprehensive utilization of a kind of Folium Zingiberis.
Background technology
Rhizoma Zingiberis Recens, Zingiberaceae Rhizoma Zingiberis Recens belongs to herbaceos perennial, has yellow green flower the rhizome of irritant fragrance, is a kind of industrial crops having higher value of exploiting and utilizing.Rhizoma Zingiberis Recens is in addition to containing the biological active substances such as (4-hydroxy-3-methoxyphenyl)ethyl methyl ketone, gingerol, possibly together with protein, polysaccharide, vitamin and various trace elements, integrate nutrition, seasoning, health care, it is considered as the health product of integration of edible and medicinal herbs from ancient times by physician, there is the plurality of health care functions such as cold relieving, damp eliminating, warming the stomach, acceleration blood circulation.
In China, the edible and medicinal history of Rhizoma Zingiberis Recens is the longest, and it develops and also compares early, and major product has Rhizoma Zingiberis, sweet Rhizoma Zingiberis Recens, Rhizoma Zingiberis Recens beans, Sucus Zingberis etc., is focused on the utilization to race stem.
Folium Zingiberis is the leaf of Rhizoma Zingiberis Recens, pungent, warm, nontoxic.The traditional Chinese medical science is thought that Folium Zingiberis has and is controlled blood stasis of injuring, warming the lung, heart disease, the liver benefiting, spleen invigorating, stomach function regulating, strong muscle, beauty care, logical blood, effect of regulating menstruation.As described in " Medical Treasures of the Golden Chamber ": " meat chopped into small pieces is many does not disappears for food, becomes disease sick, rises with one of Folium Zingiberis juice drink ";Described in " book on Chinese herbal medicine converges and says ": " aproll is tied, and kills fish meat chopped into small pieces raw food various masses, smashes juice and beverage ".But, at present in purchase and producing, Folium Zingiberis often abandons as garbage, is not further developed it, causes the waste of resource.And fact proved, Folium Zingiberis has the biggest development and application values.Research shows, containing nutritional labelings such as rich in protein, sugar, polysaccharide, dietary fiber, vitamin, trace element in Folium Zingiberis.Meanwhile, Folium Zingiberis quintessence oil has the multiple biological activitys such as antibacterial and antioxidation, and, cosmetics, medicine and other fields fresh-keeping at food antiseptic have broad application prospects.Therefore, it is badly in need of Folium Zingiberis is carried out deep development utilization, excavates its potential value, turn waste into wealth, it is achieved its economic worth, promote that China's Rhizoma Zingiberis Recens industry deeply develops.
Summary of the invention
Present invention aim to address the deficiencies in the prior art, it is provided that a kind of efficient, Folium Zingiberis method of comprehensive utilization of environmental protection, the compositions such as Folium Zingiberis quintessence oil, water soluble ingredient, involatile constituent and extraction residue in Folium Zingiberis are carried out comprehensive development and utilization.
The technical solution used in the present invention is: the method for comprehensive utilization of a kind of Folium Zingiberis, comprises the steps: that (1) uses supercritical CO2Extraction extraction Folium Zingiberis obtains Folium Zingiberis crude oil, supercritical CO2Extracting pressure is 15~35 MPa, and extraction temperature is 35~60 DEG C, and separating I pressure is 7~10 MPa, and separating II pressure is 4.5~6.5 MPa, and separating I temperature is 30~60 DEG C, and separating II temperature is 30~60 DEG C, CO2Flow is 25~45
L/h, extraction time is 2~4 h;(2) Folium Zingiberis crude oil is obtained Folium Zingiberis quintessence oil by molecular distillation, molecular distillation feeding temperature 40~50 DEG C, chilling temperature 10~40 DEG C, system vacuum 0.1~50 Pa, distillation column temperature 110~200 DEG C, knifing machine rotating speed 150~350 r/min, distillation speed 0.1~1mL/min;(3) will be through supercritical CO2Extraction is obtained by extraction in Folium Zingiberis raw material the ethanol adding 5~40 times of quality, extraction temperature 50~80 DEG C, extraction time 2~4 h, is then passed through filtering, and filter vacuum concentrates the 1/10 of volume extremely original volume, obtains Folium Zingiberis total flavones;(4) by Folium Zingiberis total flavones by column chromatography for separation, Folium Zingiberis phenolic acid and Folium Zingiberis flavone are obtained;(5) filtering residue after alcoholic extract is added the ultra-pure water of 5~40 times of quality, extraction temperature 50~100 DEG C, extraction time 2~4 h, then filters, by the filtrate of gained through being concentrated in vacuo and be dried to obtain Folium Zingiberis polysaccharide;(6) filtering residue after being extracted by water is fabricated to briquette-fuel, replaces coal etc. as fuel;(7) the remaining ash that will burn reclaims as fertilizer.
As a further improvement on the present invention, by step (5) through water extract after filtering residue as feed additive.
As the further improvement of the present invention, in described step (4), column chromatography uses ion exchange resin to separate.
As the further improvement of the present invention, described ion exchange resin selects D918, D923, D952, D290, D296, D284,201 × 4,201 × 7.
As the further improvement of the present invention, described step (4) by Folium Zingiberis total flavones concentrated solution through chromatographic column upper prop, eluting, collection eluent, concentrate, be dried, obtain Folium Zingiberis phenolic acid and Folium Zingiberis flavone.
As the further improvement of the present invention, eluant is low-carbon alcohols, and wherein eluant strength is 20~50% to obtain Folium Zingiberis phenolic acid, and eluant strength is 70~90% to obtain Folium Zingiberis flavone.
As the further improvement of the present invention, remaining Folium Zingiberis residue is dried, add as feed additive in feed preparation, after at least one mixing in same Semen Maydis, bean cake, Testa oryzae, Testa Tritici, produce feed stripped.
As a further improvement on the present invention, remaining Folium Zingiberis residue is dried by described step (6), utilizes stalk block making machine to be pressed into solid fuel, the briquette-fuel density being pressed into: 700~1400 kilograms per cubic meter;Ash: 1~20%;Moisture≤10%, calorific value is 2000~5000 kilocalories.
Vacuum lyophilization is carried out as the product obtained by the further improvement of the present invention, step (4) and step (5).
The present invention uses and provides the benefit that: the inventive method can realize extracting Multiple components in Folium Zingiberis (Folium Zingiberis quintessence oil, Folium Zingiberis phenolic acid, Folium Zingiberis flavone, Folium Zingiberis polysaccharide etc.) simultaneously, significantly improves the comprehensive utilization ratio of Folium Zingiberis, turns waste into wealth, it is achieved economic worth.And production process can be realized without garbage generation, environmental protection.
Accompanying drawing explanation
Fig. 1 is the process route chart of the present invention.
Detailed description of the invention
Embodiment in detail below, the present invention is described further.
The method of comprehensive utilization of a kind of Folium Zingiberis, comprises the steps:
(1) supercritical CO is used2Extraction extraction Folium Zingiberis obtains Folium Zingiberis crude oil, supercritical CO2Extracting pressure is 15~35 MPa, and extraction temperature is 35~60 DEG C, and separating I pressure is 7~10 MPa, and separating II pressure is 4.5~6.5 MPa, and separating I temperature is 30~60 DEG C, and separating II temperature is 30~60 DEG C, CO2Flow is 25~45 L/h, and extraction time is 2~4 h;
(2) Folium Zingiberis crude oil is obtained Folium Zingiberis quintessence oil by molecular distillation, molecular distillation feeding temperature 40~50 DEG C, chilling temperature 10~40 DEG C, system vacuum 0.1~50 Pa, distillation column temperature 110~200 DEG C, knifing machine rotating speed 150~350 r/min, distillation speed 0.1~1mL/min;
(3) will be through supercritical CO2Extraction is obtained by extraction in Folium Zingiberis raw material the ethanol adding 5~40 times of quality, extraction temperature 50~80 DEG C, extraction time 2~4 h, is then passed through filtering, and filter vacuum concentrates the 1/10 of volume extremely original volume, obtains Folium Zingiberis total flavones;
(4) by Folium Zingiberis total flavones by column chromatography for separation, Folium Zingiberis phenolic acid and Folium Zingiberis flavone are obtained;
(5) filtering residue after alcoholic extract is added the ultra-pure water of 5~40 times of quality, extraction temperature 50~100 DEG C, extraction time 2~4 h, then filters, by the filtrate of gained through being concentrated in vacuo and be dried to obtain Folium Zingiberis polysaccharide;
(6) filtering residue after being extracted by water is fabricated to briquette-fuel, replaces coal etc. as fuel;
(7) the remaining ash that will burn reclaims as fertilizer.
Wherein step (4) by Folium Zingiberis total flavones concentrated solution through chromatographic column upper prop, eluting, collection eluent, concentrate, be dried, obtain Folium Zingiberis phenolic acid and Folium Zingiberis flavone, wherein eluant is low-carbon alcohols, wherein eluant strength is 20~50% to obtain Folium Zingiberis phenolic acid, and eluant strength is 70~90% to obtain Folium Zingiberis flavone.
In step (4), column chromatography uses ion exchange resin to separate, and step (4) ion exchange resin can select D918, D923, D952, D290, D296, D284,201 × 4,201 × 7 simultaneously.
Wherein the residue Folium Zingiberis residue obtained after step (5) is dried, add as feed additive in feed preparation, after at least one mixing in same Semen Maydis, bean cake, Testa oryzae, Testa Tritici, produce feed stripped.
Wherein step (6) is specially and is dried by remaining Folium Zingiberis residue, utilizes stalk block making machine to be pressed into solid fuel, the briquette-fuel density being pressed into: 700~1400 kilograms per cubic meter;Ash: 1~20%;Moisture≤10%, calorific value is 2000~5000 kilocalories.
Folium Zingiberis used by following example is Tongling Rhizoma Zingiberis Folium Zingiberis, and Tongling Rhizoma Zingiberis has long enjoyed a good reputation with characteristics such as " block great Pi are thin, and the many slags of juice are few, and meat is tender and crisp, aromatic flavor ", and in its Folium Zingiberis, active constituent content is the highest.
Embodiment 1, (1) supercritical CO2Extraction Folium Zingiberis, extracting pressure is 35 MPa, and extraction temperature is 40 DEG C, and separating I pressure is 10 MPa, and separating II pressure is 4.5 MPa, and separating I temperature is 35 DEG C, and separating II temperature is 30 DEG C, CO2Flow is 45 L/h, and extraction time is 4 h, separates and collects and i.e. obtains Folium Zingiberis crude oil;(2) Folium Zingiberis crude oil is continuously entered molecular still, feeding temperature 40 DEG C, chilling temperature 20 DEG C, system vacuum 1 Pa, distillation column temperature 110
DEG C, knifing machine rotating speed 160 r/min, distillation speed 0.1 mL/min, collect distillate be Folium Zingiberis quintessence oil;(3) through supercritical CO2Adding the ethanol of 10 times of quality, extraction temperature 78 DEG C, extraction time 2 h in the Folium Zingiberis raw material of extraction, filter, filter vacuum concentrates, and concentration volume, to the 1/10 of original volume, obtains Folium Zingiberis total flavones;(4) by Folium Zingiberis total flavones through D918 ion-exchange chromatography upper prop, respectively by 20~50% ethanol elution, collect eluent, concentrate, be dried, Folium Zingiberis phenolic acid is obtained;70~90% ethanol elution, collect eluent, concentrate, be dried, obtain Folium Zingiberis flavone;(5) adding the ultra-pure water of 5 times of quality, extraction temperature 100 DEG C, extraction time 2 h in the filtering residue after alcoholic extract, filter, filter vacuum is concentrated to dryness, and obtains Folium Zingiberis polysaccharide;(6) remaining Folium Zingiberis residue is dried, add as feed additive in feed preparation, after at least one mixing in same Semen Maydis, bean cake, Testa oryzae, Testa Tritici, produce feed stripped.Production procedure is as follows: raw material reception-pulverizing-dispensing and stirring-flow scheme design-granulation-discharging.
Embodiment 2, (1) supercritical CO2Extraction Folium Zingiberis, extracting pressure is 15 MPa, and extraction temperature is 60 DEG C, and separating I pressure is 7 MPa, and separating II pressure is 6.5 MPa, and separating I temperature is 60 DEG C, and separating II temperature is 40 DEG C, CO2Flow is 25 L/h, and extraction time is 2 h, separates and collects and i.e. obtains Folium Zingiberis crude oil;(2) Folium Zingiberis crude oil is continuously entered molecular still, feeding temperature 50 DEG C, chilling temperature 25 DEG C, system vacuum 10 Pa, distillation column temperature 200 DEG C, knifing machine rotating speed 310
R/min, distillation speed 1 ml/min, collect distillate and be Folium Zingiberis quintessence oil;(3) through supercritical CO2Adding the ethanol of 40 times of quality, extraction temperature 50 DEG C, extraction time 4 h in the Folium Zingiberis raw material of extraction, filter, filter vacuum concentrates, and concentration volume, to the 1/10 of original volume, obtains Folium Zingiberis total flavones;(4) by Folium Zingiberis total flavones through D918 ion-exchange chromatography upper prop, by 20~50% ethanol elution, collect eluent, concentrate, be dried, Folium Zingiberis phenolic acid is obtained;(5) adding the ultra-pure water of 20 times of quality, extraction temperature 60 DEG C, extraction time 4 h in the filtering residue after alcoholic extract, filter, filter vacuum is concentrated to dryness, and obtains Folium Zingiberis polysaccharide;(6) remaining Folium Zingiberis residue is dried, utilize stalk block making machine to be pressed into solid fuel, the briquette-fuel density being pressed into: 700~1400 kilograms per cubic meter;Ash: 1~20%;Moisture≤10%, calorific value is 2000~5000 kilocalories.
Embodiment 3, the method for comprehensive utilization of a kind of Folium Zingiberis, comprise the steps: that (1) uses supercritical CO2Extraction extraction Folium Zingiberis obtains Folium Zingiberis crude oil, supercritical CO2Extracting pressure is 30 MPa, and extraction temperature is 45 DEG C, and separating I pressure is 8 MPa, and separating II pressure is 5.5MPa, and separating I temperature is 45 DEG C, and separating II temperature is 45 DEG C, CO2Flow is 30 L/h, and extraction time is 3 h;(2) Folium Zingiberis crude oil is obtained Folium Zingiberis quintessence oil, molecular distillation feeding temperature 45 DEG C, chilling temperature 30 DEG C, system vacuum 30 by molecular distillation
Pa, distillation column temperature 160 DEG C, knifing machine rotating speed 240 r/min, distillation speed 0.7mL/min;(3) will be through supercritical CO2Extraction is obtained by extraction in Folium Zingiberis raw material the ethanol adding 20 times of quality, extraction temperature 65 DEG C, extraction time 3 h, is then passed through filtering, and filter vacuum concentrates the 1/10 of volume extremely original volume, obtains Folium Zingiberis total flavones;(4) by Folium Zingiberis total flavones concentrated solution through chromatographic column upper prop, eluting, collection eluent, concentrate, be dried, obtain Folium Zingiberis phenolic acid and Folium Zingiberis flavone, amount of eluent is low-carbon alcohols, and wherein eluant strength is 20~50% to obtain Folium Zingiberis phenolic acid, and eluant strength is 70~90% to obtain Folium Zingiberis flavone;(5) filtering residue after alcoholic extract is added the ultra-pure water of 20 times of quality, extraction temperature 75 DEG C, extraction time 3 h, then filters, by the filtrate of gained through being concentrated in vacuo and be dried to obtain Folium Zingiberis polysaccharide;(6) remaining Folium Zingiberis residue dries, and utilizes stalk block making machine to be pressed into solid fuel, the briquette-fuel density being pressed into: 1100 kilograms per cubic meter;Ash: 10%;Moisture: 8%, calorific value is 3500 kilocalories;(7) the remaining ash that will burn reclaims as fertilizer.
The inventive method can realize extracting Multiple components in Folium Zingiberis (Folium Zingiberis quintessence oil, Folium Zingiberis phenolic acid, Folium Zingiberis flavone, Folium Zingiberis polysaccharide etc.) simultaneously, significantly improves the comprehensive utilization ratio of Folium Zingiberis, turns waste into wealth, it is achieved economic worth.And production process can be realized without garbage generation, environmental protection.
Those skilled in the art should know; the protection scheme of the present invention is not limited only to the above embodiments; various permutation and combination and conversion can also be carried out on the basis of above-described embodiment; on the premise of spirit of the present invention, the various conversion carrying out the present invention all fall within protection scope of the present invention.
Claims (9)
1. a method of comprehensive utilization for Folium Zingiberis, is characterized in that comprising the steps:
(1) supercritical CO is used2Extraction extraction Folium Zingiberis obtains Folium Zingiberis crude oil, supercritical CO2Extracting pressure is 15~35 MPa, and extraction temperature is 35~60 DEG C, and separating I pressure is 7~10 MPa, and separating II pressure is 4.5~6.5 MPa, and separating I temperature is 30~60 DEG C, and separating II temperature is 30~60 DEG C, CO2Flow is 25~45
L/h, extraction time is 2~4 h;
(2) Folium Zingiberis crude oil is obtained Folium Zingiberis quintessence oil by molecular distillation, molecular distillation feeding temperature 40~50 DEG C, chilling temperature 10~40 DEG C, system vacuum 0.1~50 Pa, distillation column temperature 110~200 DEG C, knifing machine rotating speed 150~350 r/min, distillation speed 0.1~1mL/min;
(3) will be through supercritical CO2Extraction is obtained by extraction in Folium Zingiberis raw material the ethanol adding 5~40 times of quality, extraction temperature 50~80 DEG C, extraction time 2~4 h, is then passed through filtering, and filter vacuum concentrates the 1/10 of volume extremely original volume, obtains Folium Zingiberis total flavones;
(4) by Folium Zingiberis total flavones by column chromatography for separation, Folium Zingiberis phenolic acid and Folium Zingiberis flavone are obtained;
(5) filtering residue after alcoholic extract is added the ultra-pure water of 5~40 times of quality, extraction temperature 50~100
DEG C, extraction time 2~4 h, then filters, by the filtrate of gained through being concentrated in vacuo and be dried to obtain Folium Zingiberis polysaccharide;
(6) filtering residue after being extracted by water is fabricated to briquette-fuel, replaces coal etc. as fuel;
(7) the remaining ash that will burn reclaims as fertilizer.
The method of comprehensive utilization of a kind of Folium Zingiberis the most according to claim 1, it is characterized in that by step (5) through water extract after filtering residue as feed additive.
The method of comprehensive utilization of a kind of Folium Zingiberis the most according to claim 1, is characterized in that in described step (4), column chromatography uses ion exchange resin to separate.
The method of comprehensive utilization of a kind of Folium Zingiberis the most according to claim 3, is characterized in that described ion exchange resin selects D918, D923, D952, D290, D296, D284,201 × 4,201 × 7.
The method of comprehensive utilization of a kind of Folium Zingiberis the most according to claim 1, it is characterized in that described step (4) by Folium Zingiberis total flavones concentrated solution through chromatographic column upper prop, eluting, collection eluent, concentrate, be dried, obtain Folium Zingiberis phenolic acid and Folium Zingiberis flavone.
The method of comprehensive utilization of a kind of Folium Zingiberis the most according to claim 5, is characterized in that eluant is low-carbon alcohols, and wherein eluant strength is 20~50% to obtain Folium Zingiberis phenolic acid, and eluant strength is 70~90% to obtain Folium Zingiberis flavone.
The method of comprehensive utilization of a kind of Folium Zingiberis the most according to claim 2, it is characterized in that drying remaining Folium Zingiberis residue, feed preparation adds as feed additive, after at least one mixing in same Semen Maydis, bean cake, Testa oryzae, Testa Tritici, produces feed stripped.
The method of comprehensive utilization of a kind of Folium Zingiberis the most according to claim 1, it is characterized in that remaining Folium Zingiberis residue is dried by described step (6), stalk block making machine is utilized to be pressed into solid fuel, the briquette-fuel density being pressed into: 700~1400 kilograms per cubic meter;Ash: 1~20%;Moisture≤10%, calorific value is 2000~5000 kilocalories.
9., according to claim 1 as the method for comprehensive utilization of a kind of Folium Zingiberis described in any one in 8, it is characterized in that the product obtained by described step (4) and step (5) carries out vacuum lyophilization.
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CN114774201A (en) * | 2022-06-01 | 2022-07-22 | 山东大艾姜山农业科技有限公司 | Comprehensive treatment device and treatment method for ginger stalks used for ginger oil production |
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