CN101070508A - Method for extracting effective component in capsicum and potatos - Google Patents

Method for extracting effective component in capsicum and potatos Download PDF

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CN101070508A
CN101070508A CNA200710049323XA CN200710049323A CN101070508A CN 101070508 A CN101070508 A CN 101070508A CN A200710049323X A CNA200710049323X A CN A200710049323XA CN 200710049323 A CN200710049323 A CN 200710049323A CN 101070508 A CN101070508 A CN 101070508A
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CN100590187C (en
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周冠旻
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Guilin Shakes Ecology Agriculture Development Ltd Co
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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
    • 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
    • Y02E50/30Fuel from waste, e.g. synthetic alcohol or diesel

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Abstract

This invention has publicized the distill method of active ingredient in hot pepper and yam, the method as follows: crush the dry red pepper, separate its skin and seed, extract the hot pepper skin with the subcritical carbon dioxide fluid, separated them and got the spicy vegetable oil, spicy monosodium glutamate, bright red chilli red element, take the hot pepper seed and extract them with the subcritical carbon dioxide fluid, separated them and got the chilli oil, spicy monosodium glutamate, nacarat chilli red element; Take the dry potato and dry cassava to extract them separately with subcritical carbon dioxide fluid, separated them and got the mannitol and D-sorbitol; collect the cassava dregs and potato dregs and then process them, then got absolute ethyl alcohol and the ribonucleic acid (RNA); mix and dry each kind of the residual, then got the mix feed; Collect and process the every steps production waste, then got production water supply and methane. The distill method make the each kind of active ingredient of the hot pepper, and yam to be fully distilled and used, using subcritical carbon dioxide fluid to extract, the working pressure is low, flow is simple, the receiving rate and the purity of extracted active ingredient are higher.

Description

The extracting method of effective ingredient in capsicum, the potato class
(1) technical field:
The present invention relates to the extracting method of effective ingredient in the extracting method of effective ingredient in the plant, particularly capsicum, the potato class.
(2) background technology:
At present, industrial application to capsicum mainly is the capsaicin compound that extracts wherein, and capsaicin compound is the material that produces " pungent " in the capsicum, is commonly called as the pungent element.The main application of pungent element in medical treatment suppresses interior free yl in addition in addition, prevents effects such as toxic substance infringement DNA and prevention thrombosis at ease pain.In view of the pungency of pungent element, its purposes also relates to the production, biochemical pesticide of defence product and is the speciality coating of main material production with the pungent element, and is applied to take turns barnacle to stop marine alga and halobiontic adhering to.The method of extracting at present the pungent element is solvent method, and the pungent element that adopts this method to produce has existed deficiencies such as peculiar smell, the plain component content of pungent are low.For this reason, the patent No. is ZL99114739.1, name is called the Chinese invention patent of " production method of supercritical carbon dioxide extraction capsaicin compound ", a kind of production method that adopts the supercritical carbon dioxide extraction capsaicin compound is disclosed, it adopts CO 2 fluid under supercritical state, from capsicum skin powder or oleoresin capsicum, extract the effective constituent of capsaicin compound, further purify in conjunction with solvent method and crystallization process again, can make with extra care out free from extraneous odour, the capsaicin compound component content is higher than 96% capsaicin compound product.The finished product purity height that adopts this method to produce, but this method is to extract under supercritical state, operating pressure is relatively large, and relatively also higher to the requirement of equipment, this has just increased the investment to equipment; This method is just extracted the pungent element from capsicum skin powder or oleoresin capsicum, rejected chilli seed, caused the waste of raw material, make the finished product of this method have only the pungent element, hot phycoerythrobilin in the capsicum and peppery seed oil are then sold at a bargain as industry byproduct, therefore, this method does not improve the utilization ratio of capsicum.And at present producing of N.F,USP MANNITOL mainly is that raw material is produced with glucose, used glucose feed generally all be with starch after amylase liquefaction, saccharifying enzyme saccharification, make through postprocessing working procedures such as crystallization, centrifugal and oven dry again.In glucose crystallization technology, have only 85% glucose formation crystal, make crystalline glucose through centrifugal, oven dry, enter next procedure again, be used to produce N.F,USP MANNITOL.The effective rate of utilization of glucose has only 85% in the starch like this.Starch resource this than poor efficiency not only causes the waste of starch resource, also improved the production cost of N.F,USP MANNITOL.And be that raw material is produced in the technological process of N.F,USP MANNITOL with glucose, need earlier glucose to be made concentration and be 50% glucose solution, after transforming, the subsequent technique flow process just can be used to produce N.F,USP MANNITOL again.Like this, in the time that glucose solution being made, also need expend a large amount of deionized waters, and that this kind method prepares the yield of N.F,USP MANNITOL is also lower.Application number is 200510012606.8, and name is called " a kind of is the method that raw material is produced N.F,USP MANNITOL with starch ", and to disclose a kind of be the method that raw material is produced N.F,USP MANNITOL with starch.This method is that the starch after the liquefaction is carried out saccharification, epimerization, obtains seminose and glucose mixed solution; Again above-mentioned gained mixed solution is separated, obtain being rich in the solution of seminose; Then by the glucose isomerase post, gained of last step is rich in remaining glucose moiety is converted into fructose in the mother liquor of seminose, obtain the mixed solution of glucose, seminose and fructose; With the above-mentioned mixed solution that contains glucose, seminose and fructose technology hydrogenation routinely, make the mixed solution that contains sorbyl alcohol and N.F,USP MANNITOL at last, this mixed solution is through crystallization, refining, the N.F,USP MANNITOL crystal.Can stably produce N.F,USP MANNITOL by this method with higher yields.But the liquefying time of this method is longer, and saccharification temperature is higher, and pressure is also bigger, and operation exists certain danger.
(3) summary of the invention:
The present invention will disclose the extracting method that operational safety, cost are lower, can extract multiple effective ingredient from capsicum, potato class.
The extracting method of effective ingredient in capsicum of the present invention, the potato class, its step is as follows:
1) gets and carry out the skin seed after chilli is pulverized and separate;
2) the capsicum skin of gained is pulverized, the gained crushed material carries out liquefaction processing, and the liquefaction thing of gained is sent in the extraction kettle and to be fed subcritical CO 2 fluid and extract, and extraction temperature is controlled at 20~30 ℃, pressure is 3~10MPa, and the extraction time is 10~60 minutes; The effusive CO 2 fluid that contains extract enters in the separating still after step-down and separates from extraction kettle, obtain spicy oil, pungent element and large red Capsorubin, then they are concentrated respectively, crystallization, spicy oil finished product, the plain finished product of pungent and large red Capsorubin finished product;
During described liquefaction processing, the Ye Huamei that adopts is generally α-Dian Fenmei, certainly also can adopt other Ye Huamei, the add-on of Ye Huamei is 1,000,000 of a crushed material weight/to 3/1000000ths, when crushed material is 55~65 ℃ in temperature, under the condition between pH=3~7, liquefied 10~30 minutes;
For reaching better effect of extracting, before capsicum skin liquefaction thing is carried out subcritical abstraction, the entrainment agent in the time of can in capsicum skin liquefaction thing, adding ethanol as extraction, its add-on is 20~30% of capsicum skin liquefaction thing weight;
The CO 2 fluid that contains extract can be adopted the secondary separation method to separate, flash trapping stage is to be 2.5~7MPa at pressure, and temperature is that peppery seed oil precipitation is separated out under 25~35 ℃ the condition; It is to be 2~6MPa at pressure that secondary separates, and temperature is under 30~40 ℃ the condition, successively to isolate the plain and large red Capsorubin of pungent; Also can carry out rectifying to isolated large red Capsorubin, described rectifying is to be 1.5~5MPa at pressure, and temperature is under 30~45 ℃ the large red Capsorubin to be purified;
3) chilli seed of gained is pulverized, the crushed material of gained carries out liquefaction processing earlier, and the liquefaction thing of gained is sent in the extraction kettle and to be fed subcritical CO 2 fluid and extract, and extraction temperature is controlled at 20~30 ℃, pressure is 3~10MPa, and the extraction time is 10~60 minutes; The effusive CO 2 fluid that contains extract enters in the separating still after step-down and separates from extraction kettle, obtain spicy oil, pungent element and orange Capsorubin, then they are concentrated respectively, crystallization, spicy oil finished product, the plain finished product of pungent and orange Capsorubin finished product;
During described liquefaction processing, the Ye Huamei of employing is generally α-Dian Fenmei, also can adopt other Ye Huamei certainly; The add-on of Ye Huamei is 1,000,000 of a crushed material weight/to 3/1000000ths, when crushed material is 55~65 ℃ in temperature, under the condition between pH=3~7, liquefied 10~30 minutes;
For reaching better effect of extracting, before chilli seed liquefaction thing is carried out subcritical carbon dioxide abstraction, the entrainment agent in the time of can in chilli seed liquefies thing, adding ethanol as extraction, its add-on is 20~30% of a chilli seed liquefaction thing weight;
The CO 2 fluid that contains extract can be adopted the secondary separation method to separate, flash trapping stage is to be 2.5~7MPa at pressure, and temperature is that peppery seed oil precipitation is separated out under 25~35 ℃ the condition; It is to be 2~6MPa at pressure that secondary separates, and temperature is under 30~40 ℃ the condition, successively to isolate the plain and orange Capsorubin of pungent; Also can carry out rectifying to isolated orange Capsorubin, described rectifying is to be 1.5~5MPa at pressure, and temperature is under 30~45 ℃ the orange Capsorubin to be purified;
4) getting dried cassava pulverizes, the dried Tapioca Starch of gained minces and carries out liquefaction processing, and the cassava that obtains liquefaction thing filters, and obtains filter pulp and manioc waste, get filter pulp and carry out the saccharification processing, the hydrogen catalysis reaction is carried out in the syrup decolorization of gained, filtration, the filter pulp of gained, and reacted slurries are placed extraction kettle, feeding subcritical CO 2 fluid extracts, extraction temperature is controlled at 20~30 ℃, and pressure is 3~10MPa, and the extraction time is 10~60 minutes; The effusive CO 2 fluid that contains extract enters in the separating still after step-down and separates from extraction kettle, obtains N.F,USP MANNITOL and sorbyl alcohol, again they are concentrated respectively, crystallization, finished product;
During described liquefaction processing, the Ye Huamei of employing is generally α-Dian Fenmei; The add-on of Ye Huamei is 1,000,000 of a gained crushed material weight/to 3/1000000ths, when crushed material is 55~65 ℃ in temperature, under the condition between the pH=5-8, liquefied 10~30 minutes;
When described saccharification was handled, the saccharification catalyzer of employing generally can be saccharifying enzyme and adds isoamylase, and the proportioning of saccharifying enzyme and isoamylase can be arbitrary proportion; The add-on of saccharification catalyzer is that Tapioca Starch minces that 1,000,000 of weight/to 3/1000000ths, saccharification time is 10~30 minutes, and saccharification temperature is 55~65 ℃;
In the described hydrogen catalysis reaction, the consumption of hydrogen is 5/1000ths to 7/1000ths of a filter pulp weight; The catalysis time is 10~30 minutes; Catalytic temperature is 5~30 ℃; Catalysis pressure is 1.5~5MPa;
For reaching better effect of extracting, before the slurries to hydrogen catalysis reaction back gained carry out subcritical abstraction, the entrainment agent in the time of can in the slurries of gained, adding ethanol as extraction, its add-on is 20~30% of a slurry weight;
The CO 2 fluid that will contain extract adopts the secondary separation method to separate, and flash trapping stage is 2.5~7MPa at pressure, and temperature is to isolate N.F,USP MANNITOL under 25~35 ℃ the condition; It is 2~6MPa that secondary is separated in pressure, and temperature is to isolate sorbyl alcohol under 30~40 ℃ the condition; Also can carry out rectifying to isolated N.F,USP MANNITOL, described rectifying is to be 1.5~5MPa at pressure, and temperature is under 30~45 ℃ N.F,USP MANNITOL to be purified;
5) getting dry sweet potato pulverizes, the sweet potato powder of gained minces and carries out liquefaction processing, and the Ipomoea batatas that obtains liquefaction thing filters, and obtains filter pulp and sweet potato waste, get filter pulp and carry out the saccharification processing, the syrup of gained decolours, filters, and the hydrogen catalysis reaction is carried out in the filter pulp of gained again, places extraction kettle at reacted slurries, feed subcritical CO 2 fluid, extraction temperature is controlled at 20~30 ℃, and pressure is 3~10MPa, and the extraction time is 10~60 minutes; The effusive CO 2 fluid that contains extract enters in the separating still after step-down and separates from extraction kettle, obtains N.F,USP MANNITOL and sorbyl alcohol, again they are concentrated respectively, crystallization, finished product;
During described liquefaction processing, the Ye Huamei of employing generally can be α-Dian Fenmei; The add-on of Ye Huamei is 1,000,000 of a gained crushed material weight/to 3/1000000ths, when crushed material is 55~65 ℃ in temperature, under the condition between the pH=5-8, liquefied 10~30 minutes;
When described saccharification was handled, the saccharification catalyzer of employing was saccharifying enzyme+isoamylase, and the proportioning of saccharifying enzyme and isoamylase can be arbitrary proportion; The add-on of saccharification catalyzer is that sweet potato powder minces that 1,000,000 of weight/to 3/1000000ths, saccharification time is 10~30 minutes, and saccharification temperature is 55~65 ℃;
In the described hydrogen catalysis reaction, the consumption of hydrogen is 5/1000ths to 7/1000ths of a filter pulp weight; The catalysis time is 10~30 minutes, and catalytic temperature is 5~30 ℃, and catalysis pressure is 1.5~5MPa;
For reaching better effect of extracting, before the slurries to hydrogen catalysis reaction back gained carry out subcritical abstraction, the entrainment agent in the time of can in the slurries of gained, adding ethanol as extraction, its add-on is 20~30% of a slurry weight;
The CO 2 fluid that will contain extract adopts the secondary separation method to separate, and flash trapping stage is 2.5~7MPa at pressure, and temperature is to isolate N.F,USP MANNITOL under 25~35 ℃ the condition; It is 2~6MPa that secondary is separated in pressure, and temperature is to isolate sorbyl alcohol under 30~40 ℃ the condition; Also can carry out rectifying to isolated N.F,USP MANNITOL, described rectifying is to be 1.5~5MPa at pressure, and temperature is under 30~45 ℃ N.F,USP MANNITOL to be purified;
6) sweet potato waste after the liquefaction thing filters in manioc waste after the liquefaction thing filters in the collection step 4) and the step 5) mixes, the mixture of gained liquefies, saccharification is handled, again the mixture after the saccharification is carried out yeast-inoculated, it is continuously fermented, fermented product to gained carries out centrifugation, obtain liquid and yeast slurry respectively, again the gained liquid filtering is obtained clear liquid and fermentation potato slag, again clear liquid is distilled and obtain aqueous ethanol, then aqueous ethanol is placed extraction kettle to carry out subcritical CO 2 fluid extraction, extraction temperature is controlled at 20~30 ℃, pressure is 3~10MPa, the extraction time is 10~60 minutes, and the effusive CO 2 fluid that contains extract enters in the separating still through step-down from extraction kettle, obtains dehydrated alcohol through separation;
During described liquefaction processing, the Ye Huamei of employing is generally α-Dian Fenmei; The add-on of Ye Huamei is 1,000,000 of a mixture weight/to 3/1000000ths, when mixture is 55~65 ℃ in temperature, under the condition between the pH=5-8, liquefied 10~30 minutes;
When described saccharification was handled, the saccharification catalyzer of employing was saccharifying enzyme+isoamylase; The add-on of saccharification catalyzer be after the liquefaction processing gained liquefaction thing weight 1,000,000/to 3/1000000ths, saccharification time is 10~30 minutes, saccharification temperature is 55~65 ℃;
Mixture after the described saccharification can be used yeast-inoculated, and it is continuously fermented, and leavening temperature is generally 55~60 ℃, pH=5~7, and fermentation time is 8~10 hours; Described yeast can be distiller's yeast yeast arbitrarily, the zymic add-on be after the saccharification mixture weight 10~20%;
Described clear liquid distillatory temperature is 40~90 ℃, and pressure is 0.1~1MPa;
For reaching better effect of extracting, before aqueous ethanol is carried out subcritical abstraction, the entrainment agent in the time of can in aqueous ethanol, adding ethylene glycol as extraction, its add-on is 20~30% of an aqueous ethanol weight;
The described CO 2 fluid that will contain extract is 2.5~7MPa at pressure, and temperature is to isolate dehydrated alcohol under 25~35 ℃ the condition;
7) the pH value with the yeast slurry of gained after the centrifugation in the step 6) transfers to neutrality, then the neutral yeast slurry is placed extraction kettle to carry out subcritical CO 2 fluid extraction, extraction temperature is controlled at 20~30 ℃, pressure is 3~10MPa, the extraction time is 10~60 minutes, the effusive CO 2 fluid that contains extract enters in the separating still through step-down from extraction kettle, obtains Yeast Nucleic Acid and yeast body refuse through separation again;
Described pH value with yeast slurry transfers to neutrality, be that to add down hydrochloric acid or weight concentration be 10~20% dilute sulphuric acid that the pH value of yeast slurry is transferred to neutrality at 40~90 ℃, then the neutral yeast slurry be cooled to 20~30 ℃ and carry out subcritical CO 2 fluid and extract;
For reaching better effect of extracting, before the neutral yeast slurry is carried out subcritical abstraction, the entrainment agent in the time of can in the neutral yeast slurry, adding ethanol as extraction, its add-on is 10~20% of a neutral yeast slurry weight;
The described CO 2 fluid that will contain extract is 2.5~7MPa at pressure, and temperature is to isolate Yeast Nucleic Acid under 25~35 ℃ the condition;
8) collect step 2) in fermentation potato slag after filtering in the residual chilli seed slag in extraction back, the step 6) in the residual capsicum skin slag in extraction back, step 3) and the step 7) yeast body refuse after the extraction mix, drying, obtain mixed fodder;
9) collect the production waste that produces in the above-mentioned steps, enter in the fermentation vat and ferment, enter in the settling tank after the fermentation and precipitate, the throw out of getting the post precipitation gained carries out press filtration, and filter residue enters in the mathane generating pool and ferments, and obtains producing the biogas of usefulness; The liquid of getting the post precipitation gained filters, and sterilization is filtered, and obtains water of productive use.
The extracting method of effective ingredient in capsicum of the present invention, the potato class, be to be raw material with capsicum, Ipomoea batatas, cassava, the employing carbonic acid gas is an extraction solvent, under subcritical state, extract, from capsicum, extract natural effective ingredient Capsorubin, pungent element, spicy oil, from cassava, Ipomoea batatas, extract N.F,USP MANNITOL, sorbyl alcohol, and utilize the remaining residue in extraction back to extract other multiple effective ingredient.With subcritical CO 2 fluid extraction, its operating pressure is lower, flow process is simple, this just greatly reduces the investment of equipment, improve production security, and still can keep the advantage of supercritical fluid extraction, good as environment, need not repeatedly extracting operation etc., and the effective ingredient yield that extracts and purity are all higher.Residue after the extraction can continue to extract dehydrated alcohol, utilize subcritical carbon dioxide solvent to manioc waste, the isolated yeast slurry extracting ribonucleic acid in sweet potato waste fermentation back, also can utilize the residue mixing oven dry after extracting in each step to make mixed fodder, the mixed fodder of gained has immunizing power, the day weight gain that can improve animal, reduces advantages such as feeding cost; In addition, also the factory effluent waste residue that produces in each step is handled, made factory effluent change into water of productive use, the water of productive use of gained can be recycled, and waste water reaches zero release; The waste residue generation biogas that ferments, the biogas of gained is compressed to 162 kg/cm, or be cooled to subzero 160 ℃ and become liquid, just can be purified to biological methane gas, can solve about 70% energy consumption in the heating system in the production process, thereby the trade effluent waste residue is fully used.
(4) embodiment:
Embodiment 1:
1) gets and carry out the skin seed after chilli is pulverized and separate;
2) the capsicum skin of gained is pulverized, in the gained crushed material, add and be equivalent to the millionth α-Dian Fenmei of its weight, when temperature is 55 ℃, under the condition of pH=3, liquefied 30 minutes, in the liquefaction thing of gained, add the entrainment agent of ethanol during be equivalent to its weight 20% as extraction, send into then in the extraction kettle and to feed subcritical CO 2 fluid and extract, extraction temperature is controlled at 30 ℃, and pressure is 10MPa, and the extraction time is 60 minutes; The effusive CO 2 fluid that contains extract enters after step-down and carries out secondary in the separating still and separate from extraction kettle, and flash trapping stage is to be 7MPa at pressure, and temperature is under 35 ℃ the condition peppery seed oil precipitation to be separated out; It is to be 6MPa at pressure that secondary separates, and temperature is under 40 ℃ the condition, successively to isolate the plain and large red Capsorubin of pungent; Then isolated large red Capsorubin is carried out rectifying, described rectifying is to be 5MPa at pressure, temperature is under 45 ℃ the large red Capsorubin to be purified, at last they are concentrated respectively, crystallization, spicy oil finished product, the plain finished product of pungent and large red Capsorubin finished product;
3) chilli seed of gained is pulverized, in the gained crushed material, add the α-Dian Fenmei that is equivalent to its weight 3/1000000ths, in temperature is 65 ℃, under the condition of pH=7, liquefied 10 minutes, in the liquefaction thing of gained, add the entrainment agent of ethanol during be equivalent to its weight 30% then as extraction, send in the extraction kettle and to feed subcritical CO 2 fluid and extract, extraction temperature is controlled at 20 ℃, and pressure is 3MPa, and the extraction time is 60 minutes; The effusive CO 2 fluid that contains extract enters after step-down and carries out secondary in the separating still and separate from extraction kettle, and flash trapping stage is to be 2.5MPa at pressure, and temperature is under 25 ℃ the condition peppery seed oil precipitation to be separated out; It is to be 2MPa at pressure that secondary separates, and temperature is under 30 ℃ the condition, successively to isolate the plain and orange Capsorubin of pungent; Then isolated orange Capsorubin is carried out rectifying, described rectifying is to be 1.5MPa at pressure, temperature is under 35 ℃ the orange Capsorubin to be purified, at last they are concentrated respectively, crystallization, spicy oil finished product, the plain finished product of pungent and orange Capsorubin finished product;
4) getting dried cassava pulverizes, in the dried Tapioca Starch of gained minces, add and be equivalent to the millionth α-Dian Fenmei of its weight, in temperature is 65 ℃, under the condition of pH=5, liquefied 10 minutes, the cassava that obtains liquefaction thing filters, and obtains filter pulp and manioc waste, get filter pulp add saccharifying enzyme and isoamylase as the saccharification catalyzer in 55 ℃ of following saccharification 30 minutes; The add-on of described saccharification catalyzer is Tapioca Starch 1,000,000 of weight/(wherein, the weight proportion between saccharifying enzyme and the isoamylase is 1: 1) of mincing; The hydrogen catalysis reaction is carried out in the syrup decolorization of gained, filtration, the filter pulp of gained, and the catalysis time of described hydrogen catalysis reaction is 30 minutes, and catalytic temperature is 5 ℃, and catalysis pressure is 1.5MPa, and the consumption of hydrogen is 7/1000ths of a filter pulp weight; In the reacted slurries of hydrogen catalysis, add the entrainment agent when quite its weight 20% ethanol is as extraction then, mix and be placed in the extraction kettle, feed subcritical CO 2 fluid and extract, extraction temperature is controlled at 20 ℃, pressure is 3MPa, and the extraction time is 60 minutes; The effusive CO 2 fluid that contains extract enters after step-down and carries out secondary in the separating still and separate from extraction kettle, and flash trapping stage is 2.5MPa at pressure, and temperature is to isolate N.F,USP MANNITOL under 35 ℃ the condition; It is 2MPa that secondary is separated in pressure, and temperature is to isolate sorbyl alcohol under 40 ℃ the condition; Also can carry out rectifying to isolated N.F,USP MANNITOL, described rectifying is to be 1.5MPa at pressure, and temperature is under 45 ℃ N.F,USP MANNITOL to be purified; Again they are concentrated respectively, crystallization, finished product;
5) getting dry sweet potato pulverizes, add during the sweet potato powder of gained minces and be equivalent to the millionth α-Dian Fenmei of its weight, in temperature is 55 ℃, under the condition of pH=8, liquefied 30 minutes, the Ipomoea batatas liquefaction thing that obtains filters, obtain filter pulp and sweet potato waste, get filter pulp add saccharifying enzyme and isoamylase as the saccharification catalyzer in 65 ℃ of following saccharification 10 minutes, the add-on of saccharification catalyzer is mince 3/1000000ths (wherein, the weight proportion between saccharifying enzyme and the isoamylase is 1: 1) of weight of Tapioca Starch; The syrup of gained decolours, filters, and the hydrogen catalysis reaction is carried out in the filter pulp of gained again, and the catalysis time of described hydrogen catalysis reaction is 30 minutes, and catalytic temperature is 30 ℃, and catalysis pressure is 5MPa, and the consumption of hydrogen is 5/1000ths of a filter pulp weight; In the reacted slurries of hydrogen catalysis, add the entrainment agent when quite its weight 20% ethanol is as extraction then, mix and be placed in the extraction kettle, feed subcritical CO 2 fluid, extraction temperature is controlled at 30 ℃, pressure is 3MPa, and the extraction time is 60 minutes; The effusive CO 2 fluid that contains extract enters after step-down and carries out secondary in the separating still and separate from extraction kettle, and flash trapping stage is 2.5MPa at pressure, and temperature is to isolate N.F,USP MANNITOL under 35 ℃ the condition; It is 2MPa that secondary is separated in pressure, and temperature is to isolate sorbyl alcohol under 40 ℃ the condition; Also can carry out rectifying to isolated N.F,USP MANNITOL, described rectifying is to be 1.5MPa at pressure, and temperature is under 45 ℃ N.F,USP MANNITOL to be purified; Again they are concentrated respectively, crystallization, finished product;
6) sweet potato waste after the liquefaction thing filters in manioc waste after the liquefaction thing filters in the collection step 4) and the step 5) mixes, mixture adding at gained is equivalent to the millionth α-Dian Fenmei of its weight, in temperature is 65 ℃, under the condition of pH=8, liquefies 30 minutes; The liquefaction thing that obtains add saccharifying enzyme and isoamylase as the saccharification catalyzer 55 ℃ of following saccharification 30 minutes, the add-on of saccharification catalyzer is mince 3/1000000ths (wherein, the weight proportion between saccharifying enzyme and the isoamylase is 1: 1) of weight of Tapioca Starch; Again the mixture after the saccharification being adopted the distiller's yeast inoculation, is 60 ℃ in temperature, under the condition of pH=5, fermented 8 hours, the add-on of distiller's yeast be after the saccharification mixture weight 10%; Fermented product to gained carries out centrifugation, obtain liquid and yeast slurry respectively, again the gained liquid filtering is obtained clear liquid and fermentation potato slag, again clear liquid is carried out at 1MPa, distillation obtains aqueous ethanol in 40 ℃, in aqueous ethanol, add then and be equivalent to the ethylene glycol of its weight 20% as entrainment agent, mix to be placed on and carry out subcritical CO 2 fluid extraction in the extraction kettle, extraction temperature is controlled at 20 ℃, pressure is 10MPa, the extraction time is 60 minutes, to enter in the separating still at pressure through step-down be 7MPa to the effusive CO 2 fluid that contains extract from extraction kettle, and temperature is under 25 ℃ the condition, to obtain dehydrated alcohol through separation;
7) yeast slurry with gained after the centrifugation in the step 6) adds hydrochloric acid down at 40 ℃, its pH value is transferred to neutrality, neutral yeast slurry with gained is cooled to 20 ℃ again, and adding is equivalent to the ethanol of its weight 20% as entrainment agent in the neutral yeast slurry, place extraction kettle to carry out subcritical CO 2 fluid extraction then, extraction temperature is controlled at 30 ℃, pressure is 3MPa, the extraction time is 60 minutes, the effusive CO 2 fluid that contains extract enters in the separating still through step-down from extraction kettle, at pressure is 2.5MPa, and temperature is to separate under 35 ℃ the condition to obtain Yeast Nucleic Acid and yeast body refuse;
8) collect step 2) in fermentation potato slag after filtering in the residual chilli seed slag in extraction back, the step 6) in the residual capsicum skin slag in extraction back, step 3) and the step 7) yeast body refuse after the extraction mix, in 98 ℃ of oven dry, obtain mixed fodder;
9) collect the production waste that produces in the above-mentioned steps, enter in the fermentation vat and ferment, enter in the settling tank after the fermentation and precipitate, the throw out of getting the post precipitation gained adopts pressure filter to carry out press filtration, and filter residue enters in the mathane generating pool and ferments, and obtains producing the biogas of usefulness; The liquid of getting the post precipitation gained filters, and sterilization is filtered, and obtains water of productive use.
Embodiment 2:
1) gets and carry out the skin seed after chilli is pulverized and separate;
2) the capsicum skin of gained is pulverized, in the gained crushed material, add the α-Dian Fenmei that is equivalent to its weight 3/1000000ths, when temperature is 65 ℃, under the condition of pH=7, liquefied 10 minutes, the liquefaction thing of gained is sent in the extraction kettle and to be fed subcritical CO 2 fluid and extract, and extraction temperature is controlled at 20 ℃, pressure is 3MPa, and the extraction time is 10 minutes; The effusive CO 2 fluid that contains extract enters after step-down and carries out secondary in the separating still and separate from extraction kettle, and flash trapping stage is to be 2.5MPa at pressure, and temperature is under 25 ℃ the condition peppery seed oil precipitation to be separated out; It is to be 2MPa at pressure that secondary separates, and temperature is under 30 ℃ the condition, successively to isolate the plain and large red Capsorubin of pungent; And then isolated large red Capsorubin carries out rectifying, described rectifying is to be 1.5MPa at pressure, temperature is under 35 ℃ the large red Capsorubin to be purified, then they are concentrated respectively, crystallization, spicy oil finished product, the plain finished product of pungent and large red Capsorubin finished product;
3) chilli seed of gained is pulverized, in the gained crushed material, add and be equivalent to the millionth α-Dian Fenmei of its weight, in temperature is 55 ℃, under the condition of pH=3, liquefied 30 minutes, the liquefaction thing of gained is sent in the extraction kettle and to be fed subcritical CO 2 fluid and extract, and extraction temperature is controlled at 30 ℃, pressure is 10MPa, and the extraction time is 10 minutes; The effusive CO 2 fluid that contains extract enters after step-down and carries out secondary in the separating still and separate from extraction kettle, and flash trapping stage is to be 7MPa at pressure, and temperature is under 35 ℃ the condition peppery seed oil precipitation to be separated out; It is to be 6MPa at pressure that secondary separates, and temperature is under 40 ℃ the condition, successively to isolate the plain and orange Capsorubin of pungent; Then isolated orange Capsorubin is carried out rectifying, described rectifying is to be 5MPa at pressure, temperature is under 45 ℃ the orange Capsorubin to be purified, then they are concentrated respectively, crystallization, spicy oil finished product, the plain finished product of pungent and orange Capsorubin finished product;
4) getting dried cassava pulverizes, in mincing, the dried Tapioca Starch of gained adds the α-Dian Fenmei that is equivalent to its weight 3/1000000ths, in temperature is 55 ℃, under the condition of pH=8, liquefied 30 minutes, the cassava that obtains liquefaction thing filters, and obtains filter pulp and manioc waste, get filter pulp add saccharifying enzyme and isoamylase as the saccharification catalyzer in 65 ℃ of following saccharification 10 minutes; The add-on of described saccharification catalyzer is mince 3/1000000ths (wherein, the weight proportion between saccharifying enzyme and the isoamylase is 1: 1) of weight of Tapioca Starch; The hydrogen catalysis reaction is carried out in the syrup decolorization of gained, filtration, the filter pulp of gained, and the catalysis time of described hydrogen catalysis reaction is 10 minutes, and catalytic temperature is 30 ℃, and catalysis pressure is 5MPa, and the consumption of hydrogen is 5/1000ths of a filter pulp weight; Then the reacted slurries of hydrogen catalysis are placed extraction kettle, feed subcritical CO 2 fluid and extract, extraction temperature is controlled at 30 ℃, and pressure is 10MPa, and the extraction time is 10 minutes; The effusive CO 2 fluid that contains extract enters after step-down and carries out secondary in the separating still and separate from extraction kettle, and flash trapping stage is 7MPa at pressure, and temperature is to isolate N.F,USP MANNITOL under 35 ℃ the condition; It is 6MPa that secondary is separated in pressure, and temperature is to isolate sorbyl alcohol under 40 ℃ the condition; Also can carry out rectifying to isolated N.F,USP MANNITOL, described rectifying is to be 5MPa at pressure, and temperature is under 45 ℃ N.F,USP MANNITOL to be purified; Again they are concentrated respectively, crystallization, finished product;
5) getting dry sweet potato pulverizes, during mincing, the sweet potato powder of gained adds the α-Dian Fenmei that is equivalent to its weight 3/1000000ths, in temperature is 65 ℃, under the condition of pH=5, liquefied 10 minutes, the Ipomoea batatas liquefaction thing that obtains filters, obtain filter pulp and sweet potato waste, get filter pulp add saccharifying enzyme and isoamylase as the saccharification catalyzer in 55 ℃ of following saccharification 30 minutes, the add-on of saccharification catalyzer is Tapioca Starch 1,000,000 of weight/(wherein, the weight proportion between saccharifying enzyme and the isoamylase is 1: 1) of mincing; The syrup of gained decolours, filters, and the hydrogen catalysis reaction is carried out in the filter pulp of gained again, and the catalysis time of described hydrogen catalysis reaction is 10 minutes, and catalytic temperature is 5 ℃, and catalysis pressure is 1.5MPa, and the consumption of hydrogen is 7/1000ths of a filter pulp weight; The reacted slurries of hydrogen catalysis place extraction kettle, feed subcritical CO 2 fluid, and extraction temperature is controlled at 20 ℃, and pressure is 10MPa, and the extraction time is 10 minutes; The effusive CO 2 fluid that contains extract enters after step-down and carries out secondary in the separating still and separate from extraction kettle, and flash trapping stage is 7MPa at pressure, and temperature is to isolate N.F,USP MANNITOL under 25 ℃ the condition; It is 6MPa that secondary is separated in pressure, and temperature is to isolate sorbyl alcohol under 30 ℃ the condition; Also can carry out rectifying to isolated N.F,USP MANNITOL, described rectifying is to be 5MPa at pressure, and temperature is under 35 ℃ N.F,USP MANNITOL to be purified; Again they are concentrated respectively, crystallization, finished product;
6) sweet potato waste after the liquefaction thing filters in manioc waste after the liquefaction thing filters in the collection step 4) and the step 5) mixes, mixture at gained adds the α-Dian Fenmei that is equivalent to its weight 3/1000000ths, in temperature is 55 ℃, under the condition of pH=5, liquefies 10 minutes; The liquefaction thing that obtains add saccharifying enzyme and isoamylase as the saccharification catalyzer 65 ℃ of following saccharification 10 minutes, the add-on of saccharification catalyzer is Tapioca Starch 1,000,000 of weight/(wherein, the weight proportion between saccharifying enzyme and the isoamylase is 1: 1) of mincing; Again the mixture after the saccharification being adopted the distiller's yeast inoculation, is 55 ℃ in temperature, under the condition of pH=7, fermented 10 hours, the add-on of distiller's yeast be after the saccharification mixture weight 20%; Fermented product to gained carries out centrifugation, obtain liquid and yeast slurry respectively, again the gained liquid filtering is obtained clear liquid and fermentation potato slag, again clear liquid distillation in 0.1MPa, 90 ℃ is obtained aqueous ethanol, then aqueous ethanol is placed extraction kettle to carry out subcritical CO 2 fluid extraction, extraction temperature is controlled at 30 ℃, pressure is 3MPa, the extraction time is 10 minutes, to enter in the separating still at pressure through step-down be 2.5MPa to the effusive CO 2 fluid that contains extract from extraction kettle, temperature is under 35 ℃ the condition, to obtain dehydrated alcohol through separation;
7) with the yeast slurry of gained after the centrifugation in the step 6) under 90 ℃, be that 10% dilute sulphuric acid transfers to neutrality with its pH value with weight concentration, neutral yeast slurry with gained is cooled to 30 ℃ again, place extraction kettle to carry out subcritical CO 2 fluid extraction then, extraction temperature is controlled at 20 ℃, pressure is 10MPa, the extraction time is 10 minutes, the effusive CO 2 fluid that contains extract enters in the separating still through step-down from extraction kettle, at pressure is 7MPa, and temperature is to separate under 25 ℃ the condition to obtain Yeast Nucleic Acid and yeast body refuse;
8) collect step 2) in fermentation potato slag after filtering in the residual chilli seed slag in extraction back, the step 6) in the residual capsicum skin slag in extraction back, step 3) and the step 7) yeast body refuse after the extraction mix, in 98 ℃ of oven dry, obtain mixed fodder;
9) collect the production waste that produces in the above-mentioned steps, enter in the fermentation vat and ferment, enter in the settling tank after the fermentation and precipitate, the throw out of getting the post precipitation gained adopts pressure filter to carry out press filtration, and filter residue enters in the mathane generating pool and ferments, and obtains producing the biogas of usefulness; The liquid of getting the post precipitation gained filters, and sterilization is filtered, and obtains water of productive use.

Claims (10)

1, the extracting method of effective ingredient in capsicum, the potato class, its step is as follows:
1) gets and carry out the skin seed after chilli is pulverized and separate;
2) the capsicum skin of gained is pulverized, the gained crushed material carries out liquefaction processing, and the liquefaction thing of gained is sent in the extraction kettle and to be fed subcritical CO 2 fluid and extract, and extraction temperature is controlled at 20~30 ℃, pressure is 3~10MPa, and the extraction time is 10~60 minutes; The effusive CO 2 fluid that contains extract enters in the separating still after step-down and separates from extraction kettle, obtain spicy oil, pungent element and large red Capsorubin, then they are concentrated respectively, crystallization, spicy oil finished product, the plain finished product of pungent and large red Capsorubin finished product;
3) chilli seed of gained is pulverized, the crushed material of gained carries out liquefaction processing earlier, and the liquefaction thing of gained is sent in the extraction kettle and to be fed subcritical CO 2 fluid and extract, and extraction temperature is controlled at 20~30 ℃, pressure is 3~10MPa, and the extraction time is 10~60 minutes; The effusive CO 2 fluid that contains extract enters in the separating still after step-down and separates from extraction kettle, obtain spicy oil, pungent element and orange Capsorubin, then they are concentrated respectively, crystallization, spicy oil finished product, the plain finished product of pungent and orange Capsorubin finished product;
4) getting dried cassava pulverizes, the dried Tapioca Starch of gained minces and carries out liquefaction processing, and the cassava that obtains liquefaction thing filters, and obtains filter pulp and manioc waste, get filter pulp and carry out the saccharification processing, the hydrogen catalysis reaction is carried out in the syrup decolorization of gained, filtration, the filter pulp of gained, and reacted slurries are placed extraction kettle, feeding subcritical CO 2 fluid extracts, extraction temperature is controlled at 20~30 ℃, and pressure is 3~10MPa, and the extraction time is 10~60 minutes; The effusive CO 2 fluid that contains extract enters in the separating still after step-down and separates from extraction kettle, obtains N.F,USP MANNITOL and sorbyl alcohol, again they are concentrated respectively, crystallization, finished product;
5) getting dry sweet potato pulverizes, the sweet potato powder of gained minces and carries out liquefaction processing, and the Ipomoea batatas that obtains liquefaction thing filters, and obtains filter pulp and sweet potato waste, get filter pulp and carry out the saccharification processing, the syrup of gained decolours, filters, and the hydrogen catalysis reaction is carried out in the filter pulp of gained again, places extraction kettle at reacted slurries, feed subcritical CO 2 fluid, extraction temperature is controlled at 20~30 ℃, and pressure is 3~10MPa, and the extraction time is 10~60 minutes; The effusive CO 2 fluid that contains extract enters in the separating still after step-down and separates from extraction kettle, obtains N.F,USP MANNITOL and sorbyl alcohol, again they are concentrated respectively, crystallization, finished product;
6) sweet potato waste after the liquefaction thing filters in manioc waste after the liquefaction thing filters in the collection step 4) and the step 5) mixes, the mixture of gained liquefies, saccharification is handled, again the mixture after the saccharification is carried out yeast-inoculated, it is continuously fermented, fermented product to gained carries out centrifugation, obtain liquid and yeast slurry respectively, again the gained liquid filtering is obtained clear liquid and fermentation potato slag, again clear liquid is distilled and obtain aqueous ethanol, then aqueous ethanol is placed extraction kettle to carry out subcritical CO 2 fluid extraction, extraction temperature is controlled at 20~30 ℃, pressure is 3~10MPa, the extraction time is 10~60 minutes, and the effusive CO 2 fluid that contains extract enters in the separating still through step-down from extraction kettle, obtains dehydrated alcohol through separation;
7) the pH value with the yeast slurry of gained after the centrifugation in the step 6) transfers to neutrality, then the neutral yeast slurry is placed extraction kettle to carry out subcritical CO 2 fluid extraction, extraction temperature is controlled at 20~30 ℃, pressure is 3~10MPa, the extraction time is 10~60 minutes, the effusive CO 2 fluid that contains extract enters in the separating still through step-down from extraction kettle, obtains Yeast Nucleic Acid and yeast body refuse through separation again;
8) collect step 2) in fermentation potato slag after filtering in the residual chilli seed slag in extraction back, the step 6) in the residual capsicum skin slag in extraction back, step 3) and the step 7) yeast body refuse after the extraction mix, drying, obtain mixed fodder;
9) collect the production waste that produces in the above-mentioned steps, enter in the fermentation vat and ferment, enter in the settling tank after the fermentation and precipitate, the throw out of getting the post precipitation gained carries out press filtration, and filter residue enters in the mathane generating pool and ferments, and obtains producing the biogas of usefulness; The liquid of getting the post precipitation gained filters, and sterilization is filtered, and obtains water of productive use.
2, the extracting method of effective ingredient in capsicum according to claim 1, the potato class is characterized in that: step 2) and step 3) in, during described liquefaction processing, the Ye Huamei of employing is a α-Dian Fenmei; The add-on of Ye Huamei is 1,000,000 of a crushed material weight/to 3/1000000ths, be when temperature is 55~65 ℃, under the condition between pH=3~7, liquefies 10~30 minutes.
3, the extracting method of effective ingredient in capsicum according to claim 1 and 2, the potato class, it is characterized in that: step 2) in, the CO 2 fluid that will contain extract adopts the secondary separation method to separate, flash trapping stage is to be 2.5~7MPa at pressure, and temperature is that peppery seed oil precipitation is separated out under 25~35 ℃ the condition; It is to be 2~6MPa at pressure that secondary separates, and temperature is under 30~40 ℃ the condition, successively to isolate the plain and large red Capsorubin of pungent.
4, the extracting method of effective ingredient in capsicum according to claim 1 and 2, the potato class, it is characterized in that: in the step 3), the CO 2 fluid that will contain extract adopts the secondary separation method to separate, flash trapping stage is to be 2.5~7MPa at pressure, and temperature is that peppery seed oil precipitation is separated out under 25~35 ℃ the condition; It is to be 2~6MPa at pressure that secondary separates, and temperature is successively to isolate the plain and orange Capsorubin of pungent under 30~40 ℃ the condition.
5, the extracting method of effective ingredient in capsicum according to claim 1 and 2, the potato class is characterized in that: in step 4), step 5), the step 6), during described liquefaction processing, the Ye Huamei of employing is a α-Dian Fenmei; The add-on of Ye Huamei is 1,000,000 of a gained crushed material weight/to 3/1000000ths, be when temperature is 55~65 ℃, under the condition between the pH=5-8, liquefies 10~30 minutes.
6, the extracting method of effective ingredient in capsicum according to claim 1 and 2, the potato class is characterized in that: in step 4), step 5), the step 6), when described saccharification was handled, the saccharification catalyzer of employing was saccharifying enzyme+isoamylase; The add-on of saccharification catalyzer is that Tapioca Starch minces that 1,000,000 of weight/to 3/1000000ths, saccharification time is 10~30 minutes, and saccharification temperature is 55~65 ℃.
7, the extracting method of effective ingredient in capsicum according to claim 1 and 2, the potato class is characterized in that: in step 4) and the step 5), in the described hydrogen catalysis reaction, the consumption of hydrogen is 5/1000ths to 7/1000ths of a filter pulp weight; The catalysis time is 10~30 minutes; Catalytic temperature is 5~30 ℃; Catalysis pressure is 1.5~5MPa.
8, the extracting method of effective ingredient in capsicum according to claim 1 and 2, the potato class, it is characterized in that: in the step 4), the CO 2 fluid that will contain extract adopts the secondary separation method to separate, flash trapping stage is 2.5~7MPa at pressure, and temperature is to isolate N.F,USP MANNITOL under 25~35 ℃ the condition; It is 2~6MPa that secondary is separated in pressure, and temperature is to isolate sorbyl alcohol under 30~40 ℃ the condition.
9, the extracting method of effective ingredient in capsicum according to claim 1 and 2, the potato class, it is characterized in that: in the step 5), the CO 2 fluid that will contain extract adopts the secondary separation method to separate, flash trapping stage is 2.5~7MPa at pressure, and temperature is to isolate N.F,USP MANNITOL under 25~35 ℃ the condition; It is 2~6MPa that secondary is separated in pressure, and temperature is to isolate sorbyl alcohol under 30~40 ℃ the condition.
10, the extracting method of effective ingredient in capsicum according to claim 1 and 2, the potato class, it is characterized in that: in the step 6), mixture yeast-inoculated after the described saccharification, it is continuously fermented, leavening temperature is 55~60 ℃, pH=5~7, fermentation time are 8~10 hours, the zymic add-on be after the saccharification mixture weight 10~20%.
CN200710049323A 2007-06-13 2007-06-13 Method for extracting effective component in capsicum and potatos Expired - Fee Related CN100590187C (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102614308A (en) * 2012-04-13 2012-08-01 中国农业大学 Method for extracting bioactivator in hot chili residue through subcritical water
CN107057855A (en) * 2017-01-13 2017-08-18 河南工业大学 A kind of ultrasound removal is subcritical to produce the residual molten method of giving off a strong fragrance chilli seed crude oil
CN108939610A (en) * 2018-07-21 2018-12-07 安溪县凤城建金产品外观设计服务中心 The efficient extraction process of effective component in a kind of Primula obconica Hance

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102614308A (en) * 2012-04-13 2012-08-01 中国农业大学 Method for extracting bioactivator in hot chili residue through subcritical water
CN102614308B (en) * 2012-04-13 2013-10-16 中国农业大学 Method for extracting bioactivator in hot chili residue through subcritical water
CN107057855A (en) * 2017-01-13 2017-08-18 河南工业大学 A kind of ultrasound removal is subcritical to produce the residual molten method of giving off a strong fragrance chilli seed crude oil
CN108939610A (en) * 2018-07-21 2018-12-07 安溪县凤城建金产品外观设计服务中心 The efficient extraction process of effective component in a kind of Primula obconica Hance

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