CN103173285A - Method and device for extracting active ingredients from orange peels through utilizing high-pressure solvent - Google Patents
Method and device for extracting active ingredients from orange peels through utilizing high-pressure solvent Download PDFInfo
- Publication number
- CN103173285A CN103173285A CN2013100553378A CN201310055337A CN103173285A CN 103173285 A CN103173285 A CN 103173285A CN 2013100553378 A CN2013100553378 A CN 2013100553378A CN 201310055337 A CN201310055337 A CN 201310055337A CN 103173285 A CN103173285 A CN 103173285A
- Authority
- CN
- China
- Prior art keywords
- orange peel
- extractor
- extraction
- solvent
- effective constituent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002904 solvent Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000004480 active ingredient Substances 0.000 title abstract description 5
- 238000000605 extraction Methods 0.000 claims abstract description 47
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 239000000470 constituent Substances 0.000 claims description 38
- 238000001704 evaporation Methods 0.000 claims description 38
- 230000008020 evaporation Effects 0.000 claims description 37
- 238000009833 condensation Methods 0.000 claims description 26
- 230000005494 condensation Effects 0.000 claims description 26
- 239000000284 extract Substances 0.000 claims description 23
- 238000012546 transfer Methods 0.000 claims description 19
- 238000000638 solvent extraction Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000010298 pulverizing process Methods 0.000 claims description 8
- 238000011084 recovery Methods 0.000 claims description 6
- 239000002893 slag Substances 0.000 claims description 6
- 238000012856 packing Methods 0.000 claims description 5
- 239000000498 cooling water Substances 0.000 claims description 4
- 230000008719 thickening Effects 0.000 claims description 4
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract 1
- 239000003960 organic solvent Substances 0.000 description 5
- 241000207199 Citrus Species 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 3
- 235000020971 citrus fruits Nutrition 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000001100 (2S)-5,7-dihydroxy-2-(3-hydroxy-4-methoxyphenyl)chroman-4-one Substances 0.000 description 2
- 229930003935 flavonoid Natural products 0.000 description 2
- -1 flavonoid compounds Chemical class 0.000 description 2
- 235000017173 flavonoids Nutrition 0.000 description 2
- ARGKVCXINMKCAZ-UHFFFAOYSA-N neohesperidine Natural products C1=C(O)C(OC)=CC=C1C1OC2=CC(OC3C(C(O)C(O)C(CO)O3)OC3C(C(O)C(O)C(C)O3)O)=CC(O)=C2C(=O)C1 ARGKVCXINMKCAZ-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000001256 steam distillation Methods 0.000 description 2
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 241000675108 Citrus tangerina Species 0.000 description 1
- QUQPHWDTPGMPEX-UHFFFAOYSA-N Hesperidine Natural products C1=C(O)C(OC)=CC=C1C1OC2=CC(OC3C(C(O)C(O)C(COC4C(C(O)C(O)C(C)O4)O)O3)O)=CC(O)=C2C(=O)C1 QUQPHWDTPGMPEX-UHFFFAOYSA-N 0.000 description 1
- OBIOZWXPDBWYHB-UHFFFAOYSA-N Nobiletin Natural products C1=CC(OC)=CC=C1C1=C(OC)C(=O)C2=C(OC)C(OC)=C(OC)C(OC)=C2O1 OBIOZWXPDBWYHB-UHFFFAOYSA-N 0.000 description 1
- 241001093501 Rutaceae Species 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- QUQPHWDTPGMPEX-UTWYECKDSA-N aurantiamarin Natural products COc1ccc(cc1O)[C@H]1CC(=O)c2c(O)cc(O[C@@H]3O[C@H](CO[C@@H]4O[C@@H](C)[C@H](O)[C@@H](O)[C@H]4O)[C@@H](O)[C@H](O)[C@H]3O)cc2O1 QUQPHWDTPGMPEX-UTWYECKDSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000009084 cardiovascular function Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- APSNPMVGBGZYAJ-GLOOOPAXSA-N clematine Natural products COc1cc(ccc1O)[C@@H]2CC(=O)c3c(O)cc(O[C@@H]4O[C@H](CO[C@H]5O[C@@H](C)[C@H](O)[C@@H](O)[C@H]5O)[C@@H](O)[C@H](O)[C@H]4O)cc3O2 APSNPMVGBGZYAJ-GLOOOPAXSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 210000000750 endocrine system Anatomy 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- AIONOLUJZLIMTK-AWEZNQCLSA-N hesperetin Chemical compound C1=C(O)C(OC)=CC=C1[C@H]1OC2=CC(O)=CC(O)=C2C(=O)C1 AIONOLUJZLIMTK-AWEZNQCLSA-N 0.000 description 1
- AIONOLUJZLIMTK-UHFFFAOYSA-N hesperetin Natural products C1=C(O)C(OC)=CC=C1C1OC2=CC(O)=CC(O)=C2C(=O)C1 AIONOLUJZLIMTK-UHFFFAOYSA-N 0.000 description 1
- 229960001587 hesperetin Drugs 0.000 description 1
- 235000010209 hesperetin Nutrition 0.000 description 1
- VUYDGVRIQRPHFX-UHFFFAOYSA-N hesperidin Natural products COc1cc(ccc1O)C2CC(=O)c3c(O)cc(OC4OC(COC5OC(O)C(O)C(O)C5O)C(O)C(O)C4O)cc3O2 VUYDGVRIQRPHFX-UHFFFAOYSA-N 0.000 description 1
- QUQPHWDTPGMPEX-QJBIFVCTSA-N hesperidin Chemical compound C1=C(O)C(OC)=CC=C1[C@H]1OC2=CC(O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO[C@H]4[C@@H]([C@H](O)[C@@H](O)[C@H](C)O4)O)O3)O)=CC(O)=C2C(=O)C1 QUQPHWDTPGMPEX-QJBIFVCTSA-N 0.000 description 1
- 229940025878 hesperidin Drugs 0.000 description 1
- FTODBIPDTXRIGS-UHFFFAOYSA-N homoeriodictyol Natural products C1=C(O)C(OC)=CC(C2OC3=CC(O)=CC(O)=C3C(=O)C2)=C1 FTODBIPDTXRIGS-UHFFFAOYSA-N 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- ARGKVCXINMKCAZ-UZRWAPQLSA-N neohesperidin Chemical compound C1=C(O)C(OC)=CC=C1[C@H]1OC2=CC(O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O3)O[C@H]3[C@@H]([C@H](O)[C@@H](O)[C@H](C)O3)O)=CC(O)=C2C(=O)C1 ARGKVCXINMKCAZ-UZRWAPQLSA-N 0.000 description 1
- MRIAQLRQZPPODS-UHFFFAOYSA-N nobiletin Chemical compound C1=C(OC)C(OC)=CC=C1C1=CC(=O)C2=C(OC)C(OC)=C(OC)C(OC)=C2O1 MRIAQLRQZPPODS-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 229930000044 secondary metabolite Natural products 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Landscapes
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a method and a device for extracting active ingredients from orange peels through utilizing a high-pressure solvent. The method comprises the following steps: drying fresh orange peels, then crushing the dried orange peels through a crusher, and extracting the orange peels through 75% ethanol by utilizing an extracting device, wherein extraction is carried out under the conditions of the extraction temperature of 85-95 DEG C, the extraction pressure of 4-7Mpa, the separation temperature of 80-85 DEG C and the extraction time of 1-2hours. By utilizing the method, the active ingredients of the orange peels can be completely extracted, and the method is quick in extraction speed, small in solvent usage and low in energy consumption. The extracting device disclosed by the invention is simple to operate, low in manufacturing cost and contributed to large-scale production popularization.
Description
Technical field
The invention belongs to the plant extract separation technology field, in particular to a kind of method and device that utilizes effective constituent in high pressure solvent extraction orange peel.
Background technology
Citrus is rutaceae, is most important commodity fruit in the world.Citrus peel is medically claiming dried orange peel, except containing abundant perfume oil, pectin, pigment, also contains the flavonoid compounds such as Hesperidin, neohesperidin, hesperetin, Nobiletin, dihydro river dried orange peel in orange peel.Flavonoid compound is that plant is through the secondary metabolite of a large class plant of photosynthesis generation, as a kind of functional component, that its Main Function has is antitumor, delay senility, strengthen cardiovascular function, strengthening immunity, conciliation endocrine system, protect liver, anti-inflammatory, antianaphylaxis, antibacterial, antiviral etc.China is citrus big producing country, and cultivated area is large, and output is high, and tangerine peel except part is used for Chinese medicine and food-processing, has sizable part also not to be developed and to be dropped every year at present, has both caused the waste of resource, also causes the pollution of environment.
The method of extracting now effective constituent in orange peel has the methods such as steam distillation, organic solvent extractionprocess, cold-press, supercritical carbon dioxide extraction method.Steam distillation wherein, cold-press can only extract the fragrant oily substance in orange peel, and it is extremely low that product goes out rate.Supercritical carbon dioxide extraction method is to generally acknowledge at present more satisfactory Technology to have the effective constituent do not destroyed, and yield is high, the characteristics of product with stable quality, but exists equipment price expensive, and the shortcoming that cost of manufacture is high can't large-scale production.Traditional organic solvent extractionprocess the effective constituent in orange peel all can be extracted, but the method need to consume a large amount of solvents, and correspondingly evaporation concentration link energy consumption is huge the later stage, and also there are the shortcomings such as extraction efficiency is low, extraction time is long in this method simultaneously.
Summary of the invention
In view of the deficiencies in the prior art, the object of the present invention is to provide a kind of novel process of utilizing effective constituent in high pressure solvent extraction orange peel, the extraction element that relates to this technique is provided simultaneously.
In order to realize purpose of the present invention, the contriver studies and explores by lot of experiments, has finally obtained following technical scheme:
A kind of device that utilizes effective constituent in high pressure solvent extraction orange peel, it comprises extractor, evaporation concentration and condensation combined column, solvent transfer tank and volumetric pump, be connected the bottom and be connected in the top of extractor with the condensation combined column with evaporation concentration, evaporation concentration is connected top and is connected with the top of solvent transfer tank with the condensation combined column, the bottom of solvent transfer tank is connected by volumetric pump and extractor, forms circulation line; The bottom outer wall of extractor outer wall, evaporation concentration and condensation combined column is provided with steam circulating device, and the external wall of upper portion of evaporation concentration and condensation combined column is provided with cooling water circulating device, and extractor is provided with regulator.
A kind of method of utilizing effective constituent in high pressure solvent extraction orange peel, its step is as follows:
(1) with fresh orange peel oven dry, pulverizer is pulverized;
Then the material of (2) packing into and crushing in airtight extractor adds 75% ethanol, and the temperature that extractor is kept in heating is 85-95 ℃, and the pressure of controlling simultaneously extractor is 4-7Mpa, extracts 1-2h, after separation extracting solution;
(3) 80-85 ℃ of concentrated extracting solution, get the orange peel extract.
The above-mentioned method of utilizing effective constituent in high pressure solvent extraction orange peel, wherein in step (1), fresh orange peel is dried under 55-60 ℃, crosses 20 eye mesh screens after pulverizing with pulverizer.
The above-mentioned method of utilizing effective constituent in high pressure solvent extraction orange peel, wherein in step (2), the temperature of extractor is 90 ℃, pressure is 5Mpa.
The above-mentioned method of utilizing effective constituent in high pressure solvent extraction orange peel, wherein in step (3), the temperature of concentrated extracting solution is preferably 85 ℃.
A kind of method of extracting effective constituent in orange peel according to said apparatus is characterized in that comprising the steps:
(1) with fresh orange peel oven dry, pulverizer is pulverized;
(2) extractor is filled the material that crushes, open volumetric pump, utilize volumetric pump by squeezing into 75% ethanol to extractor in solvent transfer tank, by steam circulating device, extractor and evaporation concentration and condensation combined column are heated simultaneously, make the extraction temperature of extractor maintain 85-95 ℃, the thickening temperature of evaporation concentration and condensation combined column maintains 80-85 ℃, controls regulator and makes the extracting pressure of extractor maintain 4-7Mpa, dynamic extraction 1-2h;
(3) after extraction finishes, close volumetric pump, open the regulator pressure release, continue the extractor recovery solvent of heating, during solvent-free outflow, the steam off circulation device releases the orange peel slag to evaporation concentration and the condensing tower;
(4) must contain the extract of orange peel effective constituent from evaporation concentration and condensation combined column bottom.
The method of effective constituent in the said extracted orange peel, wherein in step (1), fresh orange peel is dried under 55-60 ℃, crosses 20 eye mesh screens after pulverizing with pulverizer.
The method of effective constituent in the said extracted orange peel, wherein in step (2), the extraction temperature of extractor is 90 ℃, extracting pressure is 5Mpa.
The method of effective constituent in the said extracted orange peel, the extraction time that wherein extracts orange peel in step (2) is preferably 90Min.
The method of effective constituent in the said extracted orange peel, wherein in step (2), the thickening temperature of evaporation concentration and condensation combined column is preferably 85 ℃.
The present invention extracts that in orange peel, the principle of effective constituent is: with the temperature higher than solvent boiling point, solvent is heated, control simultaneously the pressure of solvent, make solvent still keep liquid state at this temperature.Unexpectedly, solvent phase ratio under solvent under high pressure conditions and normal pressure, both can higher dissolving power be arranged to effective constituent in material, its mass transfer and diffusibility also improve a lot, can be more effectively and quickly separation and Extraction is out from material effective constituent.
Extraction element involved in the present invention mainly is comprised of extractor, solvent transfer tank, evaporation concentration and condensation combined column and volumetric pump four parts.Whole leaching process all carries out in closed environment, avoided the injury of organic solvent to human body, evaporation concentration equipment and condensing equipment are merged into a set of equipment, reduced the input of taking up an area space and equipment, utilize solvent transfer tank that solvent cycle is reused, reduced the consumption of solvent and unnecessary waste.
In high pressure solvent extraction orange peel of the present invention, the technique of effective constituent and device are compared with conventional organic solvent extractionprocess and device, have following advantage:
(1) more complete to the extracts active ingredients in orange peel, extraction rate is faster.
(2) extraction solvent recycle, solvent load is little, and energy consumption is low.
(3) extraction element is simple to operate, and equipment manufacturing cost is low.
(4) be not only applicable to the extraction of effective constituent in orange peel, can also change the extraction that solvent is used for other active ingredient of natural plant simultaneously, be very beneficial for the popularization of large-scale production.
Description of drawings
Figure is the device schematic diagram that the present invention extracts effective constituent in orange peel; Wherein: 1-extractor, 2-evaporation concentration and condensation combined column, 3-solvent transfer tank, 4-volumetric pump.
Embodiment
Below in conjunction with accompanying drawing, technique of the present invention and working method are further elaborated:
with fresh orange peel under 55-60 ℃ the oven dry after, pulverized 20 eye mesh screens with pulverizer, pack into after crushing extractor 1. in, 75% ethanol by solvent transfer tank 3. the top valve pour into, add-on accounts for 90% of transfer tank volume, close extractor and be connected the relief valve that is connected with evaporation concentration with the condensation combined column, open volumetric pump 4., solvent in solvent transfer tank is pumped into by below extractor, open simultaneously the steam valve of extractor and evaporation concentration and condensation combined column bottom, open the cooling water valve on evaporation concentration and condensation combined column top, the steam regulation valve, make the extractor temperature maintain 85-95 ℃, evaporation concentration tower temperature maintains 80-85 ℃, controlling relief valve makes extractor pressure maintain 4-7Mpa, flow into evaporation concentration and condensation combined column with the solvent of orange peel effective constituent by the extractor upper end with this understanding, heat by steam, the solvent vaporization separates with the orange peel extract, solvent after vaporization rises to evaporation concentration and condensation combined column top, be back in solvent transfer tank after becoming liquid state by water quench, continuing to pump into extractor by volumetric pump recycles, after extraction finishes, close volumetric pump, open the relief valve pressure release fully, continuation is to the extractor recovery solvent of heating, when observing in condensing tower solvent-free outflow by form, steam off valve and cooling water valve, opening extractor releases the orange peel slag.Valve below unlatching evaporation concentration and condensation combined column picks out the orange peel extract with accepting bucket.
Embodiment 1
Fresh orange peel is dried under 55 ℃, cross 20 eye mesh screens after pulverizing with pulverizer.Get the 2500g material extractor of packing into, open volumetric pump, utilize volumetric pump by squeezing into 75% ethanol to extractor in solvent transfer tank, opening simultaneously steam valve heats to extractor and evaporation concentration tower, evaporation concentration tower temperature maintains 80-85 ℃, control relief valve and make extractor pressure maintain 5Mpa, extraction temperature is controlled at 85 ℃, 90 ℃, 95 ℃ and extracts respectively 90min.After extraction finishes, close volumetric pump, open the relief valve pressure release, continue the extractor recovery solvent of heating, during solvent-free outflow, the steam off valve releases the orange peel slag to the condensing tower.Contain the extract of orange peel effective constituent from separating tank below acquisition with accepting bucket.Weigh and obtain respectively orange peel extract 75g, 90g, 93g goes out rate and is respectively 3.00%, 3.60%, 3.72%.
Can be found out by above-mentioned example, the orange peel extraction yield raises with extraction temperature, but when extraction temperature rises to 95 ℃, goes out rate and improve not quite, therefore considers from the energy consumption angle, and selecting 90 ℃ is preferred extraction temperature.
Embodiment 2
Fresh orange peel is dried under 55 ℃, cross 20 eye mesh screens after pulverizing with pulverizer.Get the 2500g material extractor of packing into, open volumetric pump, utilize volumetric pump by squeezing into 75% ethanol to extractor in solvent transfer tank, opening simultaneously steam valve heats to extractor and evaporation concentration tower, evaporation concentration tower temperature maintains 80-85 ℃, extraction temperature is controlled at 90 ℃, and the control relief valve makes extractor pressure maintain 5Mpa, 6Mpa, 7Mpa and extracts respectively 90min.After extraction finishes, close volumetric pump, open the relief valve pressure release, continue the extractor recovery solvent of heating, during solvent-free outflow, the steam off valve releases the orange peel slag to the condensing tower.Contain the extract of orange peel effective constituent from separating tank below acquisition with accepting bucket.Weigh and obtain respectively orange peel extract 89g, 91g, 90g goes out rate and is respectively 3.56%, 3.64%, 3.60%.
Can be found out by above-mentioned example, orange peel extraction yield and extracting pressure variation relation are little, and this is to keep solvent for liquid under certain pressure because of needing only, its dissolving power and pressure independent, so the aspect consideration of slave unit cost, and selection 5Mpa is preferred extraction temperature.
Fresh orange peel is dried under 55 ℃, cross 20 eye mesh screens after pulverizing with pulverizer.Get the 2500g material extractor of packing into, open volumetric pump, utilize volumetric pump by squeezing into 75% ethanol to extractor in solvent transfer tank, opening simultaneously steam valve heats to extractor and evaporation concentration tower, evaporation concentration tower temperature maintains 80-85 ℃,, extraction temperature is controlled at 90 ℃, controls relief valve and makes extractor pressure maintain 5Mpa extraction 90min.After extraction finishes, close volumetric pump, open the relief valve pressure release, continue the extractor recovery solvent of heating, during solvent-free outflow, the steam off valve releases the orange peel slag to the condensing tower.Contain the extract of orange peel effective constituent from separating tank below acquisition with accepting bucket.Weighing obtains orange peel extract 92g, and going out rate is 3.68%.
The comparative example 1
Fresh orange peel is dried under 55 ℃, cross 20 eye mesh screens after pulverizing with pulverizer, get the 50g material and wrap into filter paper packet, take 1000ml 75% ethanol as extractant, at 70 ℃ of lower lixiviate 90min of normal pressure, take out filter paper packet, after the extracting solution evaporation concentration, obtain 0.92g orange peel extract, going out rate is 1.84%.
Can be found out by above-mentioned controlled trial, its extraction yield of technique provided by the present invention far away will be higher than the organic solvent extraction technique of routine.
Claims (10)
1. device that utilizes effective constituent in high pressure solvent extraction orange peel, it is characterized in that: it comprises extractor, evaporation concentration and condensation combined column, solvent transfer tank and volumetric pump, be connected the bottom and be connected in the top of extractor with the condensation combined column with evaporation concentration, evaporation concentration is connected top and is connected with the top of solvent transfer tank with the condensation combined column, the bottom of solvent transfer tank is connected by volumetric pump and extractor, forms circulation line; The bottom outer wall of extractor outer wall, evaporation concentration and condensation combined column is provided with steam circulating device, and the external wall of upper portion of evaporation concentration and condensation combined column is provided with cooling water circulating device, and extractor is provided with regulator.
2. method of utilizing effective constituent in high pressure solvent extraction orange peel, its step is as follows:
(1) with fresh orange peel oven dry, pulverizer is pulverized;
Then the material of (2) packing into and crushing in airtight extractor adds 75% ethanol, and the temperature that extractor is kept in heating is 85-95 ℃, and the pressure of controlling simultaneously extractor is 4-7Mpa, extracts 1-2h, after separation extracting solution;
(3) 80-85 ℃ of concentrated extracting solution, get the orange peel extract.
3. utilize according to claim 2 the method for effective constituent in high pressure solvent extraction orange peel, it is characterized in that: in step (1), fresh orange peel is dried under 55-60 ℃, crosses 20 eye mesh screens after pulverizing with pulverizer.
4. utilize according to claim 2 the method for effective constituent in high pressure solvent extraction orange peel, it is characterized in that: in step (2), the temperature of extractor is 90 ℃, and pressure is 5Mpa.
5. utilize according to claim 2 the method for effective constituent in high pressure solvent extraction orange peel, it is characterized in that: in step (3), the temperature of concentrated extracting solution is 85 ℃.
6. one kind is installed the method for extracting effective constituent in orange peel according to claim 1, it is characterized in that comprising the steps:
(1) with fresh orange peel oven dry, pulverizer is pulverized;
(2) extractor is filled the material that crushes, open volumetric pump, utilize volumetric pump by squeezing into 75% ethanol to extractor in solvent transfer tank, by steam circulating device, extractor and evaporation concentration and condensation combined column are heated simultaneously, make the extraction temperature of extractor maintain 85-95 ℃, the thickening temperature of evaporation concentration and condensation combined column maintains 80-85 ℃, controls regulator and makes the extracting pressure of extractor maintain 4-7Mpa, dynamic extraction 1-2h;
(3) after extraction finishes, close volumetric pump, open the regulator pressure release, continue the extractor recovery solvent of heating, during solvent-free outflow, the steam off circulation device releases the orange peel slag to evaporation concentration and the condensing tower;
(4) must contain the extract of orange peel effective constituent from evaporation concentration and condensation combined column bottom.
7. according to the method for effective constituent in the described extraction orange peel of claim 6, it is characterized in that: in step (1), fresh orange peel is dried under 55-60 ℃, crosses 20 eye mesh screens after pulverizing with pulverizer.
8. according to the method for effective constituent in the described extraction orange peel of claim 6, it is characterized in that: in step (2), the extraction temperature of extractor is 90 ℃, and extracting pressure is 5Mpa.
9. according to the method for effective constituent in the described extraction orange peel of claim 6, it is characterized in that: the extraction time that extracts orange peel in step (2) is 90Min.
10. according to the method for effective constituent in the described extraction orange peel of claim 6, it is characterized in that: in step (2), the thickening temperature of evaporation concentration and condensation combined column is 85 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310055337.8A CN103173285B (en) | 2013-02-21 | 2013-02-21 | Method and device for extracting active ingredients from orange peels through utilizing high-pressure solvent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310055337.8A CN103173285B (en) | 2013-02-21 | 2013-02-21 | Method and device for extracting active ingredients from orange peels through utilizing high-pressure solvent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103173285A true CN103173285A (en) | 2013-06-26 |
| CN103173285B CN103173285B (en) | 2014-03-05 |
Family
ID=48633481
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310055337.8A Active CN103173285B (en) | 2013-02-21 | 2013-02-21 | Method and device for extracting active ingredients from orange peels through utilizing high-pressure solvent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103173285B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103421599A (en) * | 2013-07-31 | 2013-12-04 | 安徽省霍山县聚一科技有限公司 | Camellia oil preparation system and operation method thereof |
| CN104635820A (en) * | 2014-12-26 | 2015-05-20 | 安徽华润金蟾药业股份有限公司 | Quality stability control method for Chinese prescription particle extraction process |
| CN104841161A (en) * | 2015-06-18 | 2015-08-19 | 刘欣建 | Extraction device |
| CN105169745A (en) * | 2015-10-21 | 2015-12-23 | 腾冲明馨生物技术开发有限公司 | Extraction device with water inlet and water outlet and steam pipes in balanced distribution |
| CN108299846A (en) * | 2018-01-08 | 2018-07-20 | 罗莱生活科技股份有限公司 | A kind of orange peel dyestuff and its preparation method and application |
| CN113576978A (en) * | 2021-08-27 | 2021-11-02 | 黄桦 | Composition containing orange medicinal material extract and preparation method and application thereof |
| CN115433637A (en) * | 2022-09-29 | 2022-12-06 | 东莞市鸿馥生物科技有限公司 | Preparation method of green tea spice |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1454694A (en) * | 2003-02-21 | 2003-11-12 | 王敬东 | Hot reflux high-pressure extracting-vacuum concentrating process |
| CN201445825U (en) * | 2009-01-23 | 2010-05-05 | 华南师范大学 | Device for extracting, concentrating and recycling |
| CN102363085A (en) * | 2011-11-11 | 2012-02-29 | 惠州市众惠能源科技有限公司 | Method and special device for extracting and concentrating water extraction liquid medicine of Chinese medicine |
| CN102552363A (en) * | 2010-12-15 | 2012-07-11 | 中国医药研究开发中心有限公司 | Preparation method for mother chrysanthemum extract |
-
2013
- 2013-02-21 CN CN201310055337.8A patent/CN103173285B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1454694A (en) * | 2003-02-21 | 2003-11-12 | 王敬东 | Hot reflux high-pressure extracting-vacuum concentrating process |
| CN201445825U (en) * | 2009-01-23 | 2010-05-05 | 华南师范大学 | Device for extracting, concentrating and recycling |
| CN102552363A (en) * | 2010-12-15 | 2012-07-11 | 中国医药研究开发中心有限公司 | Preparation method for mother chrysanthemum extract |
| CN102363085A (en) * | 2011-11-11 | 2012-02-29 | 惠州市众惠能源科技有限公司 | Method and special device for extracting and concentrating water extraction liquid medicine of Chinese medicine |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103421599A (en) * | 2013-07-31 | 2013-12-04 | 安徽省霍山县聚一科技有限公司 | Camellia oil preparation system and operation method thereof |
| CN104635820A (en) * | 2014-12-26 | 2015-05-20 | 安徽华润金蟾药业股份有限公司 | Quality stability control method for Chinese prescription particle extraction process |
| CN104841161A (en) * | 2015-06-18 | 2015-08-19 | 刘欣建 | Extraction device |
| CN105169745A (en) * | 2015-10-21 | 2015-12-23 | 腾冲明馨生物技术开发有限公司 | Extraction device with water inlet and water outlet and steam pipes in balanced distribution |
| CN105169745B (en) * | 2015-10-21 | 2017-02-01 | 腾冲明馨生物技术开发有限公司 | Extraction device with water inlet and water outlet and steam pipes in balanced distribution |
| CN108299846A (en) * | 2018-01-08 | 2018-07-20 | 罗莱生活科技股份有限公司 | A kind of orange peel dyestuff and its preparation method and application |
| CN113576978A (en) * | 2021-08-27 | 2021-11-02 | 黄桦 | Composition containing orange medicinal material extract and preparation method and application thereof |
| CN115433637A (en) * | 2022-09-29 | 2022-12-06 | 东莞市鸿馥生物科技有限公司 | Preparation method of green tea spice |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103173285B (en) | 2014-03-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103173285B (en) | Method and device for extracting active ingredients from orange peels through utilizing high-pressure solvent | |
| CN103266010B (en) | A kind of method of microwave reinforced same Cheng Cui extracting tea seed oil and tea saponin | |
| CN102772912B (en) | Device and method for extracting effective components from natural plant by high-pressure spraying reverse-flow process | |
| CN102924438B (en) | Method for extracting silymarin and silybum mariamum oil from silybum mariamum seed | |
| CN101712908A (en) | Method and device for extracting aroma component | |
| CN102746939A (en) | Method for extracting tea saponin and tea seed oil with mixed solvent | |
| CN105112155A (en) | Preparation method of high-quality cape jasmine seed oil rich in linoleic acid | |
| CN104629902A (en) | Method for extracting maize germ oil assisted by ethyl alcohol and steam explosion | |
| CN110317126A (en) | A kind of method and system for extracting cannabidiol in industrial hemp with microwave-assisted Subcritical Water Extraction technology | |
| CN101912445B (en) | Method for extracting general flavonoids from toona sinensis leaves under assistance of surfactant | |
| CN102617693A (en) | Method and device utilizing subcritical water extraction technology to extract and prepare ursolic acid from loquat leaves | |
| CN203458833U (en) | Continuous extracting, concentrating and drying production line | |
| CN101530435B (en) | Pretreatment method for extracting plant effective components | |
| CN102875350A (en) | Method for extracting paeonol | |
| CN104073355A (en) | Extraction method of pogostemon cablin essential oil | |
| CN106147989A (en) | Semen Persicae supplementing the brain Oleum Camelliae subcritical abstraction technique | |
| CN102028724A (en) | Method for preparing total flavone extracts from roundpod jute leaves | |
| CN109096353A (en) | A kind of method that continuous phase transistion extracts aurantiamarin and pectin in citrus young fruit | |
| CN104152262A (en) | Method for co-producing eucommia seed oil, eucommia rubber and eucommia extract by refining eucommia fruits through steam explosion | |
| CN104402957A (en) | Method for extracting purified phytosterol from corn stigma | |
| CN104083556A (en) | Method for extracting konjak ceramide from konjak | |
| CN205235459U (en) | Natural products active ingredient's pressurization reverse cycle extraction element | |
| CN102816169B (en) | Extraction method and extraction system for bergenin | |
| CN104119410B (en) | A kind of processing method preparing aucubin monomer from bark of eucommia fruit | |
| CN109705179A (en) | A method of the extraction purification high-purity scutellarin from radix scutellariae seed shell |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: QINGDAO LIHE EXTRACT SCIENCE + TECHNOLOGY CO., LTD Free format text: FORMER OWNER: TIANJIN UNIVERSITY OF COMMERCE Effective date: 20150416 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 300134 BEICHEN, TIANJIN TO: 264200 QINGDAO, SHANDONG PROVINCE |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20150416 Address after: 264200, Houhai, Chengyang District, Qingdao Province, Shandong, 0774 Hong Kong Nishimura Patentee after: QINGDAO LIHE EXTRACT SCIENCE & TECHNOLOGY CO., LTD. Address before: Tianjin highway 300134 east of Tianjin city Beichen District Tianjin Commercial University Patentee before: Tianjin University Of Commerce |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Method and device for extracting active ingredients from orange peels through utilizing high-pressure solvent Effective date of registration: 20151203 Granted publication date: 20140305 Pledgee: Qingdao high technology financing Company limited by guarantee Pledgor: QINGDAO LIHE EXTRACT SCIENCE & TECHNOLOGY CO., LTD. Registration number: 2015990001076 |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| C56 | Change in the name or address of the patentee | ||
| CP03 | Change of name, title or address |
Address after: 266000, Qingdao District, Shandong City, Chengyang District, Hong Kong beach after the double lane road, 210 community Patentee after: QINGDAO H.EXTRACT CO., LTD. Address before: 264200, Houhai, Chengyang District, Qingdao Province, Shandong, 0774 Hong Kong Nishimura Patentee before: QINGDAO LIHE EXTRACT SCIENCE & TECHNOLOGY CO., LTD. |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20161009 Granted publication date: 20140305 Pledgee: Qingdao high technology financing Company limited by guarantee Pledgor: QINGDAO LIHE EXTRACT SCIENCE & TECHNOLOGY CO., LTD. Registration number: 2015990001076 |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Method and device for extracting active ingredients from orange peels through utilizing high-pressure solvent Effective date of registration: 20161011 Granted publication date: 20140305 Pledgee: Qingdao high technology financing Company limited by guarantee Pledgor: QINGDAO H.EXTRACT CO., LTD. Registration number: 2016990000862 |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20170731 Granted publication date: 20140305 Pledgee: Qingdao high technology financing Company limited by guarantee Pledgor: QINGDAO H.EXTRACT CO., LTD. Registration number: 2016990000862 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Method and device for extracting active ingredients from orange peels through utilizing high-pressure solvent Effective date of registration: 20170822 Granted publication date: 20140305 Pledgee: Qingdao high technology financing Company limited by guarantee Pledgor: QINGDAO H.EXTRACT CO., LTD. Registration number: 2017370010048 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20180814 Granted publication date: 20140305 Pledgee: Qingdao high technology financing Company limited by guarantee Pledgor: QINGDAO H.EXTRACT CO., LTD. Registration number: 2017370010048 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Method and device for extracting active ingredients from orange peels through utilizing high-pressure solvent Effective date of registration: 20180821 Granted publication date: 20140305 Pledgee: Qingdao high technology financing Company limited by guarantee Pledgor: QINGDAO H.EXTRACT CO., LTD. Registration number: 2018370010087 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20191202 Granted publication date: 20140305 Pledgee: Qingdao high technology financing Company limited by guarantee Pledgor: QINGDAO H.EXTRACT CO., LTD. Registration number: 2018370010087 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Method and device for extracting active ingredients from orange peels through utilizing high-pressure solvent Effective date of registration: 20191202 Granted publication date: 20140305 Pledgee: Qingdao high technology financing Company limited by guarantee Pledgor: QINGDAO H.EXTRACT CO., LTD. Registration number: Y2019990000635 |
|
| CP03 | Change of name, title or address |
Address after: No.210, Shuangyuan Road, houhaixi community, Jihongtan street, Qingdao, Shandong Province Patentee after: Lihe flavor (Qingdao) Food Industry Co., Ltd Address before: 266000, Qingdao District, Shandong City, Chengyang District, Hong Kong beach after the double lane road, 210 community Patentee before: QINGDAO LIHE EXTRACT Co.,Ltd. |
|
| CP03 | Change of name, title or address | ||
| PM01 | Change of the registration of the contract for pledge of patent right | ||
| PM01 | Change of the registration of the contract for pledge of patent right |
Change date: 20201104 Registration number: Y2019990000635 Pledgor after: Lihe flavor (Qingdao) Food Industry Co., Ltd Pledgor before: QINGDAO LIHE EXTRACT Co.,Ltd. |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20201123 Granted publication date: 20140305 Pledgee: Qingdao high technology financing Company limited by guarantee Pledgor: Lihe flavor (Qingdao) Food Industry Co., Ltd Registration number: Y2019990000635 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A method and device for extracting effective components from orange peel by high pressure solvent Effective date of registration: 20211025 Granted publication date: 20140305 Pledgee: Qingdao high technology financing Company limited by guarantee Pledgor: Lihe flavor (Qingdao) Food Industry Co., Ltd Registration number: Y2021370010105 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20211124 Granted publication date: 20140305 Pledgee: Qingdao high technology financing Company limited by guarantee Pledgor: Lihe flavor (Qingdao) Food Industry Co., Ltd Registration number: Y2021370010105 |