CN102429140A - Supercritical CO2Method for extracting propolis with fluid - Google Patents
Supercritical CO2Method for extracting propolis with fluid Download PDFInfo
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- CN102429140A CN102429140A CN2011103309920A CN201110330992A CN102429140A CN 102429140 A CN102429140 A CN 102429140A CN 2011103309920 A CN2011103309920 A CN 2011103309920A CN 201110330992 A CN201110330992 A CN 201110330992A CN 102429140 A CN102429140 A CN 102429140A
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- 241000241413 Propolis Species 0.000 title claims abstract description 92
- 229940069949 propolis Drugs 0.000 title claims abstract description 92
- 239000012530 fluid Substances 0.000 title claims abstract description 51
- 238000000605 extraction Methods 0.000 claims abstract description 69
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000010298 pulverizing process Methods 0.000 claims abstract description 22
- 244000299461 Theobroma cacao Species 0.000 claims abstract description 14
- 235000009470 Theobroma cacao Nutrition 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims description 20
- 238000009792 diffusion process Methods 0.000 claims description 15
- 238000000746 purification Methods 0.000 claims description 15
- 238000005243 fluidization Methods 0.000 claims description 10
- 238000012546 transfer Methods 0.000 claims description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 125000004122 cyclic group Chemical group 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 230000035699 permeability Effects 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 230000002906 microbiologic effect Effects 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 2
- 241000196324 Embryophyta Species 0.000 abstract description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 2
- 239000011575 calcium Substances 0.000 abstract description 2
- 229910052791 calcium Inorganic materials 0.000 abstract description 2
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- 239000011777 magnesium Substances 0.000 abstract description 2
- 229910052749 magnesium Inorganic materials 0.000 abstract description 2
- 230000000050 nutritive effect Effects 0.000 abstract description 2
- 239000011591 potassium Substances 0.000 abstract description 2
- 229910052700 potassium Inorganic materials 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract 5
- 238000007710 freezing Methods 0.000 abstract 1
- 230000008014 freezing Effects 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000011716 vitamin B2 Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 239000000284 extract Substances 0.000 description 5
- 235000013305 food Nutrition 0.000 description 4
- 230000036541 health Effects 0.000 description 4
- 206010012601 diabetes mellitus Diseases 0.000 description 3
- 241000256844 Apis mellifera Species 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 210000004185 liver Anatomy 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000008542 thermal sensitivity Effects 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 241000050051 Chelone glabra Species 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003444 anaesthetic effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000009534 blood test Methods 0.000 description 1
- 210000000748 cardiovascular system Anatomy 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 235000006694 eating habits Nutrition 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 238000011866 long-term treatment Methods 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 231100000957 no side effect Toxicity 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 208000011580 syndromic disease Diseases 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 231100000041 toxicology testing Toxicity 0.000 description 1
Landscapes
- Jellies, Jams, And Syrups (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
Abstract
The invention discloses supercritical CO2Method for fluid extraction of propolis comprises dewaxing propolis, quick freezing, pulverizing, and granulatingPutting into a reaction kettle, and starting supercritical CO2Extraction plant of CO2Pressurizing and heating to extract propolis in supercritical liquid state in the extraction tank. Adding cocoa powder after extracting and purifying propolis, pulverizing propolis into powder by a pulverizer, adding cocoa powder according to seasons, and stirring to keep propolis powder. Cocoa powder contains vitamin B2And potassium, magnesium, calcium, iron, etc. to improve the nutritive value of propolis. The invention is a green, low-temperature and pure physical separation method, no carrying agent is used in the extraction process, compared with the traditional ethanol method, no solvent residue is left, thermosensitive components and active components are well preserved, the average extraction yield of propolis reaches 30%, and the extraction time is shortened to be within 4 hours.
Description
Technical field
The present invention relates to a kind of supercritical CO
2The method of fluid extraction propolis.
Background technology
Propolis is the maximum a kind of living resources of active component in human edible natural drug and the food.As the health care resource of ideals of human being, the applicating history in existing more than 3,000 year.Propolis has compiled the elite of animal and plant, is rich in more than 300 kind of active skull cap components, is human edible desirable health care resource.Propolis mainly contains eight large effects: the effect of (1) resisting pathogenic microbes; (2) calm, anesthetic effect; (3) promote the organization restoration effect; (4) to the influence of impaired cardiovascular system; (5) protect the liver, liver protection effect; (6) antitumor action; (7) anti-oxidant, removing free radical effect; (8) other action of nervous system.
Especially in current society, owing to receive environmental pollution, social competition and bad cause influences such as eating habit, diseases of cardiovascular and cerebrovascular systems, diabetes to become the main killer who threatens human health.And propolis has excellent prevention and therapeutic action to these diseases, and has no side effect.
Scientific research personnel of honeybee research institute of the Chinese Academy of Agricultural Sciences and the long-term treatment observation discovery of relevant medical institutions, utilizing propolis treatment diabetes total effective rate is 94.7%, and can prevent the generation and the development of diabetic syndrome.It is about 88% that the expert Ni Keluofu of the former Soviet Union uses propolis treatment hypertension, high fat of blood test total effective rate.1991, Ministry of Health of the People's Republic of China's Food Hygiene Surveillance check was carried out safety examination according to " toxicological evaluation of food safety procedure " to Beijing propolis, does not see the toxicity reflection.In June, 2002, the Ministry of Agriculture classified propolis as pollution-free food, and standard code is NY5136-2002.
But owing to receive the restriction of propolis output and extractive technique, the technical development of China's bee glue product slowly relatively always.
At present, China's propolis product suitability for industrialized production mainly is to adopt the organic solvent lixiviate, this method extract the propolis composition be polar component, there is dissolvent residual in extraction product, lead tolerance is high, needing further, processing could eat.
Summary of the invention
The technical issues that need to address of the present invention just are to overcome the defective of prior art, and a kind of supercritical CO is provided
2The method of fluid extraction propolis; It is the separation method of a kind of green, low temperature, pure physics, in extraction process, does not use any agent of carrying, and compares with traditional Ethanol Method; There is not any dissolvent residual; The intact preservation of thermal sensitivity composition and active component, propolis extract average yield and reach 30%, and the extraction time shortened in 4 hours.
For addressing the above problem, the present invention adopts following technical scheme:
The invention provides a kind of supercritical CO
2The method of fluid extraction propolis, said method for propolis is dewaxed, quick-frozen, pulverizing, granulation, drop in the reflection still, open supercritical CO
2Extraction equipment is with CO
2Pressurize, heat, it is extracted propolis in extractor with the supercritical liq state, add cocoa power after the propolis purification by liquid extraction.
Said method is for making propolis particle and CO
2Fluidization makes propolis particle and CO
2Carry out mass transfer between fluid, conduct heat and make solid particle to be suspended in the critical fluids, the diffusion process of fortification substance makes CO
2The bottom-up biofilm carrier that flows through of fluid; Biofilm carrier is a kind of microbiologic population of very thin bonding; Play a part to divide and cut apart cell; With the cell biomembrane that works be to form naturally along with the generation of propolis, make carrier layer be flow regime, thereby in the unit interval, strengthen the same CO of biomembrane
2Fluid contact area, abundant mass transfer are through particle and CO
2The cyclic process of the fluidisation diffusion between fluid, dissolving, separation makes CO
2Fluid evenly distributes in extraction kettle, improves CO
2Fluid permeability and diffusion rate, thus CO strengthened
2The cocoa power that adds propolis gross mass 20%-30% after the carrying capacity, propolis purification by liquid extraction.
Extracting pressure is that 20-36Mpa gets, and extraction temperature is 25-40 ℃; The extraction time is 3-4 hour; CO
2Flow velocity 3-5Kg/Kgh, extraction is the one-level extraction, secondary separates; One-level knockout drum pressure is 4-9Mpa, and temperature is 25-40 ℃; The secondary knockout drum is 2-6Mpa, and temperature is 15-25 ℃.
Stirring pulverizing with stainless steel pulverizing machine after the propolis purification by liquid extraction, stir the cocoa power that adds propolis gross mass 20%-30% when pulverizing, is block after propolis is purified, and pulverizes through pulverizer to be powdery.
The CO that one-level is separated
2Gas behind purification utensil, recycle.
Supercritical CO of the present invention
2The method of fluid extraction propolis is the separation method of a kind of green, low temperature, pure physics, in extraction process, does not use any agent of carrying, and compares with traditional Ethanol Method; There is not any dissolvent residual, the intact preservation of thermal sensitivity composition and active component, propolis extracts average yield and reaches 30%; The extraction time shortened in 4 hours, was block after propolis is purified, and used stainless steel to pulverize and stir in the machine to pulverize to be powdery; Add the cocoa power of 20%-30% this moment in the propolis of purification by liquid extraction, propolis is not lumpd, and is heated summer to be prone to caking; So what add is many, make propolis keep powdery, cocoa power contains Cobastab
2Reach elements such as potassium, magnesium, calcium, iron, improved the nutritive value of propolis.
The present invention can reject impurity effectively, the propolis product no solvent residue of extraction; Extract to greatest extent and save propolis Semi-polarity composition and nonpolarity element from damage; The propolis material composition of extraction is comparatively stable and complete.
Thereby advantage of the present invention has: a. adopts CO
2With the propolis granule fluid; B. technology is simple, and the extraction time is short, and production cost is low; C. reject impurity effectively; D. no solvent residue; E. extract to greatest extent and save propolis Semi-polarity composition and nonpolarity element from damage; F. adopt the extraction of different operating pressure state multi-stage separation jar; G. the propolis material composition of extraction is comparatively stable and complete, and the propolis yield is high.
The specific embodiment
Embodiment 1
The invention provides a kind of supercritical CO
2The method of fluid extraction propolis, with propolis dewax, quick-frozen, pulverizing, granulation, drop in the reflection still, open supercritical CO
2Extraction equipment is with CO
2Pressurize, heat, it is extracted propolis in extractor with the supercritical liq state.
Make propolis particle and CO
2Fluidization makes propolis particle and CO
2Carry out mass transfer between fluid, conduct heat and make solid particle to be suspended in the critical fluids, the diffusion process of fortification substance makes CO
2The bottom-up biofilm carrier that flows through of fluid, CO
2Flow velocity 5Kg/Kgh; Biofilm carrier is a kind of microbiologic population of very thin bonding, and playing a part to divide and cutting apart cell and the cell biomembrane that works is formation naturally along with the generation of propolis; Make carrier layer be flow regime, thereby in the unit interval, strengthen the same CO of biomembrane
2Fluid contact area, abundant mass transfer are through particle and CO
2The cyclic process of the fluidisation diffusion between fluid, dissolving, separation makes CO
2Fluid evenly distributes in extraction kettle, improves CO
2Fluid permeability and diffusion rate, thus CO strengthened
2Carrying capacity.
Extracting pressure is that 20Mpa gets, and extraction temperature is 40 ℃; The extraction time is 3 hours; Extraction is the one-level extraction, and secondary separates; One-level knockout drum pressure is 9Mpa, and temperature is 25 ℃; The secondary knockout drum is 6Mpa, and temperature is 15 ℃.
Stirring pulverizing with stainless steel pulverizing machine after the propolis purification by liquid extraction, stir the cocoa power that adds propolis gross mass 30% when pulverizing summer, is block after propolis is purified, and pulverizes through pulverizer to be powdery.
The CO that one-level is separated
2Gas behind purification utensil, recycle.
Embodiment 2
The invention provides a kind of supercritical CO
2The method of fluid extraction propolis, with propolis dewax, quick-frozen, pulverizing, granulation, drop in the reflection still, open supercritical CO
2Extraction equipment is with CO
2Pressurize, heat, it is extracted propolis in extractor with the supercritical liq state.
Make propolis particle and CO
2Fluidization makes propolis particle and CO
2Carry out mass transfer between fluid, conduct heat and make solid particle to be suspended in the critical fluids, the diffusion process of fortification substance makes CO
2The bottom-up biofilm carrier that flows through of fluid, CO
2Flow velocity 5Kg/Kgh; Biofilm carrier is a kind of microbiologic population of very thin bonding, and playing a part to divide and cutting apart cell and the cell biomembrane that works is formation naturally along with the generation of propolis; Make carrier layer be flow regime, thereby in the unit interval, strengthen the same CO of biomembrane
2Fluid contact area, abundant mass transfer are through particle and CO
2The cyclic process of the fluidisation diffusion between fluid, dissolving, separation makes CO
2Fluid evenly distributes in extraction kettle, improves CO
2Fluid permeability and diffusion rate, thus CO strengthened
2Carrying capacity.
Extracting pressure is that 36Mpa gets, and extraction temperature is 25 ℃; The extraction time is 4 hours; Extraction is the one-level extraction, and secondary separates; One-level knockout drum pressure is 4Mpa, and temperature is 40 ℃; The secondary knockout drum is 2Mpa, and temperature is 25 ℃.
Stirring pulverizing with stainless steel pulverizing machine after the propolis purification by liquid extraction, stir the cocoa power that adds propolis gross mass 20% when pulverizing winter, is block after propolis is purified, and pulverizes through pulverizer to be powdery.
The CO that one-level is separated
2Gas behind purification utensil, recycle.
Embodiment 3
The invention provides a kind of supercritical CO
2The method of fluid extraction propolis, with propolis dewax, quick-frozen, pulverizing, granulation, drop in the reflection still, open supercritical CO
2Extraction equipment is with CO
2Pressurize, heat, it is extracted propolis in extractor with the supercritical liq state.
Make propolis particle and CO
2Fluidization makes propolis particle and CO
2Carry out mass transfer between fluid, conduct heat and make solid particle to be suspended in the critical fluids, the diffusion process of fortification substance makes CO
2The bottom-up biofilm carrier that flows through of fluid, CO
2Flow velocity 3-5Kg/Kgh makes carrier layer be flow regime, thereby in the unit interval, strengthens the same CO of biomembrane
2Fluid contact area, abundant mass transfer are through particle and CO
2The cyclic process of the fluidisation diffusion between fluid, dissolving, separation makes CO
2Fluid evenly distributes in extraction kettle, improves CO
2Fluid permeability and diffusion rate, thus CO strengthened
2Carrying capacity.
Extracting pressure is that 30Mpa gets, and extraction temperature is 35 ℃; The extraction time is 3.5 hours; Extraction is the one-level extraction, and secondary separates; One-level knockout drum pressure is 6Mpa, and temperature is 35 ℃; The secondary knockout drum is 4Mpa, and temperature is 20 ℃.
Stirring pulverizing with stainless steel pulverizing machine after the propolis purification by liquid extraction, stir the cocoa power that adds propolis gross mass 20% when pulverizing winter, is block after propolis is purified, and pulverizes through pulverizer to be powdery.
The CO that one-level is separated
2Gas behind purification utensil, recycle.
What should explain at last is: obviously, the foregoing description only be for clearly the present invention is described and is done for example, and be not qualification to embodiment.For the those of ordinary skill in affiliated field, can also make other multi-form variation or change on the basis of the above description.Here need not also can't give exhaustive to all embodiments.And conspicuous variation of being amplified out thus or change still are among protection scope of the present invention.
Claims (5)
1. supercritical CO
2The method of fluid extraction propolis is characterized in that: said method for propolis is dewaxed, quick-frozen, pulverizing, granulation, drop in the reflection still, open supercritical CO
2Extraction equipment is with CO
2Pressurize, heat, it is extracted propolis in extractor with the supercritical liq state, add cocoa power after the propolis purification by liquid extraction.
2. supercritical CO as claimed in claim 1
2The method of fluid extraction propolis is characterized in that: said method is for making propolis particle and CO
2Fluidization makes propolis particle and CO
2Carry out mass transfer between fluid, conduct heat and make solid particle to be suspended in the critical fluids, the diffusion process of fortification substance makes CO
2The bottom-up biofilm carrier that flows through of fluid; Biofilm carrier is a kind of microbiologic population of very thin bonding; Play a part to divide and cut apart cell; With the cell biomembrane that works be to form naturally along with the generation of propolis, make carrier layer be flow regime, thereby in the unit interval, strengthen the same CO of biomembrane
2Fluid contact area, abundant mass transfer are through particle and CO
2The cyclic process of the fluidisation diffusion between fluid, dissolving, separation makes CO
2Fluid evenly distributes in extraction kettle, improves CO
2Fluid permeability and diffusion rate, thus CO strengthened
2The cocoa power that adds propolis gross mass 20%-30% after the carrying capacity, propolis purification by liquid extraction.
3. supercritical CO as claimed in claim 2
2The method of fluid extraction propolis is characterized in that: extracting pressure is that 20-36Mpa gets, and extraction temperature is 25-40 ℃; The extraction time is 3-4 hour; CO
2Flow velocity 3-5Kg/Kgh, extraction is the one-level extraction, secondary separates; One-level knockout drum pressure is 4-9Mpa, and temperature is 25-40 ℃; The secondary knockout drum is 2-6Mpa, and temperature is 15-25 ℃.
4. supercritical CO as claimed in claim 3
2The method of fluid extraction propolis is characterized in that: stirring pulverizing with stainless steel pulverizing machine after the propolis purification by liquid extraction, stir the cocoa power that adds propolis gross mass 20%-30% when pulverizing, is block after propolis is purified, and pulverizes through pulverizer to be powdery.
5. supercritical CO as claimed in claim 4
2The method of fluid extraction propolis is characterized in that: the CO that one-level is separated
2Gas behind purification utensil, recycle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103309920A CN102429140B (en) | 2011-10-27 | 2011-10-27 | Supercritical CO2 fluid extraction method of propolis |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103309920A CN102429140B (en) | 2011-10-27 | 2011-10-27 | Supercritical CO2 fluid extraction method of propolis |
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| CN102429140A true CN102429140A (en) | 2012-05-02 |
| CN102429140B CN102429140B (en) | 2013-07-24 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2011103309920A Expired - Fee Related CN102429140B (en) | 2011-10-27 | 2011-10-27 | Supercritical CO2 fluid extraction method of propolis |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103549249A (en) * | 2013-10-11 | 2014-02-05 | 吕明 | Purification technology for propolis |
| CN104770629A (en) * | 2015-03-24 | 2015-07-15 | 南昌同心紫巢生物工程有限公司 | Supercritical CO2 extraction method for high flavone content propolis |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103549249A (en) * | 2013-10-11 | 2014-02-05 | 吕明 | Purification technology for propolis |
| CN104770629A (en) * | 2015-03-24 | 2015-07-15 | 南昌同心紫巢生物工程有限公司 | Supercritical CO2 extraction method for high flavone content propolis |
| CN104770629B (en) * | 2015-03-24 | 2018-02-09 | 南昌同心紫巢生物工程有限公司 | A kind of supercritical CO of high flavones content propolis2Extracting process |
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| Publication number | Publication date |
|---|---|
| CN102429140B (en) | 2013-07-24 |
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