CN1096456C - Process for continuously extracting glycitin, olegose and saponin - Google Patents
Process for continuously extracting glycitin, olegose and saponin Download PDFInfo
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- CN1096456C CN1096456C CN00109111A CN00109111A CN1096456C CN 1096456 C CN1096456 C CN 1096456C CN 00109111 A CN00109111 A CN 00109111A CN 00109111 A CN00109111 A CN 00109111A CN 1096456 C CN1096456 C CN 1096456C
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- feed liquid
- ethanol
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- glycitin
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Abstract
The present invention discloses a technology for continuously extracting soybean isoflavone, oligosaccharide and saponin, which comprises the following steps: step (1), the extraction of soybean isoflavone, ethanol solution is added to raw materials; the mixture is filtered, and filter liquor is collected; ethanol is recycled, and water whose volume is 1 to 4 times bigger than the that of raw material liquor is added; the pH value is adjusted to 2 to 3.5; the raw material liquor is separated with a separating machine to obtain flocculation precipitates and supernatant liquor; the flocculation precipitates are dissolved with ethanol solution, and the mixed solution is separated to collect supernatant liquor; ethanol is recycled, and the raw material liquor is concentrated until isoflavone is separated out; the raw material liquor is sterilized, and is dried by spray to obtain soybean isoflavone; step (2), the extraction of soybean oligosaccharide; step (3), the extraction of soybean saponin. Because the technology of the present invention can be used for continuously extracting three kinds of products, the waste and the cost is reduced; meanwhile, the application prospect of the present invention is good.
Description
The invention belongs to soybean deep processing field, particularly relate to the technology of a kind of continuously extracting glycitin, oligose, saponin.
Soybean isoflavones, oligose and saponin are several important component that contain in the soybean seeds.Soybean isoflavones can be converted into the compound that is similar to hormone by bacterium in the intestines, can block blood vessel hyperplasia effectively in the breeding of malignant tumour, and breaks off the nutriment source, thereby delays or stop neoplastic disease to become cancer.Simultaneously, soybean isoflavones can also be directly inhibition bone unusual again, preventing osteoporosis disease, and have antimycotic, prevent and treat effect such as hot flush, so soybean isoflavones will play important effect in pharmacy and medical health field.Because extract the complex process of isoflavones, cost is too high, so the holding at high price of soybean isoflavones on the world market at present.Soybean oligosaccharide is probiotics--the food of bifidus bacillus in the human intestinal, can promote activation, the propagation of bifidus bacillus, improve environment in the intestines, enhance metabolism, have defaecation, prevent treating constipation, reducing the generation of interior poisonous tunning of enteron aisle and unwanted bacteria enzyme, the effect of enhancing body immunity, be used widely in food, pharmacy and health care industry.Soyasaponin has removes free radical, anti-oxidant and reduce the effect of lipid peroxide, can suppress the oxidation of lipid in the serum, reduces the content of blood cholesterol and triglyceride.Soyasaponin can also stop growth of tumour cell, suppresses the infection of hiv virus, and infected cells is had the certain protection effect, has broad application prospects in pharmacy and medical health field.
At present, when soybean deep processing enterprise produces soybean isoflavones, oligose and saponin, because complex process is with high content of technology, generally all uses single Technology, produce single kind, in the waste behind the extraction object, often still contain the material of a lot of preciousnesses, caused the very big wasting of resources, simultaneously make product cost too high, the market competitiveness is not strong yet.
The technology that the purpose of this invention is to provide a kind of continuous production soybean isoflavones, soybean oligosaccharide and Soyasaponin.
The present invention takes following design: the technology of a kind of continuously extracting glycitin, oligose and saponin, consist essentially of following steps,
(1), extracts soybean isoflavones
1., raw material: the soybean plumular axis of skimmed soy beans and pulverizing;
2., add in the raw material to put in the multi-functional lixiviate stirred pot behind the 50-80% ethanolic soln and stir, raw material and alcoholic acid ratio of weight and number are 1: 8-15;
3., the feed liquid that stirs is filtered collection filtrate with filter;
4., reclaim the ethanol in the above-mentioned filtrate, and in the gained feed liquid, add material liquid volume 1-4 water doubly;
5., with above-mentioned feed liquid acidifying, transfer pH to 2-3.5;
6., the feed liquid after the acidifying changeed with 6000 above/minute separating machine separate, obtain flocculation precipitation and supernatant A;
7., with flocculation precipitation 80-90% dissolve with ethanol solution, the gained feed liquid is changeed above/minute separating machine by 6000, collects supernatant liquor, is B liquid;
8., reclaim the ethanol among the supernatant liquor B after, feed liquid is continued to concentrate, separate out to isoflavones:
9., above-mentioned feed liquid sterilization, spraying drying are obtained soybean isoflavones;
(2), extract soybean oligosaccharide
1., with above-mentioned supernatant A desalination, make its specific conductivity reach 50 μ s/cm
2Below;
2., with above-mentioned feed liquid by macroporous adsorbent resin, obtain by the material C of absorption with macroporous adsorbent resin and effusive feed liquid D;
3., feed liquid D is through concentrating, sterilization, spraying, drying obtains soybean oligosaccharide;
(3), extract Soyasaponin
1., ethanol or the methyl alcohol with 50-60% will be obtained elutriant E by material C wash-out on macroporous adsorbent resin of absorption with macroporous adsorbent resin;
2., elutriant E is 15-20% through reclaiming ethanol or methyl alcohol to the concentration of ethanol or methyl alcohol, obtain feed liquid F, add acetone-ether solvent, the volume ratio of feed liquid F and acetone-ether solvent is 1: 4-7, stirring obtains feed liquid G, that feed liquid G changes by 6000 is above/minute separating machine separate, collect flocculation precipitation;
3., above-mentioned flocculation precipitation is dissolved in water after, concentrate and vapor away ethanol or methyl alcohol and acetone-ether, obtain feed liquid H;
4., feed liquid H is concentrated, sterilization, spraying, drying obtains Soyasaponin.
The present invention is owing to adopted above-mentioned design, can continuously the soybean isoflavones in the raw material, soybean oligosaccharide and Soyasaponin be separated, obtain three kinds of products, and the quality of three kinds of products and net content all occupy first place in the world, overcome fully and used single Technology, produced the wasting of resources that single variety caused.Technology of the present invention is simple, and required equipment is the common unit of soybean deep processing industry, is highly susceptible to promoting, and has broad application prospects, and for reducing product cost, it is significant to improve the market competitiveness.
The invention will be further described below in conjunction with specific embodiment.
The processing step of continuously extracting glycitin, soybean oligosaccharide and Soyasaponin is as follows:
(1), extracts soybean isoflavones
1., the raw material that is adopted is that (soybean plumular axis is disallowable when immersion oil for defatted soybean meal behind the immersion oil and the soybean plumular axis of pulverizing, because of being rich in soybean isoflavones and Soyasaponin in the soybean plumular axis, for avoiding waste, collect and be used), after adding the soybean plumular axis that collects through pulverizing in the defatted soybean meal, mix;
2., put in the multi-functional lixiviate stirred pot behind add 70% in the raw material ethanolic soln of (50-80% all can) and stir, raw material and alcoholic acid ratio of weight and number are 1: 11 (1: 8-15 gets final product), churning time is 45 minutes (getting final product between 30-60 minute), and whipping temp is 30 ℃ (getting final product between 20 ℃-45 ℃);
3., the feed liquid that stirs is filtered with 120 orders (between the 100-150 order) filter, collect filtrate, that filtrate is changeed with 6000 is above/minute separating machine separate the collection supernatant liquor;
4., reclaim the ethanol of going up in the step gained supernatant liquor, and in the gained feed liquid, add the water of material liquid volume 3 times (1-4 doubly gets final product), and feed liquid is cooled off with the vacuum concentration method;
5., with above-mentioned feed liquid with 38% salt acid for adjusting pH value to 3 (between the 2-3.5 all can), so that soybean isoflavones is separated out;
6., after the feed liquid after the acidifying leaves standstill 18 (15-20 gets final product) minute, change with 6000 above/minute separating machine separate, obtain flocculation precipitation and contain the supernatant A of soybean oligosaccharide and saponin; To add entry in the flocculation precipitation, the ratio of weight and number of flocculation precipitation and water is 1: 8 (1: 5-10 all can), adjust pH to 3 (between the 2-3.5 all can), change with 6000 above/minute separating machine separate, collect flocculation precipitation;
7., with flocculation precipitation with 85% (80-90% all can) dissolve with ethanol solution, the gained feed liquid is collected supernatant liquor B by 10000 rev/mins of (6000 change above/minute) separating machines;
8., after the vacuum concentration method reclaims ethanol among the supernatant liquor B, feed liquid is continued to concentrate, separate out until isoflavones;
9., above-mentioned feed liquid sterilization, spraying, drying are obtained the soybean isoflavones of net content more than 80%;
(2), extract soybean oligosaccharide
1., above-mentioned supernatant A is carried out desalination with methods such as electrodialysis, ion-exchanges, make its specific conductivity reach 50 μ s/cm
2Below;
2., with above-mentioned feed liquid by macroporous adsorbent resin (macroporous adsorbent resin is nonpolar or polar macroporous adsorption resin, as D201, D370, HP-20 etc.), obtain by the material C that contains Soyasaponin and the effusive feed liquid D of absorption with macroporous adsorbent resin;
3., feed liquid D concentrates the back sterilization by membrane separation plant (Beijing's rising sun becomes ultrafiltration apparatus factory, the CLW-05 type), spraying, drying obtains the soybean oligosaccharide of net content more than 40%;
(3), extract Soyasaponin
1., the ethanol (or methyl alcohol) of (50-60% all can) will be obtained elutriant E by material C wash-out on macroporous adsorbent resin of absorption with macroporous adsorbent resin with 55%;
2., elutriant E reclaims ethanol (or methyl alcohol) through vacuum concentration, monitor the concentration of ethanol (or methyl alcohol) with Ebullioscope, be 18% (15-20% all can) to the concentration of ethanol (or methyl alcohol), obtain feed liquid F, the volume ratio that adds acetone and ether in feed liquid F is acetone-ether solvent of 1: 1, the volume ratio of feed liquid F and acetone-ether solvent is 1: 5 (1: 4-7 gets final product), fully being stirred to Soyasaponin separates out, obtain feed liquid G, that feed liquid G changes by 6000 is above/minute separating machine separate, collect the flocculation precipitation that is rich in Soyasaponin;
3., above-mentioned flocculation precipitation is dissolved in water, enable to carry out vacuum spray drying, amount of water is to make the concentration of solid substance be 6% (4-8% all can), and vacuum concentration vapors away ethanol (or methyl alcohol) and acetone-ether, obtains feed liquid H;
4., feed liquid H is concentrated, sterilization, spraying, drying obtains the Soyasaponin of net content more than 60%.
In the above-described embodiments, used raw material can also be the degreasing soybean meal that obtains behind the immersion oil or the mixture of defatted soybean meal and degreasing soybean meal, can also be the waste matter that obtains after the oil expression.
Claims (10)
1, the technology of a kind of continuously extracting glycitin, oligose and saponin is characterized in that: consist essentially of following steps,
(1), extracts soybean isoflavones
1., raw material: the soybean plumular axis of skimmed soy beans and pulverizing;
2., add in the raw material to put in the lixiviate stirred pot behind the 50-80% ethanolic soln and stir, raw material and alcoholic acid ratio of weight and number are 1: 8-15;
3., the feed liquid that stirs is filtered collection filtrate with filter;
4., reclaim the ethanol in the above-mentioned filtrate, and in the gained feed liquid, add material liquid volume 1-4 water doubly;
5., with above-mentioned feed liquid acidifying, transfer pH to 2-3.5;
6., the feed liquid after the acidifying changeed with 6000 above/minute separating machine separate, obtain flocculation precipitation and supernatant A;
7., with flocculation precipitation 80-90% dissolve with ethanol solution, the gained feed liquid is changeed above/minute separating machine by 6000, collects supernatant liquor, is B liquid;
8., reclaim the ethanol among the supernatant liquor B after, feed liquid is continued to concentrate, separate out to isoflavones;
9., above-mentioned feed liquid sterilization, spraying drying are obtained soybean isoflavones;
(2), extract soybean oligosaccharide
1., with above-mentioned supernatant A desalination, make its specific conductivity reach 50 μ s/cm
2Below;
2., with above-mentioned feed liquid by macroporous adsorbent resin, obtain by the material C of absorption with macroporous adsorbent resin and effusive feed liquid D;
3., feed liquid D is through concentrating, sterilization, spraying, drying obtains soybean oligosaccharide;
(3), extract Soyasaponin
1., ethanol or the methyl alcohol with 50-60% will be obtained elutriant E by material C wash-out on macroporous adsorbent resin of absorption with macroporous adsorbent resin;
2., elutriant E is 15-20% through reclaiming ethanol or methyl alcohol to the concentration of ethanol or methyl alcohol, obtain feed liquid F, add acetone-ether solvent, the volume ratio of feed liquid F and acetone-ether solvent is 1: 4-7, stirring obtains feed liquid G, that feed liquid G changes by 6000 is above/minute separating machine separate, collect flocculation precipitation;
3., above-mentioned flocculation precipitation is dissolved in water after, concentrate and vapor away ethanol or methyl alcohol and acetone-ether, obtain feed liquid H;
4., feed liquid H is concentrated, sterilization, spraying, drying obtains Soyasaponin.
2, the technology of a kind of continuously extracting glycitin according to claim 1, oligose and saponin, it is characterized in that: described (1), extract soybean isoflavones and the feed liquid that stirs filtered with filter in 3. after, that the filtrate of collecting is changeed through 6000 is above/minute separating machine separate after, collect supernatant liquor, entered for the 4. step again.
3, the technology of a kind of continuously extracting glycitin according to claim 1 and 2, oligose and saponin, it is characterized in that: after 6. obtaining flocculation precipitation and supernatant A in described (1), the extraction soybean isoflavones, entry will be added in the flocculation precipitation, the ratio of weight and number of flocculation precipitation and water is 1: 5-10, transfer pH2-3.5, change with 6000 above/minute separating machine separate, collect flocculation precipitation, entered for the 7. step again.
4, the technology of a kind of continuously extracting glycitin according to claim 1 and 2, oligose and saponin is characterized in that: the 1. middle skimmed soy beans of described (1), extraction soybean isoflavones is one or both in defatted soybean meal or the degreasing soybean meal; 2. middle churning time is 30-60 minute, and whipping temp is 20 ℃-45 ℃; 3. the order number of used filter is 100-150 in; 4. reclaim ethanol with the vacuum concentration method in; 5. use the salt acid for adjusting pH value in; 6. the feed liquid after the middle acidifying left standstill after 15-20 minute separates with separating machine again; 8. reclaim ethanol with the vacuum concentration method in.
5, the technology of a kind of continuously extracting glycitin according to claim 3, oligose and saponin is characterized in that: the 1. middle skimmed soy beans of described (1), extraction soybean isoflavones is one or both in defatted soybean meal or the degreasing soybean meal; 2. middle churning time is 30-60 minute, and whipping temp is 20 ℃-45 ℃; 3. the order number of used filter is 100-150 in; 4. reclaim ethanol with the vacuum concentration method in; 5. use the salt acid for adjusting pH value in; 6. the feed liquid after the middle acidifying left standstill after 15-20 minute separates with separating machine again; 8. reclaim ethanol with the vacuum concentration method in.
6, the technology of a kind of continuously extracting glycitin according to claim 1 and 2, oligose and saponin is characterized in that: described (2), extraction soybean oligosaccharide are 1. middle with electrodialytic method desalination; 2. used macroporous adsorbent resin is nonpolar or polar macroporous adsorption resin in; 3. middle feed liquid D concentrates by reverse osmosis equipment.
7, the technology of a kind of continuously extracting glycitin according to claim 3, oligose and saponin is characterized in that: described (2), extraction soybean oligosaccharide are 1. middle with electrodialytic method desalination; 2. used macroporous adsorbent resin is nonpolar or polar macroporous adsorption resin in; 3. middle feed liquid D concentrates by reverse osmosis equipment.
8, the technology of a kind of continuously extracting glycitin according to claim 4, oligose and saponin is characterized in that: described (2), extraction soybean oligosaccharide are 1. middle with electrodialytic method desalination; 2. used macroporous adsorbent resin is nonpolar or polar macroporous adsorption resin in; 3. middle feed liquid D concentrates by reverse osmosis equipment.
9, the technology of a kind of continuously extracting glycitin according to claim 1 and 2, oligose and saponin is characterized in that: described (3), extract in the Soyasaponin 2. that elutriant E reclaims ethanol or methyl alcohol through vacuum concentration; The volume ratio of acetone and ether is 1: 1 in described acetone-ether solvent; 3. the amount of water that in flocculation precipitation is dissolved in water is that to make the concentration of solid substance be 4-8%; Vapor away ethanol or methyl alcohol and acetone-ether with vacuum concentration.
10, the technology of a kind of continuously extracting glycitin according to claim 3, oligose and saponin is characterized in that: described (3), extract in the Soyasaponin 2. that elutriant E reclaims ethanol or methyl alcohol through vacuum concentration; The volume ratio of acetone and ether is 1: 1 in described acetone-ether solvent; 3. the amount of water that in flocculation precipitation is dissolved in water is that to make the concentration of solid substance be 4-8%; Vapor away ethanol or methyl alcohol and acetone-ether with vacuum concentration.
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| CN00109111A CN1096456C (en) | 2000-06-08 | 2000-06-08 | Process for continuously extracting glycitin, olegose and saponin |
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| CN00109111A CN1096456C (en) | 2000-06-08 | 2000-06-08 | Process for continuously extracting glycitin, olegose and saponin |
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| CN1327983A CN1327983A (en) | 2001-12-26 |
| CN1096456C true CN1096456C (en) | 2002-12-18 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100346161C (en) * | 2004-10-29 | 2007-10-31 | 胡传璞 | Soybean saponins detection method |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7553505B2 (en) | 2006-01-12 | 2009-06-30 | The Hong Kong University Of Science And Technology | Health care product containing isoflavone aglycones and method of producing the same |
| TWI473572B (en) | 2007-06-13 | 2015-02-21 | 大塚製藥股份有限公司 | An extract containing equol (EQUOL), a method for producing the same, an equol extraction method and an equol-containing food |
| CN102617702A (en) * | 2012-03-09 | 2012-08-01 | 姜浩奎 | Production method of peptidoglycan |
| CN103342691B (en) * | 2013-07-09 | 2015-03-11 | 内蒙古科然生物高新技术有限责任公司 | Method and equipment for extracting isoflavone, saponin and oligosaccharide from soy molasses |
| CN107287362B (en) * | 2017-06-30 | 2021-01-26 | 山东中阳生物科技有限公司 | Method for extracting soybean oligosaccharide by using soybean molasses |
| CN113318144A (en) * | 2021-06-18 | 2021-08-31 | 山东东宇生态科技有限公司 | Preparation method of isoflavone and saponin in soybean |
| CN114213476B (en) * | 2021-12-29 | 2022-11-01 | 江南大学 | Separation method and application of 4-pentanetriol-beta-methyl gentiobioside in badam |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1116657A (en) * | 1995-04-24 | 1996-02-14 | 国内贸易部西安油脂科学研究设计院 | Process for producing soya oligose by membrane separation process |
| WO1999006057A1 (en) * | 1997-07-30 | 1999-02-11 | Indena S.P.A. | Soya extract, process for its preparation and pharmaceutical composition |
| CN1245811A (en) * | 1999-08-05 | 2000-03-01 | 哈尔滨医科大学公共卫生学院 | Method for extracting soybean saponin from deffated soybean cake or soybean chips |
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2000
- 2000-06-08 CN CN00109111A patent/CN1096456C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1116657A (en) * | 1995-04-24 | 1996-02-14 | 国内贸易部西安油脂科学研究设计院 | Process for producing soya oligose by membrane separation process |
| WO1999006057A1 (en) * | 1997-07-30 | 1999-02-11 | Indena S.P.A. | Soya extract, process for its preparation and pharmaceutical composition |
| CN1245811A (en) * | 1999-08-05 | 2000-03-01 | 哈尔滨医科大学公共卫生学院 | Method for extracting soybean saponin from deffated soybean cake or soybean chips |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100346161C (en) * | 2004-10-29 | 2007-10-31 | 胡传璞 | Soybean saponins detection method |
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