CN106386872A - Sunflower straw bacteriostatic agent, and preparation method and applications thereof in preventing and treating alternaria solani sorauer - Google Patents
Sunflower straw bacteriostatic agent, and preparation method and applications thereof in preventing and treating alternaria solani sorauer Download PDFInfo
- Publication number
- CN106386872A CN106386872A CN201610789434.3A CN201610789434A CN106386872A CN 106386872 A CN106386872 A CN 106386872A CN 201610789434 A CN201610789434 A CN 201610789434A CN 106386872 A CN106386872 A CN 106386872A
- Authority
- CN
- China
- Prior art keywords
- sunflower straw
- antibacterial
- sunflower
- solvent
- straw
- 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
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/12—Asteraceae or Compositae [Aster or Sunflower family], e.g. daisy, pyrethrum, artichoke, lettuce, sunflower, wormwood or tarragon
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Plant Pathology (AREA)
- Biotechnology (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Agronomy & Crop Science (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Botany (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention provides a sunflower straw bacteriostatic agent. The sunflower straw bacteriostatic agent comprises a sunflower straw extract obtained via extraction from sunflower straw with a solvent, and the solvent is petroleum ether. A preparation method comprises following steps: 1, sunflower straw is smashed so as to obtain sunflower straw powder; 2, the sunflower powder is mixed with the solvent for extraction so as to obtain an extracted liquid; and 3, the extracted liquid is subjected to centrifugalization, and an obtained supernate is the sunflower straw bacteriostatic agent. In applications of the sunflower straw bacteriostatic agent in preventing and treating alternaria solani sorauer, bacteriostasis rate achieves 10.57% to 18.02% when mass concentration of the sunflower straw bacteriostatic agent is controlled to be 80 to 360mg/ml.
Description
Technical field
The present invention relates to a kind of novel agrochemical and preparation method and application and in particular to a kind of sunflower straw antibacterial and
Its preparation method and the application in preventing and treating target.
Background technology
Target (Alternaria solani Sorauer) is mutually every interlinkage spore (Alternaria
Alternata a kind of worldwide disease) causing, is distributed more universal in China Rhizoma Solani tuber osi producing region.Early blight mostly occurs in horse
Bell potato Later growth, causes blade to dry up in advance, yield reduction, individually the serious full Tian Wushou in plot.In recent years, early blight is being permitted
Many Rhizoma Solani tuber osis producing region is frequently anti-raw and on the rise, and the general time can cause the Rhizoma Solani tuber osi underproduction 5%~10%, serious time
Output reduction is up to more than 50%.Also become the one of Potato Industry by the storage period horse good several piece stem rot mutually causing every interlinkage spore is rotten
Individual serious problems, in some areas, storage tuber loss reaches 30%.Target is in a bad way, and production loss is bigger,
When disease is seriously 50%, production loss 20%, when disease severity is 100%, production loss is 40%.
In actual production, the Potato Cultivars of anti-early blight are less, rely primarily on Agro-chemicals control, conventional sterilization
Agent mainly has Mancozeb, Bravo, Fluoxastrobin etc., but these Agro-chemicals control effects are undesirable, and use cost is higher,
And abroad report mutually develops immunity to drugs every interlinkage spore Fluoxastrobin.In order to improve prevention effect and reduces cost, prior art
In often carry out mixture using the antibacterial in producing, to delay the drug-fast generation of pathogenic bacteria, such as Tai Lianmei et al. studies mixture
(mixture antibacterial is to the preventive effect of target and to product for the preventive effect to target for the antibacterial and the impact to yield
The impact of amount, Tai Lianmei, Jiangsu's agriculture science, the 9th phase of volume 42,2014:110-112), mixed using Fluoxastrobin and Mancozeb
With reaching mutual supplement with each other's advantages, but mixture antibacterial still can promote pathogenic bacteria to develop immunity to drugs.
Content of the invention
In view of this, it is an object of the invention to provide a kind of plant-based bacteriostat-sunflower straw extract, make described
Sunflower straw extract has inhibitory action to the mutual of the target causing every interlinkage spore, thus reaching early to Rhizoma Solani tuber osi
The purpose of the preventive effect of epidemic disease.
In order to realize foregoing invention purpose, the present invention provides technical scheme below:
The invention provides sunflower straw antibacterial, including with sunflower straw as raw material, obtained using solvent extraction
Sunflower straw extract, described solvent be petroleum ether.
Preferably, the quality of described sunflower straw and the volume ratio of solvent are 1kg:(5~15) L.
Preferably, the method for described extraction comprises the following steps:
1) sunflower straw is pulverized, the sunflower straw powder obtaining;
2) described sunflower straw powder is mixed with solvent, extraction, obtain lixiviating solution;
3) by described step 2) centrifugation of the lixiviating solution that obtains, the supernatant obtaining is sunflower straw antibacterial.
Preferably, the time of described extraction is 3~5d.
Preferably, described step 3) in centrifugation after also include:The supernatant obtaining is concentrated and is dried.
The present invention also provides a kind of preparation method of described sunflower straw antibacterial, comprises the following steps:
1) sunflower straw is pulverized, the sunflower straw powder obtaining;
2) described sunflower straw powder is mixed with solvent, extraction, obtain lixiviating solution, described solvent is petroleum ether, second
Acetoacetic ester or petroleum ether;
3) by described step 2) centrifugation of the lixiviating solution that obtains, the supernatant obtaining is sunflower straw antibacterial.
Preferably, described step 2) in sunflower straw powder before mixing with solvent cross 60~100 mesh sieves.
Preferably, described step 3) in centrifugation rotating speed be 2000~4000r/min rotating speed;Described step 3) in centrifugation
Time be 10~20min.
Present invention also offers application in inhibition of potato early epidemic pathogenic bacteria for the described sunflower straw antibacterial.
Preferably, the mass concentration of described sunflower straw antibacterial is 80~360mg/ml.
The invention provides sunflower straw antibacterial, solvent extraction is adopted to obtain including with sunflower straw for raw material
Sunflower straw extract, described solvent is petroleum ether.Using petroleum ether, for Extraction solvent, the extraction from sunflower straw is lived
Property material, the active substance in gained sunflower straw ligroin extraction all has bacteria resistance function.
Meanwhile, the invention provides sunflower straw antibacterial, the raw material sources of extraction extensively, are readily available, by inciting somebody to action
Sunflower straw extracts antibacterial substance, and sunflower straw is turned waste into wealth, and decreases sunflower straw because burning to environment simultaneously
The pollution causing, also reduces the processing cost of sunflower straw.
The present invention also provides a kind of preparation method of described sunflower straw antibacterial, after sunflower straw is pulverized
The powder arriving is mixed with solvent, extraction, centrifugation, and the supernatant obtaining is sunflower straw antibacterial.Described preparation method has
Method is simple, easy and simple to handle, not high to the technical requirements of operator, the reproducible feature of preparation method.
The present invention also provides application in inhibition of potato early epidemic pathogenic bacteria for the described sunflower straw antibacterial.Described to
Day certain herbaceous plants with big flowers straw antibacterial can effectively suppress to cause the mutual growth every interlinkage spore of target, thus reaching to Rhizoma Solani tuber osi
The inhibitory action of early blight, bacteriostasis rate reaches 10.57%~18.02%.
Further, sunflower straw antibacterial of the present invention when mass concentration is 80~360mg/mL to causing
The mutual antibacterial circle diameter every interlinkage spore of target is 12.30~12.83mm, to the mutual bacteriostasis rate every interlinkage spore is
15.27%~17.75%.
Specific embodiment
The invention provides sunflower straw antibacterial, including with sunflower straw as raw material, obtained using solvent extraction
Sunflower straw extract, described solvent be petroleum ether.
The invention provides sunflower straw antibacterial, using in the solvent Petroleum ether extraction sunflower straw of low pole
Active substance, the active substance in the sunflower straw ligroin extraction obtaining has bacteria resistance function.
In the present invention, the quality of described sunflower straw and the volume ratio of solvent are preferably 1kg:(5~15) L, more excellent
Elect 1kg as:10L.
In the present invention, the method for described extraction preferably includes following steps:
1) sunflower straw is pulverized, obtain sunflower straw powder;
2) described sunflower straw powder is mixed with solvent, extraction, obtain lixiviating solution;
3) by described step 2) centrifugation of the lixiviating solution that obtains, the supernatant obtaining is sunflower straw extract.
In the present invention, described sunflower straw selects no insect pest, the sunflower straw gone mouldy.
In the present invention, described sunflower straw was preferably dried before pulverizing.The temperature of described drying is preferably
35~60 DEG C, more preferably 37~50 DEG C;The time dried is preferably 1~5h, more preferably 2~4h.
In the present invention, the method for described pulverizing is not particularly limited, using pulverizing well-known to those skilled in the art
Method.In the present invention, the described method realization pulverized by grinding.
In the present invention, described pulverize after sunflower straw granularity be preferably 60~100 mesh, more preferably 70~90
Mesh.
After obtaining sunflower straw powder, described sunflower straw powder is mixed by the present invention with solvent, extraction, is soaked
Extract.The present invention is not particularly limited to the method for described mixing, using mixed method well-known to those skilled in the art is
Can.In embodiments of the present invention, described mixing makes raw material and solvent mix homogeneously using the method for stirring.
In the present invention, the time of described extraction is 3~5d.Described extraction is preferably carried out under normal temperature condition.
After obtaining lixiviating solution, the present invention is centrifuged to described lixiviating solution, obtains supernatant.In the present invention, described from
The speed of the heart is preferably 2000~4000r/min, more preferably 3500r/min.The time of described centrifugation is 10~20min, more
It is preferably 15min.
After obtaining supernatant, described supernatant is preferably concentrated and is dried by the present invention, obtains sunflower straw and extracts
Thing pressed powder.
In the present invention, described concentration is preferably rotary distillation concentration.The temperature that described rotary distillation concentrates is preferably
30~45 DEG C, more preferably 35~40 DEG C.The time of described concentration is preferably 1~5h, more preferably 2~4h.
In the present invention, described drying is preferably and is vacuum dried.Described vacuum drying condenser temperature is preferably -25
~-55 DEG C, more preferably -30~-45 DEG C.Described vacuum drying vacuum preferably 15~110KPa, more preferably 30
~100KPa.
In the present invention, sunflower straw antibacterial preferably also includes the adjuvant of pesticide field acceptance, makes pesticide field
Dosage form.
The present invention also provides a kind of preparation method of described sunflower straw antibacterial, comprises the following steps:
1) sunflower straw is pulverized, the sunflower straw powder obtaining;
2) described sunflower straw powder is mixed with solvent, extraction, obtain lixiviating solution, described solvent is petroleum ether, second
Acetoacetic ester or petroleum ether;
3) by described step 2) centrifugation of the lixiviating solution that obtains, the supernatant obtaining is sunflower straw antibacterial.
In the present invention, described sunflower straw powder 60~100 mesh sieves excessively before mixing with solvent, more preferably 70~
90 mesh.
In the present invention, the rotating speed of described centrifugation is preferably 2000~4000r/min, more preferably 3500r/min;Described
The time of centrifugation is preferably 10~20min, more preferably 15min.
In the present invention, the described sunflower straw antibacterial obtaining preferably also includes the adjuvant of pesticide field reception.
In the present invention, the species of the adjuvant that described pesticide field accepts preferably preferably includes wetting agent, dispersant, collapses
Solution agent, stabilizer, pH value regulator, defoamer, one of synergist and filler and several.
In the present invention, described sunflower straw antibacterial is preferably made the antibacterial dosage form of pesticide field.
In the present invention, the species of described dosage form is preferably petroleum ether dispersible granule or wettable powder.
Present invention also offers application in inhibition of potato early epidemic pathogenic bacteria for the described sunflower straw antibacterial.
In the present invention, the mass concentration of described sunflower straw antibacterial is preferably 80~36mg/ml, more preferably
160~240mg/ml.
The sunflower straw antibacterial that the present invention provided with reference to embodiment, preparation method and its in preventing and treating Rhizoma Solani tuber osi
Application in early blight is described in detail, but they can not be interpreted as limiting the scope of the present invention.
Embodiment 1
The sunflower straw select no insect pest, going mouldy is raw material, makes powdery with pulverizer, crosses 95 mesh sieves, and collection obtains
Sunflower straw powder.Weigh powder 1kg, mix with the petroleum ether of 10L, add in bucket and extract 3 days, lixiviating solution is with 3000r/
Min rotating speed is centrifuged 20min, collects supernatant, concentrated by rotary evaporation 2h under conditions of 45 DEG C, concentrate, through vacuum lyophilization, obtains
Extract powder, in 4 DEG C of refrigerators, preservation is standby.
Embodiment 2
The sunflower straw select no insect pest, going mouldy is raw material, makes powdery with pulverizer, crosses 70 mesh sieves, and collection obtains
Sunflower straw powder.Weigh powder 1kg, mix with the petroleum ether of 15L, add in bucket and extract 5 days, lixiviating solution is with 4000r/
Min rotating speed is centrifuged 10min, collects supernatant, concentrated by rotary evaporation 3h under conditions of 35 DEG C, concentrate, through vacuum lyophilization, obtains
Extract powder, in 4 DEG C of refrigerators, preservation is standby.
Embodiment 3
The sunflower straw select no insect pest, going mouldy is raw material, makes powdery with pulverizer, crosses 60 mesh sieves, and collection obtains
Sunflower straw powder.Weigh powder 1kg, mix with the petroleum ether of 5L, add in bucket and extract 4 days, lixiviating solution is with 3500r/
Min rotating speed is centrifuged 15min, collects supernatant, concentrated by rotary evaporation 4h under conditions of 30, concentrate, through vacuum lyophilization, must carry
Take thing powder, in 4 DEG C of refrigerators, preservation is standby.
Embodiment 4,5 and 6
By embodiment 1, the sunflower straw petroleum ether extract powder that embodiment 2 and embodiment 3 obtain is configured to matter respectively
Amount concentration is 80mg/mL, 160mg/mL, 240mg/mL and 360mg/mL.
Sunflower straw ligroin extraction bacteriostatic test prepares 4 culture dishs containing 20mLPDA, after PDA solidification, by 9
The extracting solution of individual concentration is respectively dropped into 1mL and and is coated with uniformly as test group, the culture dish not dealt with to different culture dishs
For blank.Each culture dish is inverted and equidistant is accessed 1 week mutual of 3 cultures every Alternariaspp cake (a diameter of 6mm).Inoculation
Afterwards, 24h cultivated in 28 DEG C of constant incubators by all culture dishs.After culture terminates, measured with crossing method with slide gauge
Calculate the meansigma methodss of 3 colony diameters in each culture dish, and bacteriostasis rate is calculated according to equation below.
The sunflower straw ligroin extraction that embodiment 1, embodiment 2 and embodiment 3 obtain is to mutually every the suppression of interlinkage spore
Make of being shown in Table 1.
Table 1 sunflower straw ligroin extraction is to mutually every inhibition zone and the bacteriostasis rate result of the generation of interlinkage spore
As seen from the above embodiment, the invention provides sunflower straw antibacterial, including with sunflower straw as raw material
The sunflower straw extract being obtained using solvent extraction, described solvent is petroleum ether.Described sunflower straw antibacterial is effective
Constituent concentration is in more than 80mg/mL to target pathogen-mutually have obvious fungistatic effect, bacteriostasis rate every interlinkage spore
For 10.72%, and increase with effective ingredient concentration and strengthen to mutually there is obvious fungistatic effect every interlinkage spore.From cost angle
Degree considers, preferably sunflower straw antibacterial effective ingredient concentration can reach preferably antibacterial effect in 160~240mg/mL
Really, bacteriostasis rate 15.27%~17.75%.When sunflower straw antibacterial effective ingredient concentration is in 360mg/mL, bacteriostasis rate highest
Reach 18.02%.
The above is only the preferred embodiment of the present invention it is noted that ordinary skill people for the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. sunflower straw antibacterial, including the extract with sunflower straw as raw material, being obtained using solvent extraction process;Institute
State solvent and include petroleum ether.
2. the sunflower straw antibacterial described in claim 1 is it is characterised in that the quality of described sunflower straw and solvent
Volume ratio is 1kg:(5~15) L.
3. the sunflower straw antibacterial described in claim 1 or 2 is it is characterised in that described extraction comprises the following steps:
1) sunflower straw is pulverized, the sunflower straw powder obtaining;
2) described sunflower straw powder is mixed with solvent, extraction, obtain lixiviating solution;
3) by described step 2) in arrive lixiviating solution centrifugation, the supernatant obtaining be sunflower straw extract.
4. sunflower straw antibacterial according to claim 3 is it is characterised in that the time of described extraction is 3~5d.
5. sunflower straw antibacterial according to claim 3 is it is characterised in that described step 3) in centrifugation after also wrap
Include:The supernatant obtaining is concentrated and is dried.
6. the sunflower straw antibacterial described in Claims 1 to 5 any one preparation method it is characterised in that include with
Lower step:
1) sunflower straw is pulverized, the sunflower straw powder obtaining;
2) described sunflower straw powder is mixed with solvent, extraction, obtain lixiviating solution, described solvent is petroleum ether, acetic acid second
Ester or petroleum ether;
3) by described step 2) centrifugation of the lixiviating solution that obtains, the supernatant obtaining is sunflower straw antibacterial.
7. preparation method according to claim 6 is it is characterised in that described step 2) in sunflower straw powder with
60~100 mesh sieves are crossed before solvent mixing.
8. preparation method according to claim 6 is it is characterised in that described step 3) in centrifugation rotating speed be 2000~
4000r/min rotating speed;Described step 3) in centrifugation time be 10~20min.
9. application in inhibition of potato early epidemic pathogenic bacteria for the sunflower straw antibacterial described in Claims 1 to 5 any one.
10. the application according to claim 9 is it is characterised in that the concentration of described sunflower straw antibacterial is 80
~360mg/ml.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610789434.3A CN106386872B (en) | 2016-08-31 | 2016-08-31 | Sunflower straw bacteriostatic agent, preparation method and its application in preventing target |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610789434.3A CN106386872B (en) | 2016-08-31 | 2016-08-31 | Sunflower straw bacteriostatic agent, preparation method and its application in preventing target |
Publications (2)
Publication Number | Publication Date |
---|---|
CN106386872A true CN106386872A (en) | 2017-02-15 |
CN106386872B CN106386872B (en) | 2018-10-23 |
Family
ID=58001328
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201610789434.3A Expired - Fee Related CN106386872B (en) | 2016-08-31 | 2016-08-31 | Sunflower straw bacteriostatic agent, preparation method and its application in preventing target |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN106386872B (en) |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1307809A (en) * | 2001-02-28 | 2001-08-15 | 高福兴 | Preparation of green pesticide |
CN107641010A (en) * | 2017-08-31 | 2018-01-30 | 覃海平 | A kind of Rice Ecology special fertilizer |
-
2016
- 2016-08-31 CN CN201610789434.3A patent/CN106386872B/en not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1307809A (en) * | 2001-02-28 | 2001-08-15 | 高福兴 | Preparation of green pesticide |
CN107641010A (en) * | 2017-08-31 | 2018-01-30 | 覃海平 | A kind of Rice Ecology special fertilizer |
Non-Patent Citations (1)
Title |
---|
吴云 黄启亮: "《实用有机化学技术》", 31 January 2008 * |
Also Published As
Publication number | Publication date |
---|---|
CN106386872B (en) | 2018-10-23 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN103724077B (en) | A kind of Enoki mushroom cultivation material containing sorghum husk and preparation method thereof | |
CN103343150A (en) | Preparation method of phenazine-1-formylhydrazine biological germicide | |
CN107439561A (en) | A kind of peach control shoot agent containing flumetralim and paclobutrazol | |
CN102674961A (en) | Organic fertilizer produced from tea cakes | |
CN103564600A (en) | Natural food preservative and preparation method thereof | |
CN101099495B (en) | Hickory nut husk disinfectant and its producing method | |
CN104909893A (en) | Special compound fertilizer for prevention and treatment of edible lily anthracnose | |
CN104256162A (en) | Caprine feed prepared from crop straws | |
CN113875763A (en) | Chelerythrine suspending agent and preparation method and application thereof | |
CN101810188A (en) | Compound imidacloprid aqueous suspension prepared by using tea saponin as synergist and surface active agent | |
CN112851430A (en) | Seaweed fertilizer and pesticide mixed composition and application thereof | |
CN106376606A (en) | Sunflower floral disc bacterial depressant, preparation method and application of sunflower floral disc bacterial depressant for preventing and treating potato early blight | |
CN103238639B (en) | Plant fungicide for preventing and treating chill continuous cropping withering disease and preparation method thereof | |
CN110050941B (en) | Aspergillus flavus growth inhibition and aflatoxin B degradation1Method (2) | |
CN106386872A (en) | Sunflower straw bacteriostatic agent, and preparation method and applications thereof in preventing and treating alternaria solani sorauer | |
CN102308806B (en) | Pesticide composition containing oxine-copper and epoxiconazole | |
CN103875740A (en) | Environment-friendly insecticide and preparation method thereof | |
CN106538624A (en) | A kind of coptis bactericide and its application in preventing and treating crop epidemic disease | |
CN105994421B (en) | A kind of botanical sterilization preparation and the application in vegetables droop is prevented | |
CN108934773A (en) | A kind of Medium for Ganoderma lucidum and preparation method thereof | |
CN107285818A (en) | Tea seed cake extract and preparation method thereof | |
CN106508971B (en) | Floral disc of sunflower bacteriostatic agent, preparation method and its application in prevention and treatment dry rot of potato | |
CN108244155A (en) | A kind of antiseptic and antibiotic packaging material prepared based on microbial method | |
CN108477218B (en) | Paddy field bactericide and application thereof | |
CN107691456B (en) | Bactericidal composition containing fluoxastrobin and shenqinmycin |
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 | ||
CF01 | Termination of patent right due to non-payment of annual fee | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20181023 Termination date: 20200831 |