CN105340941A - Insecticide composition containing benclothiaz and sulfoxaflor - Google Patents

Insecticide composition containing benclothiaz and sulfoxaflor Download PDF

Info

Publication number
CN105340941A
CN105340941A CN201510923996.8A CN201510923996A CN105340941A CN 105340941 A CN105340941 A CN 105340941A CN 201510923996 A CN201510923996 A CN 201510923996A CN 105340941 A CN105340941 A CN 105340941A
Authority
CN
China
Prior art keywords
benclothiaz
fluorine pyridine
worm amine
pyridine worm
pesticidal combination
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.)
Pending
Application number
CN201510923996.8A
Other languages
Chinese (zh)
Inventor
张英
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jinan Shunhao Biotechnology Co Ltd
Original Assignee
Jinan Shunhao Biotechnology Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Jinan Shunhao Biotechnology Co Ltd filed Critical Jinan Shunhao Biotechnology Co Ltd
Priority to CN201510923996.8A priority Critical patent/CN105340941A/en
Publication of CN105340941A publication Critical patent/CN105340941A/en
Pending legal-status Critical Current

Links

Classifications

    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/72Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N47/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/40Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Agronomy & Crop Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention relates to an insecticide composition containing benclothiaz and sulfoxaflor. The insecticide composition is characterized by containing active components of benclothiaz and sulfoxaflor and the balance of auxiliary components for preparing a pesticide formulation, wherein the weight part ratio of the active components of benclothiaz to sulfoxaflor is (1 to 30):(30 to 1), the insecticide composition can be prepared into the pesticide formulations of wettable powder, suspending agents, dissoluble liquid, emulsion in water and water dispersible granules, and the total weight parts of the active components of benclothiaz and sulfoxaflor in the pesticide formulation account for 5 percent to 40 percent of the total weight parts of the formulation. In the composition, the two active components of benclothiaz and sulfoxaflor have obvious synergistic effect, the insecticidal spectrum is enlarged, the amount of pesticides is reduced, the control efficiency is improved, the residues are few, the lasting period is long, the generation of drug resistance of injurious insects is delayed, and the environment protection is benefited.

Description

A kind of Pesticidal combination containing benclothiaz and fluorine pyridine worm amine nitrile
Technical field
The present invention relates to technical field of pesticide combination, be specifically related to a kind of Pesticidal combination containing benclothiaz and fluorine pyridine worm amine nitrile.
Background technology
Benclothiaz is considered to nematocide usually, thinks the highest to nematode activity, and since compound structure is announced, seldom see the activity research to other field or other insects, the more rare application in agriculture chemical compounding field, its chemical structural formula is as follows:
Fluorine pyridine worm amine nitrile (Sulfoxaflor), its chemical name: [1-6-(trifluoromethyl) pyridin-3-yl] ethyl]-λ 4-sulfydryl cyanamide; Molecular formula: C 10h 10f 3n 3oS, structural formula is:
Fluorine pyridine worm amine nitrile is sulfimide insecticide, acts on binding site unique in choline receptor and plays insecticidal function.Can through leaf, stem, root absorption and entering in plant corpus.Fluorine pyridine worm amine nitrile is applicable to control cotton fleahopper, aphid, aleyrodid, plant hopper and coccid etc.; Efficiently, fast and the longevity of residure long, can effectively prevent and treat nicotinoids, chrysanthemum ester class, the suction juice class pest of organophosphate and carbamate pesticide generation resistance.There is the advantages such as rapid-action, strong drug action, consumption are low, in cotton and paddy rice market, there is extensive prospect.Although fluorine pyridine worm amine eyeball mechanism of action and anabasine insecticide similar, all act on the anabasine acceptor in insect bodies, Sulfoxaflor is the new class insecticide different with anabasine, has larger potential market.
The insecticide that Long-Time Service is single, insect is easy to develop immunity to drugs, and pesticide dosage is increased, and cause the adverse consequencess such as high poison, consumption are large, residual many, drug effect is poor, and effect field is more single.And research and develop the agricultural chemical compound that seems, then the R&D cycle is long, and screening compounds arrangement works is very numerous and diverse, and non-general research and development institution can bear.But the different mechanism of action and without the insecticide rational mixture by a certain percentage of cross resistance, crop disease prevention effect can be improved, reduce dosage, residual few, reduce environmental pollution, effectively reducing the pesticide resistance of crop, is the study hotspot of current medium and small research and development institution.
Summary of the invention
According to the deficiencies in the prior art; the present invention proposes a kind of Pesticidal combination containing benclothiaz and fluorine pyridine worm amine nitrile; said composition contains benclothiaz and fluorine pyridine worm amine nitrile two kinds of effective active components, and can be prepared into the preparation being suitable for agricultural application, and this Pesticidal combination has notable synergistic effect; expand insecticidal spectrum; decrease pesticide volume, improve preventive effect, residual few; lasting period is long, and the pesticide resistance being conducive to delaying insect produces and environmental protection.
The application is a kind of Pesticidal combination containing benclothiaz and fluorine pyridine worm amine nitrile, its feature is that in this Pesticidal combination, active component is benclothiaz and fluorine pyridine worm amine nitrile, all the other are the auxiliary element of the preparation formulations of pesticide, and wherein the ratio of weight and number of active component benclothiaz and fluorine pyridine worm amine nitrile is 1 ~ 30: 30 ~ 1.
In above-described Pesticidal combination, the ratio of weight and number of active component benclothiaz and fluorine pyridine worm amine nitrile is 5 ~ 20: 5 ~ 20.
The formulations of pesticide that above-described Pesticidal combination can be prepared into are wetting powder, suspending agent, soluble liquid, aqueous emulsion and water dispersible granules.
In the application's formulations of pesticide, active component benclothiaz and fluorine pyridine worm amine nitrile total weight parts account for 5% ~ 40% of formulation total weight parts.
In the application's formulations of pesticide, active component benclothiaz and fluorine pyridine worm amine nitrile total weight parts account for 8% ~ 25% of formulation total weight parts.
The application's Pesticidal combination may be used for preventing and treating paddy rice, cotton, wheat, fruit tree, insect on vegetables, may be used for preventing and treating Noctuidae, Pyralidae, Carposinidae, tortricid, miller section, diamond-back moth section, Gracilariidae, aphid section, Aleyrodidae, Cicadellidae, Delphacidae, Culculionidae, Chrysomelidae, Agromyzidae, Bemisia tabaci insect and nematode, acarid.Can effectively prevent and treat nicotinoids, chrysanthemum ester class, organophosphate and carbamate pesticide produces the suction juice class pest of resistance.
When the application's Pesticidal combination is prepared as wetting powder, the parts by weight of each component are:
Benclothiaz1 ~ 30 part
Fluorine pyridine worm amine nitrile 1 ~ 30 part
Dispersant 5 ~ 15 parts
Wetting agent 3 ~ 10 parts
Filler 40 ~ 70 parts.
The concrete procedure of processing of this Pesticidal combination wetting powder is: by above-mentioned formula by benclothiaz and fluorine pyridine worm amine nitrile and the mixing of dispersant, wetting agent and filler, uniform stirring in stirred tank, mixing after airslide disintegrating mill, namely can be made into the wetting powder of the present composition.
When the application's Pesticidal combination is prepared as suspending agent, the parts by weight of each component are:
Benclothiaz1 ~ 30 part
Fluorine pyridine worm amine nitrile 1 ~ 30 part
Dispersant 4 ~ 12 parts
Antifreezing agent 1 ~ 4 part
Thickener 0.1 ~ 4 part
Defoamer 0.1 ~ 1 part
Water surplus.
The concrete production stage of this suspending agent is for first to mix other auxiliary agents, mix through high speed shear, add benclothiaz and fluorine pyridine worm amine nitrile, abrading-ball 2 ~ 3 hours in ball crusher, make a diameter all at below 5mm, the aqueous suspension formulations of obtained Pesticidal combination described in the application.
When the application's Pesticidal combination is prepared as aqueous emulsion, the parts by weight of each component are:
Benclothiaz1 ~ 30 part
Fluorine pyridine worm amine nitrile 1 ~ 30 part
Emulsifier 3 ~ 8 parts
Solvent 5 ~ 15 parts
Stabilizing agent 2 ~ 7 parts
Antifreezing agent 1 ~ 4 part
Defoamer 0.1 ~ 8 part
Thickener 0.2 ~ 2 part
Water surplus.
The concrete production stage of this aqueous emulsion is: first former medicine benclothiaz and fluorine pyridine worm amine nitrile, solvent and emulsifier, cosolvent are added together, make to be dissolved into uniform oil phase; By part water, antifreeze, other the insecticides adjuvant such as antimicrobial mixes uniformly aqueous phase; While high-speed stirred, oil phase is added aqueous phase in a kettle., slowly add water until reach phase inversion point, open clipper and carry out high speed shear, and add remaining water, shear about half an hour, form the aqueous emulsion of oil-in-water type.
When the application's Pesticidal combination is prepared as water dispersible granules, the parts by weight of each component are:
Benclothiaz1 ~ 30 part
Fluorine pyridine worm amine nitrile 1 ~ 30 part
Dispersant 4 ~ 12 parts
Wetting agent 3 ~ 8 parts
Disintegrant 2 ~ 8 parts
Filler 40 ~ 70 parts.
The concrete procedure of processing of this Pesticidal combination water dispersible granules is: benclothiaz, fluorine pyridine worm amine nitrile and dispersant, wetting agent, disintegrant and filler are mixed by above-mentioned formula, pulverize with micro jet, through mediating, then add in fluidized-bed granulation dryer and carry out through sample analysis after granulation, drying, screening, be i.e. the water dispersible granules of obtained Pesticidal combination.
Described emulsifier is selected from the mixture that calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether form.
Described solvent is methyl alcohol.
Described dispersant is selected from lignosulfonates.
Described wetting agent is selected from the one in lauryl sodium sulfate, spaonin powder.
Described disintegrant is selected from the one in bentonite, aluminium chloride.
Described thickener is selected from the one in xanthans, CMC, hydroxyethylcellulose, methylcellulose.
Described stabilizing agent is selected from the one in sodium citrate, resorcinol.
Described antifreezing agent is selected from the one in ethylene glycol, propane diols, glycerine.
Described defoamer is selected from silicone oil, silicone compound, C 10-20saturated fat acid compounds, C 8-10one in aliphatic alcohols compound.
Described filler is selected from the one in kaolin, diatomite, bentonite, attapulgite, white carbon, starch, precipitated calcium carbonate.
In addition, the Pesticidal combination of the application compares similar medicament also has other obvious advantages a lot, the first, compares single dose sphere of action wider, can expand insecticidal spectrum; The second, greatly delay the generation of pest resistance to insecticide, decreased agricultural chemicals Reusability number of times, reduce Pesticide use amount, reduce agricultural cost; 3rd, the residual quantity of this Pesticidal combination is lower, more friendly to environment, is significant to the increasing both production and income of agricultural region.
Embodiment:
Clearly understand to make object of the present invention, technical scheme and advantage; the following specific embodiment of the present invention is described; following examples are the preferred embodiment of the application, do not represent only test example, and the application's protection domain is as the criterion with claims.
Indoor biometrics screening and field experiment:
The method that the present invention adopts indoor bioassay and field trial to combine.If no special instructions, the ratio (comprising percentage) below mentioned is all ratio of weight and number.
Determination of activity example:
(1) reagent agent
The former medicine of benclothiaz, Syngenta Co., Ltd, the former medicine of 98% fluorine pyridine worm amine nitrile.
(2) for examination worm source
Indoor diamondback moth larvae of for many generations raising, indoor conditions: temperature (26 ± 2) oc, relative moisture 68% ± 5%, periodicity of illumination 16/8h (L/D).
(3) single dose assay method
Adopt dip method respectively two groups of former medicines all to be used a small amount of acetone solution, then be diluted to into the dense solution of 5 of equal difference with the Tween solution of 0.1%, be diluted in for subsequent use in beaker, and with clear water in contrast.
Diamondback moth larvae of the same size is flooded 5S in the liquid of leaching worm cage, and being placed on diameter after sucking unnecessary liquid is in the culture dish of 9cm, is placed with fresh vegetable leaf and adds a cover in ware.Every concentration process 10, repeats 4 times, if blank.Check lethality keep 24h in (27 ± 1) DEG C illumination box after, it is dead for touching polypide nonresponder by pulling needle.Lethality Abbott formula correction, then according to log concentration---lethality probit value analyzes (Bliss) method, obtains virulence regression equation and puts dead middle amount LC 50value.
(4) the joint toxicity measuring method of different ratio
According to the toxicity test result of single dose, by active ingredient ratio of weight and number benclothiaz: fluorine pyridine worm amine nitrile is respectively 12:5,10:7,9:9,8:9,6:11.
Adopt above-mentioned 1.3 methods to carry out toxicity test, calculate LC 50, and press abundant method calculating co-toxicity coefficient (CTC) of Sun Yun.
(5) toxicity test result and analysis
Table 1benclothiaz, fluorine pyridine worm amine nitrile are to the indoor measurement result of diamond-back moth
As can be seen from the table, in the mixture of different proportion, its co-toxicity coefficient is all greater than 120, shows certain synergistic effect, wherein benclothiaz: synergistic effect when fluorine pyridine worm amine nitrile is 8: 9 is the most obvious, and co-toxicity coefficient is 189.32.Result of the test shows, fluorine pyridine worm amine nitrile, benclothiaz two kinds of medicaments all have higher activity to diamond-back moth in room conditions, the result of the test of different proportion proportioning shows, by active ingredient benclothiaz: when fluorine pyridine worm amine nitrile is 12:5,10:7,9:9,8:9,6:11, all show stronger synergistic effect, wherein with benclothiaz: when fluorine pyridine worm amine nitrile is 8: 9, synergistic effect is best.Suggestion carries out further field control effectiveness test to the mixture preparation of suitable proportion about 8:9 scope, to evaluate its field practical application effect.
Field experiment example: field experiment control beet armyworm test
(1) test method
Test and carry out in wild cabbage plantation, carry out routine to water spray by each process design concentration.Spraying equipment is WF-16 type knapsack hand sprayer, and shower nozzle is single fan nozzle, and operating pressure is 0.2-0.4Mpa, and spray amount is 0.36-0.48L/min, carries out routine spraying, makes every effort to evenly thoughtful during spray medicine.During dispenser, field beet armyworm is 1 ~ 2 instar larvae peak period, every 667m 2be 70kg to the water yield.
Duration of test weather is good, and daily mean temperature is 18.5 ~ 27.9 DEG C.Dispenser fine day on the same day.
(2) investigation method
Diagonal 15 sampling is pressed, often some wild cabbage 2 ~ 3 strain (depending on insect density) choosing Beet Armyworm Eggs and larva in dispenser Qian Mei community.Beet exigua larvae head number in probability demarcation strain, in this, as insect population radix before dispenser.After dispenser the 3rd, 7,10d investigates the beet exigua larvae number determining residual survival in strain, respectively to correct Revision insect recluced rate as control efficiency.
(3) drug effect computational methods.
Revision insect recluced rate (%)= × 100
Rectifying efficacies (%)= × 100;
(4) poisoning investigation method
Duration of test observes each process community wild cabbage well-grown, all finds no poisoning phenomenon and occurs.
(5) field control effectiveness test result of the test
Table 2 treatment agent control Laphygma exigua Hubner field control effectiveness test result
As can be seen from Table 2, the successful of the mixture combination control Laphygma exigua Hubner of 8%benclothiaz+9% fluorine pyridine worm amine nitrile is better than 20% fluorine pyridine worm amine nitrile SC and contrasts single dose, 8%benclothiaz+9% fluorine pyridine worm amine nitrile insecticidal effect of 10 days after medicine is respectively 94.49%, 94.23% and 95.15%, insecticidal effect increases progressively along with the increase of consumption, estimate according to field, substantially disease is not had with the wild cabbage of 8%benclothiaz+9% fluorine pyridine worm amine nitrile, and growth fraction is more vigorous, and occur that disease is more with the wild cabbage of 20% fluorine pyridine worm amine nitrile SC single dose, the disease plant much about about 7% of ratio complex preparation.
In addition within the scope of test dose, plant growth is normal, and the poisoning phenomenon to wild cabbage does not all appear in each treatment agent, illustrates that it is safe to wild cabbage.

Claims (7)

1. one kind contains the Pesticidal combination of benclothiaz and fluorine pyridine worm amine nitrile, it is characterized in that: in this Pesticidal combination, active component is benclothiaz and fluorine pyridine worm amine nitrile, all the other are the auxiliary element of the preparation formulations of pesticide, and wherein the ratio of weight and number of active component benclothiaz and fluorine pyridine worm amine nitrile is 1 ~ 30: 30 ~ 1.
2. a kind of Pesticidal combination containing benclothiaz and fluorine pyridine worm amine nitrile according to claim 1, is characterized in that: in described Pesticidal combination, the ratio of weight and number of active component benclothiaz and fluorine pyridine worm amine nitrile is 5 ~ 20: 5 ~ 20.
3. a kind of Pesticidal combination containing benclothiaz and fluorine pyridine worm amine nitrile according to claim 1 and 2, is characterized in that: the formulations of pesticide that described Pesticidal combination can be prepared into are wetting powder, suspending agent, soluble liquid, aqueous emulsion and water dispersible granules.
4. a kind of Pesticidal combination containing benclothiaz and fluorine pyridine worm amine nitrile according to claim 3, is characterized in that: in the formulations of pesticide, active component benclothiaz and fluorine pyridine worm amine nitrile total weight parts account for 5% ~ 40% of formulation total weight parts.
5. a kind of Pesticidal combination containing benclothiaz and fluorine pyridine worm amine nitrile according to claim 1 or 2 or 4, is characterized in that: in the formulations of pesticide, active component benclothiaz and fluorine pyridine worm amine nitrile total weight parts account for 8% ~ 25% of formulation total weight parts.
6. a kind of Pesticidal combination containing benclothiaz and fluorine pyridine worm amine nitrile according to claim 1 or 2 or 4, is characterized in that: this Pesticidal combination may be used for preventing and treating the insect on paddy rice, cotton, wheat, fruit tree, vegetables.
7. a kind of Pesticidal combination containing benclothiaz and fluorine pyridine worm amine nitrile according to claim 6, is characterized in that: this Pesticidal combination may be used for preventing and treating Noctuidae, Pyralidae, Carposinidae, tortricid, miller section, diamond-back moth section, Gracilariidae, aphid section, Aleyrodidae, Cicadellidae, Delphacidae, Culculionidae, Chrysomelidae, Agromyzidae, Bemisia tabaci insect and nematode, acarid.
CN201510923996.8A 2015-12-14 2015-12-14 Insecticide composition containing benclothiaz and sulfoxaflor Pending CN105340941A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510923996.8A CN105340941A (en) 2015-12-14 2015-12-14 Insecticide composition containing benclothiaz and sulfoxaflor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510923996.8A CN105340941A (en) 2015-12-14 2015-12-14 Insecticide composition containing benclothiaz and sulfoxaflor

Publications (1)

Publication Number Publication Date
CN105340941A true CN105340941A (en) 2016-02-24

Family

ID=55317228

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510923996.8A Pending CN105340941A (en) 2015-12-14 2015-12-14 Insecticide composition containing benclothiaz and sulfoxaflor

Country Status (1)

Country Link
CN (1) CN105340941A (en)

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
张静等: "具有生物活性的异噻唑类化合物研究进展", 《农药》 *
王彭等: "氟啶虫胺腈对水稻褐飞虱的室内杀虫活性及田间药效", 《农药》 *

Similar Documents

Publication Publication Date Title
CN102986700A (en) Insecticide composition containing flutenzine and bistrifluron
CN102232385A (en) Insecticidal composition containing clothianidin and abamectin
CN102484991B (en) Synergic farm pesticide composition of ivermectin and tea saponin
CN105340948A (en) Insecticide composition containing benclothiaz and efficient cyhalothrin
CN105340950A (en) Insecticide composition containing o-phenylenediamine pesticide and efficient cyhalothrin
CN105340941A (en) Insecticide composition containing benclothiaz and sulfoxaflor
CN105475336A (en) Insecticidal combination containing benclothiaz and imidacloprid
CN104255735A (en) Pyridalyl and tetra-chlorantraniliprole compounded insecticidal composition
CN105475332A (en) Insecticidal combination containing o-phenylendiamine insecticide and sulfoxaflor
CN104082323B (en) There is the insect-killing composition of synergism
CN105454259A (en) Insecticidal combination containing o-phenylenediamine insecticide and abamectin
CN105340910A (en) Insecticide composition containing benclothiaz and flonicamid
CN105360133A (en) Insecticide composition containing o-phenylenediamine insecticide and chlorantraniliprole
CN105340909A (en) Insecticide composition containing benclothiaz and chlorfenapyr
CN105325419A (en) Insecticidal combination containing o-phenylenediamine insecticide and chlorfenapyr
CN105340924A (en) Insecticide composition containing o-phenylenediamine pesticide and sophocarpidine
CN105475329A (en) Insecticidal combination containing o-phenylendiamine insecticide and indoxacarb
CN105340940A (en) Insecticide composition containing benclothiaz and indoxacarb
CN105325427A (en) Insecticidal combination containing benclothiaz and ethiprole
CN105454243A (en) Insecticidal combination containing o-phenylenediamine insecticide and ethiprole
CN103704263B (en) A kind of Pesticidal combination containing indoxacarb
CN105475337A (en) Insecticidal combination containing o-phenylendiamine insecticide and imidacloprid
CN105309448A (en) Insecticide composition containing benclothiaz and pleocidin
CN105325448A (en) Insecticidal combination containing o-phenylenediamine insecticide and thiamethoxam
CN105340922A (en) Insecticide composition containing benclothiaz and abamectin

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20160224