CN108963255A - A kind of preparation method of the conduction liquid of containing graphene - Google Patents
A kind of preparation method of the conduction liquid of containing graphene Download PDFInfo
- Publication number
- CN108963255A CN108963255A CN201810562875.9A CN201810562875A CN108963255A CN 108963255 A CN108963255 A CN 108963255A CN 201810562875 A CN201810562875 A CN 201810562875A CN 108963255 A CN108963255 A CN 108963255A
- Authority
- CN
- China
- Prior art keywords
- finished product
- graphene
- conduction liquid
- preparation
- plies
- 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
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of preparation method of the conduction liquid of containing graphene, include the following steps: that raw material graphene oxide is centrifugated by A., take upper liquid, low temperature drying obtains the less graphene oxide powder of the number of plies；B. drying under the less graphene oxide powder vacuum of the above-mentioned number of plies is formed into thick finished product；C. above-mentioned thick finished product is mixed with additive, is dissolved in heated solvent and stirring evenly, then filters while hot, filter vacuum heat drying obtains finished product Q；D. using above-mentioned finished product Q as one of ingredient, graphene conductive liquid is configured, weight percent composition is as follows: finished product Q 1%-25%, dispersing agent 0.1-3%, stabilizer 5-10%, balance of solvent.Wherein, the less graphene oxide powder number of plies of the number of plies is 1 ~ 6 layer.It is found by comparative experiments, the addition of the conduction liquid of the graphene can significantly promote battery performance.
Description
Technical field
The present invention relates to conductive agent technical fields, and in particular, to a kind of preparation method of the conduction liquid of containing graphene.
Background technique
Battery conductive agent is the key that battery plus-negative plate material, electrode interconnection auxiliary material, to the charge and discharge number of battery,
Internal resistance, power-performance produce a very large impact.Graphene is a kind of more new carbon of Recent study, has excellent lead
Electrical property and high rate performance are applied in lithium ion battery material, lithium-sulfur cell and plumbic acid, can increase substantially battery
Capacitance and high rate charge-discharge performance.
Grapheme material unique advantage in terms of lithium ion battery applications has following 3 aspect.
1. graphene has excellent conductive speed and high thermal conductivity characteristic.Graphene powder itself has had good electronics
Transmission channel and transmission rate, this can be greatly reduced the internal resistance of cell, and the excellent conduction heat transfer performance of graphene also ensures
Stability and safety of the graphene in lithium-ion-power cell system, this also further improves the safety of lithium battery
Energy.
2. the scale of graphene sheet layer is micro-nano in the macroscopical graphene combination electrode material system formed by preparation
Rice magnitude, much smaller than lithium iron phosphate positive material, ternary (NCA and NCM), graphite cathode and lithium titanate anode etc., this makes lithium
Diffusion path of the ion between graphene sheet layer is shorter, and diffusion velocity significantly improves；And the spacing between graphene sheet layer
, degree of graphitization higher graphite cathode material good also greater than crystallinity, this is more advantageous to the diffusion transport speed for improving lithium ion
Degree, and then improve battery charging and discharging speed and efficiency.
3. there is quick ion transmission channel and electricity simultaneously by the compound positive and negative pole material of graphene conductive agent electrode
Sub- transmission channel, improves efficiency of transmission, has saved a large amount of transmission times, this is very beneficial for Li-ion batteries piles multiplying power and function
Rate performance significantly improves, and solves problem present in existing lithium battery.
But graphene is as key component in conductive agent, since solubility is extremely low in its polar solvent, be easy to appear with
The problem that other compositions are incompatible, dispersion is uneven, to seriously affect the performances such as the efficiency for charge-discharge of lithium battery.Therefore, how
It researches and develops and a kind of enables to that graphene uniform disperses and the stable conduction liquid of dispersion is the emphasis that the present invention inquires into.
Summary of the invention
It is an object of the invention to overcome the above-mentioned deficiency of the prior art, a kind of preparation of the conduction liquid of containing graphene is provided
Method, solving existing conduction liquid cannot achieve the technical problem of graphene uniform dispersion and stability difference.
Surprisingly found, before the conduction liquid of preparation containing graphene, graphene is pre-processed, can be promoted
The stability and dispersibility of conduction liquid.
In order to achieve the above-mentioned object of the invention, technical scheme is as follows:
A kind of preparation method of the conduction liquid of containing graphene, includes the following steps:
A. raw material graphene oxide is centrifugated, takes upper liquid, low temperature drying obtains the less graphene oxide of the number of plies
Powder；
B. drying under the less graphene oxide powder vacuum of the above-mentioned number of plies is formed into thick finished product；
C. above-mentioned thick finished product is mixed with additive, is dissolved in heating organic phase and stirring evenly, then while hot with filter mistake
Filter, filter vacuum heat drying obtain finished product Q；
D. using above-mentioned finished product Q as one of ingredient, graphene conductive liquid is configured, weight percent composition is as follows:
Wherein,
The mass ratio of thick finished product and additive is 1:0.1~100:0.1；
The optional object of additive is diiodo-octane or chloronaphthalene；
The less graphene oxide powder number of plies of the number of plies is 1~6 layer.
Further, the preparation method of the conduction liquid of the containing graphene, wherein the centrifugal force of the centrifuge separation is
4000-8000×g。
Further, the preparation method of the conduction liquid of the containing graphene, wherein the organic phase is chlorobenzene, dichloro
Benzene, trichloro-benzenes, dimethylbenzene or trimethylbenzene.
Further, the preparation method of the conduction liquid of the containing graphene, wherein the dispersing agent be Sodium Polyacrylate,
Sodium alkyl benzene sulfonate, polyethylene glycol, polypropylene glycol or polytetramethylene glycol one or more of mixtures.
Further, the preparation method of the conduction liquid of the containing graphene, wherein the stabilizer selects carboxymethyl fine
Tie up one or more of element, acrylic acid, acrylic resin, hydroxyethyl cellulose, acrylate or acrylonitrile multiple copolymer
Mixture.
Further, the preparation method of the conduction liquid of the containing graphene, wherein the solvent selects water, ethyl alcohol, first
One or more of mixtures of alcohol or acetone.
Compared with prior art, the invention has the following advantages:
Go out the graphene of the suitable number of plies by controlling centrifugal force separate, and step described in its by specification is configured to conduction
Liquid can be obviously improved the stability and dispersibility of conduction liquid, and the internal resistance of cell has apparent reduction.Wherein additive and stone
The mixing of black alkene is committed step.
Specific embodiment
Further illustrate the present invention below in conjunction with specific embodiment, but embodiment the present invention is not done it is any type of
It limits.Unless stated otherwise, the present invention uses reagent, method and apparatus is the art conventional reagents, method and apparatus.
Unless stated otherwise, following embodiment agents useful for same and material are commercially available.
Embodiment 1
A kind of preparation method of the conduction liquid of containing graphene, includes the following steps:
A. raw material graphene oxide is centrifugated at 4000 × g, takes upper liquid, low temperature drying obtains the oxygen of layer 2-4
Graphite alkene powder；
B. drying under above-mentioned graphene oxide powder vacuum is formed into thick finished product；
C. above-mentioned thick finished product is mixed with diiodo-octane, the mass ratio of thick finished product and diiodo-octane is 1:0.1；It is dissolved in 120
It stirs evenly in DEG C chlorobenzene, is then filtered while hot with 0.45 micron of filter, filter vacuum heat drying obtains finished product Q.
D. using above-mentioned finished product Q as one of ingredient, graphene conductive liquid is configured, weight percent composition is as follows:
Finished product Q 1%
Sodium Polyacrylate 0.1%
Carboxymethyl cellulose 5%
Water surplus.
Comparative example 1
A kind of preparation method of the conduction liquid of containing graphene, includes the following steps:
A. raw material graphene oxide is centrifugated at 2000 × g, takes upper liquid, low temperature drying obtains 7-10 layers of oxygen
Graphite alkene powder；
B. drying under above-mentioned graphene oxide powder vacuum is formed into thick finished product；
C. above-mentioned thick finished product is dissolved in 120 DEG C of chlorobenzenes and is stirred evenly, then filtered while hot with 0.45 micron of filter, filtrate
Vacuum and heating drying obtains finished product Q.
D. using above-mentioned finished product Q as one of ingredient, graphene conductive liquid is configured, weight percent composition is as follows:
Finished product Q 1%
Sodium Polyacrylate 0.1%
Carboxymethyl cellulose 5%
Water surplus.
Embodiment 2
A kind of preparation method of the conduction liquid of containing graphene, includes the following steps:
A. raw material graphene oxide is centrifugated at 6000 × g, takes upper liquid, low temperature drying obtains 3-6 layers of oxygen
Graphite alkene powder；
B. drying under above-mentioned graphene oxide powder vacuum is formed into thick finished product；
C. above-mentioned thick finished product is mixed with chloronaphthalene, the mass ratio of thick finished product and chloronaphthalene is 1:0.5；It is dissolved in 120 DEG C of trimethylbenzenes
In stir evenly, then filtered while hot with 0.75 micron of filter, filter vacuum heat drying obtains finished product Q.
D. using above-mentioned finished product Q as one of ingredient, graphene conductive liquid is configured, weight percent composition is as follows:
Finished product Q 10%
Sodium alkyl benzene sulfonate 2%
Acrylic acid 8.5%
Methanol surplus.
Comparative example 2
A kind of preparation method of the conduction liquid of containing graphene, includes the following steps:
A. raw material graphene oxide is centrifugated at 1000 × g, takes upper liquid, low temperature drying obtains 10-30 layers
Graphene oxide powder；
B. drying under above-mentioned graphene oxide powder vacuum is formed into thick finished product；
C. above-mentioned thick finished product is dissolved in 120 DEG C of trimethylbenzenes and is stirred evenly, then filtered while hot with 0.75 micron of filter, filter
Liquid vacuum and heating drying obtains finished product Q.
D. using above-mentioned finished product Q as one of ingredient, graphene conductive liquid is configured, weight percent composition is as follows:
Finished product Q 10%
Sodium alkyl benzene sulfonate 2%
Acrylic acid 8.5%
Methanol surplus.
Embodiment 3
A kind of preparation method of the conduction liquid of containing graphene, includes the following steps:
A. raw material graphene oxide is centrifugated at 8,000 xg, takes upper liquid, low temperature drying obtains 1-4 layers of oxygen
Graphite alkene powder；
B. drying under above-mentioned graphene oxide powder vacuum is formed into thick finished product；
C. above-mentioned thick finished product is mixed with diiodo-octane, the mass ratio of thick finished product and diiodo-octane is 100:0.1；It is dissolved in
It stirs evenly in 120 DEG C of trimethylbenzenes, is then filtered while hot with 1 micron of filter, filter vacuum heat drying obtains finished product Q.
D. using above-mentioned finished product Q as one of ingredient, graphene conductive liquid is configured, weight percent composition is as follows:
Finished product Q 20%
Polyethylene glycol 3%
Hydroxyethyl cellulose 10%
Acetone surplus.
Comparative example 3
A kind of preparation method of the conduction liquid of containing graphene, includes the following steps:
A. raw material graphene oxide is centrifugated at 3000 × g, takes upper liquid, low temperature drying obtains 15-30 layers
Graphene oxide powder；
B. drying under above-mentioned graphene oxide powder vacuum is formed into thick finished product；
C. above-mentioned thick finished product is mixed with diiodo-octane, the mass ratio of thick finished product and diiodo-octane is 100:0.1；It is dissolved in
It stirs evenly in 120 DEG C of trimethylbenzenes, is then filtered while hot with 1 micron of filter, filter vacuum heat drying obtains finished product Q.
D. using above-mentioned finished product Q as one of ingredient, graphene conductive liquid is configured, weight percent composition is as follows:
Finished product Q 20%
Polyethylene glycol 3%
Hydroxyethyl cellulose 10%
Acetone surplus.
Embodiment 4
A kind of preparation method of the conduction liquid of containing graphene, includes the following steps:
A. raw material graphene oxide is centrifugated at 8,000 xg, takes upper liquid, low temperature drying obtains 1-4 layers of oxygen
Graphite alkene powder；
B. drying under above-mentioned graphene oxide powder vacuum is formed into thick finished product；
C. above-mentioned thick finished product is mixed with chloronaphthalene, the mass ratio of thick finished product and chloronaphthalene is 50:0.1；It is dissolved in 110 DEG C of dimethylbenzene
In stir evenly, then filtered while hot with 0.45 micron of filter, filter vacuum heat drying obtains finished product Q.
D. using above-mentioned finished product Q as one of ingredient, graphene conductive liquid is configured, weight percent composition is as follows:
Finished product Q 25%
Polypropylene glycol 0.5%
Acrylonitrile multiple copolymer 7.5%
Ethanol balance.
Comparative example 4
A kind of preparation method of the conduction liquid of containing graphene, includes the following steps:
A. raw material graphene oxide is centrifugated at 500 × g, takes upper liquid, low temperature drying obtains 50-100 layers
Graphene oxide powder；
B. drying under above-mentioned graphene oxide powder vacuum is formed into thick finished product；
C. above-mentioned thick finished product is mixed with chloronaphthalene, the mass ratio of thick finished product and chloronaphthalene is 50:0.1；It is dissolved in 110 DEG C of dimethylbenzene
In stir evenly, then filtered while hot with 0.45 micron of filter, filter vacuum heat drying obtains finished product Q.
D. using above-mentioned finished product Q as one of ingredient, graphene conductive liquid is configured, weight percent composition is as follows:
Finished product Q 25%
Polypropylene glycol 0.5%
Acrylonitrile multiple copolymer 7.5%
Ethanol balance.
Embodiment 5
The conduction liquid of the embodiment 1-4 and comparative example 1-4 containing graphene prepared is used to prepare lithium ion battery, is had
Body method is the graphene conductive liquid for providing embodiment 1-4 and comparative example 1-4 and LiFePO4 (electrode anode material
Material), binder according to 1:100:5 molar ratio carry out mixing treatment be prepared into electrode slurry, be then prepared into electrode, finally
It is assembled into lithium ion battery.Then select the common graphite alkene electrolyte substitution for the technical solution processing reported without the present invention real
Graphene conductive liquid remaining material applied in a 1-4 and comparative example 1-4 is constant, is finally assembled into lithium ion battery.Battery
Performance comparison is as follows:
By the above comparative experimental data it is found that the addition for the graphene conductive liquid that the present invention reports can greatly improve battery
Performance and stability, and the internal resistance of cell has apparent reduction.
Claims (6)
1. a kind of preparation method of the conduction liquid of containing graphene, which comprises the steps of:
A. raw material graphene oxide is centrifugated, takes upper liquid, low temperature drying obtains the less graphene oxide powder of the number of plies；
B. drying under the less graphene oxide powder vacuum of the above-mentioned number of plies is formed into thick finished product；
C. above-mentioned thick finished product is mixed with additive, is dissolved in heating organic phase and stirring evenly, then filters while hot, filter vacuum
Heat drying obtains finished product Q；
D. using above-mentioned finished product Q as one of ingredient, the conduction liquid of containing graphene is configured,
Wherein, the conduction liquid of the containing graphene is made of following weight percent composition:
Finished product Q 1%-25%；
Dispersing agent 0.1-3%；
Stabilizer 5-10%；
Balance of solvent；
Wherein, the mass ratio of thick finished product and additive is 1:0.1 ~ 100:0.1；
Additive is diiodo-octane or chloronaphthalene；
The powder number of plies of the less graphene oxide of the number of plies is 1 ~ 6 layer.
2. the preparation method of the conduction liquid of containing graphene according to claim 1, which is characterized in that the centrifuge separation
Centrifugal force is 4000-8000 × g.
3. the preparation method of the conduction liquid of containing graphene according to claim 1, which is characterized in that the organic phase is chlorine
Benzene, dichloro-benzenes, trichloro-benzenes, dimethylbenzene or trimethylbenzene.
4. the preparation method of the conduction liquid of containing graphene according to claim 1, which is characterized in that the dispersing agent is poly-
Sodium acrylate, sodium alkyl benzene sulfonate, polyethylene glycol, polypropylene glycol or polytetramethylene glycol one or more of mixtures.
5. the preparation method of the conduction liquid of containing graphene according to claim 1, which is characterized in that the stabilizer is selected
One in carboxymethyl cellulose, acrylic acid, acrylic resin, hydroxyethyl cellulose, acrylate or acrylonitrile multiple copolymer
Kind or several mixtures.
6. the preparation method of the conduction liquid of containing graphene according to claim 1, which is characterized in that the solvent is selected
One or more of water, ethyl alcohol, methanol or acetone mixture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810562875.9A CN108963255A (en) | 2018-06-01 | 2018-06-01 | A kind of preparation method of the conduction liquid of containing graphene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810562875.9A CN108963255A (en) | 2018-06-01 | 2018-06-01 | A kind of preparation method of the conduction liquid of containing graphene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108963255A true CN108963255A (en) | 2018-12-07 |
Family
ID=64492774
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810562875.9A Pending CN108963255A (en) | 2018-06-01 | 2018-06-01 | A kind of preparation method of the conduction liquid of containing graphene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108963255A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109811382A (en) * | 2019-03-28 | 2019-05-28 | 烟台恒诺新材料有限公司 | A kind of application of graphene oxide conductive paste in black holesization is directly electroplated |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104966837A (en) * | 2015-04-24 | 2015-10-07 | 深圳市德方纳米科技股份有限公司 | Graphene conductive liquid as well as preparation method and application thereof |
| CN104993137A (en) * | 2015-04-24 | 2015-10-21 | 深圳市德方纳米科技股份有限公司 | Graphene conductive solution, and preparation method and application thereof |
| CN105296053A (en) * | 2015-10-20 | 2016-02-03 | 唐山市烯润科技发展有限公司 | Method for preparing graphene lubricating oil additive |
| CN107394152A (en) * | 2017-07-17 | 2017-11-24 | 深圳市贝特瑞纳米科技有限公司 | The spherical composite of the high graphene-based LiFePO4 of conductance, its preparation method and include its lithium ion battery |
| CN107628610A (en) * | 2017-10-30 | 2018-01-26 | 北京万源工业有限公司 | A kind of method that mechanical stripping method prepares graphene and graphene conductive liquid |
-
2018
- 2018-06-01 CN CN201810562875.9A patent/CN108963255A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104966837A (en) * | 2015-04-24 | 2015-10-07 | 深圳市德方纳米科技股份有限公司 | Graphene conductive liquid as well as preparation method and application thereof |
| CN104993137A (en) * | 2015-04-24 | 2015-10-21 | 深圳市德方纳米科技股份有限公司 | Graphene conductive solution, and preparation method and application thereof |
| CN105296053A (en) * | 2015-10-20 | 2016-02-03 | 唐山市烯润科技发展有限公司 | Method for preparing graphene lubricating oil additive |
| CN107394152A (en) * | 2017-07-17 | 2017-11-24 | 深圳市贝特瑞纳米科技有限公司 | The spherical composite of the high graphene-based LiFePO4 of conductance, its preparation method and include its lithium ion battery |
| CN107628610A (en) * | 2017-10-30 | 2018-01-26 | 北京万源工业有限公司 | A kind of method that mechanical stripping method prepares graphene and graphene conductive liquid |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109811382A (en) * | 2019-03-28 | 2019-05-28 | 烟台恒诺新材料有限公司 | A kind of application of graphene oxide conductive paste in black holesization is directly electroplated |
| CN109811382B (en) * | 2019-03-28 | 2021-04-20 | 烟台恒诺新材料有限公司 | Application of graphene oxide conductive paste in black hole direct electroplating |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US9761881B2 (en) | Binder and lithium ion battery using the same | |
| CN111029569B (en) | Lithium ion battery lithium supplementing additive, battery electrode, preparation method and application thereof | |
| CN108306016B (en) | Method for modifying surface of battery anode material by using coupling agent | |
| CN103199252B (en) | Lithium-ion battery silicon-carbon anode material and preparation method thereof | |
| CN100463257C (en) | Anode active material, method of preparing the same, and anode and lithium battery employing the same | |
| CN110323493B (en) | Combined sheet of positive pole piece and polymer electrolyte membrane and preparation method thereof | |
| CN105280919A (en) | Anode active material for lithium secondary battery and method for preparing same | |
| CN107210482A (en) | All solid state secondary battery | |
| Lee et al. | A novel and efficient water-based composite binder for LiCoO2 cathodes in lithium-ion batteries | |
| CN101944588B (en) | Preparation method of capacitor carbon/lithium iron phosphate composite material | |
| CN104538635A (en) | High-performance binder for silicon materials for lithium ion batteries and preparation method thereof | |
| CN106299329A (en) | A kind of high power capacity titanium system's negative material and the lithium-ion-power cell of composition thereof | |
| CN110444740A (en) | A method of the small scale nanometer composite material of synthesizing graphite alkene/carbon-coated LiFePO 4 for lithium ion batteries is acted on by aniline polymerization confinement | |
| CN105470473A (en) | Positive electrode active material and secondary battery | |
| CN102208622B (en) | Method for preparing linear nano carbon conductive agent coated lithium iron phosphate anode material | |
| CN105609869A (en) | High-specific-energy and high-safety lithium ion power battery based on high-nickel ternary material | |
| JP2023517376A (en) | Cathodes and cathode slurries for secondary batteries | |
| CN112447971B (en) | Positive electrode material additive, active material, positive electrode material, preparation of positive electrode material and application of positive electrode material in lithium ion battery | |
| CN105489897B (en) | Ternary cathode material of lithium ion battery conduction liquid and preparation method thereof, lithium ion battery | |
| CN108899477B (en) | Graphene/metallic lithium composite electrode and preparation method thereof | |
| CN110190258A (en) | Aqueous composite mortar of Si-C composite material and preparation method thereof, lithium ion battery | |
| CN103730631B (en) | A kind of lithium ion battery cathode material and its preparation method | |
| CN108963255A (en) | A kind of preparation method of the conduction liquid of containing graphene | |
| CN105529461A (en) | Anode active material and secondary battery comprising the same | |
| CN103633313B (en) | The preparation method of a kind of fluorographite and LiMn2O4 composite material and prepare lithium ion battery as positive electrode |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| AD01 | Patent right deemed abandoned | ||
| AD01 | Patent right deemed abandoned |
Effective date of abandoning: 20211001 |