CN102533059A - Solvent-free impregnating varnish and preparation and use methods thereof - Google Patents
Solvent-free impregnating varnish and preparation and use methods thereof Download PDFInfo
- Publication number
- CN102533059A CN102533059A CN2011104288847A CN201110428884A CN102533059A CN 102533059 A CN102533059 A CN 102533059A CN 2011104288847 A CN2011104288847 A CN 2011104288847A CN 201110428884 A CN201110428884 A CN 201110428884A CN 102533059 A CN102533059 A CN 102533059A
- Authority
- CN
- China
- Prior art keywords
- solvent
- parts
- epoxy resin
- phenyl ether
- bismaleimides
- 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
Abstract
The invention relates to a solvent-free impregnating varnish, which comprises the following components in parts by mass: 15-40 parts of epoxy resin, 10-35 parts of bismaleimide, 40-60 parts of liquid acid anhydride and 10-30 parts of a low-viscosity epoxy active diluent. The preparation method comprises the following steps of: adding the epoxy resin into a reaction kettle; raising the temperature to 70 DEG C while stirring; adding bismaleimide; mixing and stirring uniformly; cooling to the room temperature; adding the liquid acid anhydride and the low-viscosity epoxy active diluent; and stirring for 30-40 minutes to obtain the solvent-free impregnating varnish. The impregnating varnish can be applied to insulating systems with high heat resistance grades such as motor train unit motors, subway motors and the like, and has high toughness and a high temperature resistance level.
Description
Technical field
The present invention relates to a kind of insulating resin and preparation method of use thereof, be meant a kind of solvent-free dose of impregnating varnish and preparation method of use thereof especially, belong to technical field of polymer materials.
Background technology
At a high speed, heavy duty become the transportation by railroad main development tendency, this just proposes high-power, miniaturization and and safety to locomotive traction motor and proposes higher requirement, and the insulation system of traction electric machine becomes the key that satisfies above-mentioned requirements.The insulation system of traction electric machine is made up of critical materials such as mica tape, impregnating varnishes.From the temperature resistant grade of material, external famous traction electric machine manufacturers has generally adopted 200 class B insulation systems for the express locomotive traction electric machine, and promptly the temperature resistant grade of impregnating varnish and mica tape sizing agent all can be at life-time service more than 200 ℃.The impregnating varnish that satisfies above-mentioned temperature resistant grade mainly contains three types, and the one, polyester modification phenyl ether impregnating varnish, the 2nd, organosilicon solvent-free dip varnish, the 3rd, modified epoxy acid anhydrides solvent-free immersion paint.
Modern electrical machine is produced and is generally adopted vacuum pressure impregnation (VPI) technology.This technology is that the workpiece preliminary drying is removed damp postcooling; Place vacuum environment; Air and the volatile matter of getting rid of the openpore coil inside rely on lacquer liquid gravity and coil capillary action in the vacuum, and utilize exsiccant pressurized air or rare gas element; To removing the effect that impregnating varnish liquid after the vacuum applies certain pressure, make lacquer liquid rapid permeability and be full of the insulation system internal layer.This technology can obtain the paint film of continuous densification, free of pinholes, and is significant for the safety that improves motor.The technique of vacuum pressure for dipping electrical of traction electric machine has following requirement to impregnating varnish: (1) lacquer fluid viscosity is moderate, and storage period is long, can under vacuum pressure condition, recycle for a long time; (2) the cured article heat-drawn wire is high, can long-time running under 200 ℃ of conditions; (3) the curing volatility is low; (4) machinery of paint film, electric property excellence; (5) cured product has good moisture-proof, weathering resistance.
The epoxy anhydride solvent-free immersion paint is to be solidifying agent by epoxy resin as matrix resin, acid anhydrides.But the temperature resistant grade of this system cured product and toughness are not enough; Can not satisfy the traction electric machine insulation moves down reliability requirement at 200 ℃ for a long time; Therefore need carry out modification to epoxy anhydride impregnating varnish system, be the requirement that impregnating varnish system cured article satisfies temperature resistant grade and mechanical property simultaneously.
Li Qin etc. [a kind of epoxy solvent-free impregnating resin and preparation method thereof] (application number: 200910042793.2; Publication number: CN101486826A) disclose a kind of linear electric motors, the EMUs motor is used impregnating varnish; Be primarily characterized in that adopting Bisphenol F, alicyclic epoxy and polyimide resin is matrix resin; And carry out the pre-polymerization modification, and adding heat-resisting acid anhydrides as solidifying agent, anhydride modified metal salt complex is promotor formation.This technical scheme starting material source is limited, and cost is higher.
Yu Xinhai etc. [heat-resistant solvent-free immersion paint and preparation method thereof] (application number: 201010256437.3; Publication number CN101921529A) discloses the heat-resistant solvent-free immersion paint prescription, be primarily characterized in that and adopt massfraction 10%-15% organosilicon polyfunctional epoxy resin, 15%-35% not to have the solidifying agent of silicon polyfunctional epoxy resin, 5%-10%, the reactive thinner of massfraction 45%-65%.This technical scheme discloses datas such as the water-intake rate, cohesive strength, volume specific resistance of viscosity, the package stability under the room temperature and the cured article of impregnating varnish; But be not disclosed in 60 ℃ of storage stability data under the condition, these data are very important for the motor technique of vacuum pressure for dipping electrical.
Summary of the invention
To the problems referred to above, the present invention provides a kind of solvent-free impregnating resin and preparation method of use thereof, has improved the temperature resistant grade and the toughness of curing system.
In order to reach above-mentioned purpose, the present invention adopts following technical scheme:
Solvent-free immersion paint, by the following composition of massfraction:
Described epoxy resin is one or more the compsn in bisphenol A epoxide resin, bisphenol F epoxy resin, cycloaliphatic epoxy resin, bisphenol-s epoxy resin, the novolac epoxy, and further, this epoxy resin is handled through short-path distillation
Described bismaleimides is one or more a compsn of dihydroxyphenyl propane phenyl ether bismaleimides, Bisphenol F phenyl ether bismaleimides, phenolphthalein phenyl ether bismaleimides, thymolphthalein phenyl ether bismaleimides, thymolsulfonphthalein phenyl ether bismaleimides, o-cresolphthalein phenyl ether bismaleimides, 1-naphtholphthalein phenyl ether bismaleimides, thymolphthalein phenyl ether bismaleimides.
Described liquid acid anhydrides comprises one or more compsn of high-purity methyl Tetra Hydro Phthalic Anhydride, methylhexahydrophthalic anhydride, methyl carbic anhydride, carbic anhydride etc.
The low viscosity epoxy reactive thinner is one or more compsns in phthalic acid diglycidylether, tetrahydrophthalic acid 2-glycidyl ester, resorcinol diglycidyl ether, neopentylglycol diglycidyl ether, cylohexanediol diglycidyl ether, ethylene glycol diglycidylether, USP Kosher diglycidylether, TriMethylolPropane(TMP) glycidyl ether, the isocyanuric acid three-glycidyl ether.
The invention allows for the preparation method of this solvent-free immersion paint, comprise the steps: 15～40 parts of epoxy resin are added in the reaction kettle, stir and be warming up to 70 ℃-100 ℃; Add 10～35 parts of bismaleimidess and stir 50min-100min; Behind the bismaleimide amine solvent, be cooled to 40 ℃-50 ℃, add 40～60 parts of liquid acid anhydrides and 10-30 part reactive thinner; Room temperature continues to stir 30min after continuing to stir formation transparent and uniform liquid mixture, and stirring velocity is 30-100 commentaries on classics/min.
This solvent-free immersion paint method of use, it is characterized in that this impregnating varnish with contain the low resin mica tape of acetylacetonate, middle glue mica tape is used, solidification value is controlled at 160 ℃～220 ℃, be 10～20 hours set time.
The present invention has adopted high-purity epoxy resin, high purity acid anhydrides and the thinner of short-path distillation as starting material, and no reactive hydrogen exists in the system, has effectively stoped the growth of viscosity.First and second components are stored at low temperatures and in dry environment, are used, and have prevented the hydrolysis of acid anhydrides, so the impregnating varnish excellent storage stability.Employing dissolves in high-purity bismaleimides of epoxy resin as properties-correcting agent, makes product after the curing possess good toughness, advantage that temperature resistant grade is high simultaneously.
Embodiment
To combine specific embodiment that the present invention is done further description below.
Embodiment 1
To be warmed up to 100 ℃ by in 15 parts of input reaction kettles of massfraction bisphenol F epoxy resin, and add 10 parts of dihydroxyphenyl propane phenyl ether bismaleimidess and stir 50min; After the dihydroxyphenyl propane phenyl ether bismaleimides stirring and dissolving; Be cooled to 40 ℃, add 30 parts of isocyanuric acid three-glycidyl ethers and 40 parts of methyl tetrahydrochysene phthalate anhydrides stirring 30min respectively, form the transparent and uniform liquid compsn; Room temperature continues to stir 30min and gets final product, and stirring velocity is 30-100 commentaries on classics/min.
Embodiment 2
20 parts of mixtures with 20 parts of bisphenol F epoxy resins of bisphenol A epoxide resin of massfraction meter are dropped in the reaction kettle; Be warmed up to 70 ℃, add phenolphthalein phenyl ether bismaleimides and stir 60min for 35 parts, behind the phenolphthalein phenyl ether bismaleimide amine solvent; Be cooled to 50 ℃; Add methylhexahydrophthalic anhydride and 45 parts in methyl carbic anhydride mixture, add 10 parts in the mixture of phthalic acid diglycidylether and tetrahydrophthalic acid 2-glycidyl ester again, stirring formation transparent and uniform liquid compsn; Room temperature continues to stir 30min and gets final product, and stirring velocity is 30-100 commentaries on classics/min.
Embodiment 3
In bisphenol A epoxide resin and 25 parts of input reaction kettles of novolac epoxy mixture; Be warmed up to 85 ℃; Add thymolsulfonphthalein phenyl ether bismaleimides and o-cresolphthalein phenyl ether bismaleimide amine mixt and stir 100min for 20 parts, behind the bismaleimide amine solvent, be cooled to 45 ℃; Add methyl tetrahydrochysene phthalate anhydride and 60 parts in methyl carbic anhydride mixture, 15 parts of USP Kosher diglycidylethers; Stir and form the transparent and uniform liquid compsn, room temperature continues to stir 30min and gets final product, and stirring velocity is 30-100 commentaries on classics/min.
The above; Be merely embodiment of the present invention, but protection scope of the present invention is not limited thereto, any technician who is familiar with the present technique field is in the technical scope that the present invention discloses; The variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain that claim was defined.
Claims (8)
1. solvent-free immersion paint is characterized in that comprising by the following composition of massfraction:
15 ~ 40 parts of epoxy resin
10 ~ 35 parts of bismaleimidess
40 ~ 60 parts on liquid acid anhydrides
10 ~ 30 parts of low viscosity epoxy reactive thinners.
2. solvent-free immersion paint according to claim 1 is characterized in that described epoxy resin is one or more the compsn in bisphenol A epoxide resin, bisphenol F epoxy resin, cycloaliphatic epoxy resin, bisphenol-s epoxy resin, the novolac epoxy.
3. solvent-free immersion paint according to claim 1 is characterized in that described bismaleimides is included as one or more compsn of dihydroxyphenyl propane phenyl ether bismaleimides, Bisphenol F phenyl ether bismaleimides, phenolphthalein phenyl ether bismaleimides, thymolphthalein phenyl ether bismaleimides, thymolsulfonphthalein phenyl ether bismaleimides, o-cresolphthalein phenyl ether bismaleimides, 1-naphtholphthalein phenyl ether bismaleimides, thymolphthalein phenyl ether bismaleimides.
4. solvent-free immersion paint according to claim 1 is characterized in that described liquid acid anhydrides is one or more a compsn of high-purity methyl Tetra Hydro Phthalic Anhydride, methylhexahydrophthalic anhydride, methyl carbic anhydride, carbic anhydride.
5. solvent-free immersion paint according to claim 1 is characterized in that described low viscosity epoxy reactive thinner is one or more compsns in phthalic acid diglycidylether, tetrahydrophthalic acid 2-glycidyl ester, resorcinol diglycidyl ether, neopentylglycol diglycidyl ether, cylohexanediol diglycidyl ether, ethylene glycol diglycidylether, USP Kosher diglycidylether, TriMethylolPropane(TMP) glycidyl ether, the isocyanuric acid three-glycidyl ether.
6. solvent-free immersion paint according to claim 2 is characterized in that described epoxy resin handles through short-path distillation.
7. the preparation method of solvent-free immersion paint according to claim 1 comprises the steps: 15 ~ 40 parts of epoxy resin are added in the reaction kettle, stirs and is warming up to 70 ℃ ~ 100 ℃; Add 10 ~ 35 parts of bismaleimidess and stir 50-100min; Behind the bismaleimide amine solvent, be cooled to 40 ℃-50 ℃, add 40 ~ 60 parts of liquid acid anhydrides and 10-30 part reactive thinner; Room temperature continues to stir 30min, 30-100 commentaries on classics/min after stirring formation transparent and uniform liquid mixture.
Solvent-free immersion paint according to claim 1 method of use; It is characterized in that this impregnating varnish with contain the low resin mica tape of acetylacetonate, middle glue mica tape is used; Solidification value is controlled at 160 ℃ ~ 220 ℃, and be 10 ~ 20 hours set time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104288847A CN102533059A (en) | 2011-12-21 | 2011-12-21 | Solvent-free impregnating varnish and preparation and use methods thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104288847A CN102533059A (en) | 2011-12-21 | 2011-12-21 | Solvent-free impregnating varnish and preparation and use methods thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102533059A true CN102533059A (en) | 2012-07-04 |
Family
ID=46341150
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011104288847A Pending CN102533059A (en) | 2011-12-21 | 2011-12-21 | Solvent-free impregnating varnish and preparation and use methods thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102533059A (en) |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103421424A (en) * | 2013-08-16 | 2013-12-04 | 卢儒 | Solvent-free nuclear motor coil impregnating varnish and preparation method thereof |
| CN103937169A (en) * | 2014-04-16 | 2014-07-23 | 株洲和诚科技有限责任公司 | Low-toxicity environment-friendly type solvent-free impregnating resin and preparation method thereof |
| CN104263200A (en) * | 2014-10-09 | 2015-01-07 | 六安市微特电机有限责任公司 | Non-solvent impregnating insulating paint and preparing method thereof |
| CN104312378A (en) * | 2014-10-09 | 2015-01-28 | 六安市微特电机有限责任公司 | High-temperature resistant solvent-free impregnating varnish and preparation method thereof |
| CN105462434A (en) * | 2015-12-03 | 2016-04-06 | 平高集团有限公司 | Surface coating material for epoxy cast insulating part and surface modification method |
| CN105462442A (en) * | 2015-12-28 | 2016-04-06 | 浙江港流高分子科技有限公司 | Environment-friendly epoxy resin coating, environment-friendly coiled material and preparation method thereof |
| CN105702324A (en) * | 2016-01-29 | 2016-06-22 | 郝福 | A solvent-free environment-friendly type mica tape and a preparation method thereof |
| CN103881563B (en) * | 2014-03-03 | 2017-04-26 | 江苏金陵特种涂料有限公司 | Titanium nanometer polymer alloy coating material and application method thereof |
| CN106634402A (en) * | 2015-11-03 | 2017-05-10 | 株洲时代新材料科技股份有限公司 | Epoxy anhydride impregnating varnish and preparation method and application thereof |
| CN106634440A (en) * | 2016-12-28 | 2017-05-10 | 株洲时代新材料科技股份有限公司 | Thixotropic impregnating resin composition, and preparation method thereof |
| CN107779051A (en) * | 2017-11-15 | 2018-03-09 | 黄腾飞 | A kind of wear-resistant paint of epoxy transparent frosted |
| CN109054601A (en) * | 2018-07-26 | 2018-12-21 | 株洲时代电气绝缘有限责任公司 | A kind of wet-heat resisting high tenacity modified unsaturated polyester solvent-free immersion paint and preparation method thereof |
| CN113773725A (en) * | 2021-10-22 | 2021-12-10 | 江苏泰特尔新材料科技股份有限公司 | Epoxy resin composition for insulating impregnating varnish and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1450132A (en) * | 2003-04-30 | 2003-10-22 | 广州擎天油漆化工实业有限公司 | Freon-resistant resin composition and preparation process and use thereof |
| CN1869122A (en) * | 2006-05-12 | 2006-11-29 | 吴江市太湖绝缘材料厂 | Solventless immersion resin used for high voltage electric machine vacuum pressure immersion |
| CN101486826A (en) * | 2009-03-05 | 2009-07-22 | 株洲时代新材料科技股份有限公司 | Epoxy solvent-free impregnating resin and preparation thereof |
-
2011
- 2011-12-21 CN CN2011104288847A patent/CN102533059A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1450132A (en) * | 2003-04-30 | 2003-10-22 | 广州擎天油漆化工实业有限公司 | Freon-resistant resin composition and preparation process and use thereof |
| CN1869122A (en) * | 2006-05-12 | 2006-11-29 | 吴江市太湖绝缘材料厂 | Solventless immersion resin used for high voltage electric machine vacuum pressure immersion |
| CN101486826A (en) * | 2009-03-05 | 2009-07-22 | 株洲时代新材料科技股份有限公司 | Epoxy solvent-free impregnating resin and preparation thereof |
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103421424B (en) * | 2013-08-16 | 2015-12-09 | 卢儒 | A kind of Solvent-free nuclear motor coil impregnating varnish and preparation method thereof |
| CN103421424A (en) * | 2013-08-16 | 2013-12-04 | 卢儒 | Solvent-free nuclear motor coil impregnating varnish and preparation method thereof |
| CN103881563B (en) * | 2014-03-03 | 2017-04-26 | 江苏金陵特种涂料有限公司 | Titanium nanometer polymer alloy coating material and application method thereof |
| CN103937169A (en) * | 2014-04-16 | 2014-07-23 | 株洲和诚科技有限责任公司 | Low-toxicity environment-friendly type solvent-free impregnating resin and preparation method thereof |
| CN103937169B (en) * | 2014-04-16 | 2016-04-13 | 株洲和诚科技有限责任公司 | A kind of low toxic and environment-friendly type solvent-free impregnating resin and preparation method thereof |
| CN104263200A (en) * | 2014-10-09 | 2015-01-07 | 六安市微特电机有限责任公司 | Non-solvent impregnating insulating paint and preparing method thereof |
| CN104312378A (en) * | 2014-10-09 | 2015-01-28 | 六安市微特电机有限责任公司 | High-temperature resistant solvent-free impregnating varnish and preparation method thereof |
| CN106634402B (en) * | 2015-11-03 | 2019-04-26 | 株洲时代电气绝缘有限责任公司 | A kind of epoxy anhydride impregnating varnish and its preparation method and application |
| CN106634402A (en) * | 2015-11-03 | 2017-05-10 | 株洲时代新材料科技股份有限公司 | Epoxy anhydride impregnating varnish and preparation method and application thereof |
| CN105462434A (en) * | 2015-12-03 | 2016-04-06 | 平高集团有限公司 | Surface coating material for epoxy cast insulating part and surface modification method |
| CN105462434B (en) * | 2015-12-03 | 2018-12-14 | 平高集团有限公司 | Epoxy casting insulating element coated material and surface modifying method |
| CN105462442A (en) * | 2015-12-28 | 2016-04-06 | 浙江港流高分子科技有限公司 | Environment-friendly epoxy resin coating, environment-friendly coiled material and preparation method thereof |
| CN105702324A (en) * | 2016-01-29 | 2016-06-22 | 郝福 | A solvent-free environment-friendly type mica tape and a preparation method thereof |
| CN105702324B (en) * | 2016-01-29 | 2017-12-19 | 重庆市龙泉汽车配件有限公司 | A kind of solvent-free environment-protection mica tape and preparation method thereof |
| CN106634440A (en) * | 2016-12-28 | 2017-05-10 | 株洲时代新材料科技股份有限公司 | Thixotropic impregnating resin composition, and preparation method thereof |
| CN106634440B (en) * | 2016-12-28 | 2019-04-26 | 株洲时代电气绝缘有限责任公司 | A kind of thixotropy impregnating resin composition and preparation method thereof |
| CN107779051A (en) * | 2017-11-15 | 2018-03-09 | 黄腾飞 | A kind of wear-resistant paint of epoxy transparent frosted |
| CN109054601A (en) * | 2018-07-26 | 2018-12-21 | 株洲时代电气绝缘有限责任公司 | A kind of wet-heat resisting high tenacity modified unsaturated polyester solvent-free immersion paint and preparation method thereof |
| CN109054601B (en) * | 2018-07-26 | 2020-09-08 | 株洲时代电气绝缘有限责任公司 | Humidity-heat-resistant high-toughness modified unsaturated polyester solvent-free impregnating varnish and preparation method thereof |
| CN113773725A (en) * | 2021-10-22 | 2021-12-10 | 江苏泰特尔新材料科技股份有限公司 | Epoxy resin composition for insulating impregnating varnish and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102533059A (en) | Solvent-free impregnating varnish and preparation and use methods thereof | |
| CN104755526B (en) | Epoxy curing agent | |
| CN106062030B (en) | Resin combination | |
| CA2835658C (en) | Insulation formulations | |
| CN108624194A (en) | Solventless epoxy coating, the corrosion-inhibiting coating based on its preparation and its application | |
| EP2707411B1 (en) | Insulation formulations | |
| CN102304217B (en) | Epoxy solvent-free impregnating resin with low viscosity and preparation method thereof | |
| CN102782000B (en) | Resin composition for sealing an optical semiconductor and optical semiconductor device using said resin composition | |
| EP2748224B1 (en) | Method of producing high voltage electrical insulation | |
| TW201704334A (en) | Epoxy resin composition | |
| CN108026248A (en) | It is used to prepare the thermosetting epoxy resin composition of outdoor product and thus obtained product | |
| CN103059268B (en) | A kind of electrical apparatus insulation part epoxide resin material | |
| TWI462833B (en) | Coated reinforcement and its manufacturing method | |
| CN103703048A (en) | Curable epoxy resin composition | |
| JP6294225B2 (en) | Method for impregnating air core reactor, impregnation air core reactor, and use of impregnation system | |
| CN103554436B (en) | A kind of molecular distillation epoxy VPI solvent impregnated resin without acid anhydrides and preparation method thereof | |
| CN103045144A (en) | Epoxy gas cylinder adhesive and method for preparing same | |
| CN104160454A (en) | Electrical insulating resin based on isohexide diol diglycide ethers | |
| CN102952509A (en) | Preparation method of epoxy resin sealant | |
| CN103087476A (en) | Impregnating resin for manufacturing nano composite major insulator for high-voltage motors | |
| CN115029093B (en) | Epoxy resin pouring sealant for automobile film capacitor and preparation method thereof | |
| CN103724597B (en) | There is modified epoxy solvent impregnated resin and the preparation method of high heat resistance | |
| RU2721163C2 (en) | Electrical insulation system based on epoxy resins for generators and engines | |
| DE102013018088A1 (en) | Epoxy-based coatings and a process for their preparation and their uses | |
| JP6539017B2 (en) | Two-component epoxy resin composition and method of manufacturing case mold type capacitor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20120704 |