CN107537510A - A kind of catalyst of Mo doped ferric oxides and preparation method thereof - Google Patents
A kind of catalyst of Mo doped ferric oxides and preparation method thereof Download PDFInfo
- Publication number
- CN107537510A CN107537510A CN201710834168.6A CN201710834168A CN107537510A CN 107537510 A CN107537510 A CN 107537510A CN 201710834168 A CN201710834168 A CN 201710834168A CN 107537510 A CN107537510 A CN 107537510A
- Authority
- CN
- China
- Prior art keywords
- catalyst
- molybdate
- ferric oxides
- preparation
- molysite
- 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
Landscapes
- Catalysts (AREA)
Abstract
The present invention relates to a kind of catalyst of Mo doped ferric oxides and preparation method thereof.Its technical scheme is：By molysite: molybdate mass ratio is（50~99）∶（1~50）, the molysite and the molybdate are dissolved in deionized water respectively, obtain iron salt solutions and molybdate solution.The iron salt solutions are homogeneously added into the molybdate solution under agitation, obtain mixed solution；The pH value for adjusting the mixed solution with ammoniacal liquor filters to 4 ~ 8, filtered sediment is washed with deionized to neutrality, dried under the conditions of 110 DEG C, obtain front axle shell.Then the front axle shell is calcined into 0.5 ~ 9h under the conditions of 400 DEG C ~ 900 DEG C, the catalyst of Mo doped ferric oxides is made.The molysite is one or more of iron chloride, ferric nitrate and ferric sulfate；The molybdate is one or more of ammonium molybdate and sodium molybdate.The present invention is with technique is simple, cost is low and reacts easily controllable, the size tunable and excellent catalytic effect of made product.
Description
Technical field
The invention belongs to ferric oxide catalyst technical field.More particularly to a kind of catalyst and its system of Mo doped ferric oxides
Preparation Method.
Background technology
Carbon containing refractory has been widely used as due to high-temperature behaviors such as its excellent corrosion resistance and heat-resistant knocking stabilities
In the refractory materials such as casting process middle slide plate, the mouth of a river and stopper.But due to graphite in itself easily be oxidized etc. reason, also make carbon containing resistance to
Fiery material exposes some problems in use, and the product as resinoid bond is pyrolyzed under high temperature is non crystalline structure, is answering
Brittle fracture easily occurs in the presence of power reduces mechanical behavior under high temperature, and amorphous carbon easily aoxidizes at high temperature, and reduction contains
The Residual carbon of carbon refractory.To improve the service life and high-temperature behavior of carbon containing refractory, in carbon containing refractory Central Plains
Position, which generates one-dimensional toughness reinforcing phase structure, turns into one of important means.
Mainly recombinate carbon atom by adding catalyst in carbon containing refractory at present, in-situ preparation such as carbon nanometer
The one-dimensional toughness reinforcing phase structure such as pipe, carbon whisker.When Carbon deposition supersaturation in catalyst granules, carbon atom in the catalyst is dissolved
Start to rearrange to form CNT, the direction of growth is perpendicular to substrate.Result of study shows, catalyst granules particle size with
The ratio of CNT is close to 1: 1.6 (Albert, NasibulinaPeter V, Pikhitsab, HuaJiang.
Correlation between catalyst particle and single-walled carbon nanotube
Diameters.Carbon, 2005,43（11）：2251-2257), in other words growth of the size of catalyst granules for whisker
Influence very big.
The catalyst added in carbon containing refractory is substantially containing a kind of or more in the transition elements such as Fe, Co and Ni
Kind, or co-catalyst is added to increase catalytic action.The species of addition catalyst is roughly divided into three kinds, magnesium-yttrium-transition metal, mistake
Cross family metal oxide and magnesium-yttrium-transition metal salt.Zhu Baiquan etc.（Zhu Baiquan, Li Xiangcheng, Chen Pingan are one-dimensional or two-dimentional combination is relative
The influence refractory materials of carbon containing refractory intensity and toughness, 2017,51（3）：161~171）It was found that nano metal nickel powder is added
Enter inside MgO-C refractory materials can in-situ preparation CNT and MgO whiskers, improve the intensity of MgO-C refractory materials and tough
Property.King is identical（Wang Heng, Li Yawei, Sang Shao cypress Ni superfine microcrystal graphite are to aluminum-carbon refractory material microstructure and mechanical property
The influence artificial lens journals of energy, 2014,43（7）：1815-1822）By way of being directly added into nickel nitrate as catalyst
To be catalyzed the purpose that the mode of aluminum-carbon refractory material in-situ preparation CNT and silicon carbide whisker reaches toughness reinforcing.By directly drawing
Catalysis can be played a part of by entering the mode of the inorganic salts containing transition metal, but the catalytic effect of this catalyst by purity and
The influence of the factors such as particle diameter becomes unstable, and catalytic effect is also not as being directly added into transition metal and metal oxide.
The method for preparing catalyst has：" a kind of modified phenolic resin for fire resistive material and preparation method thereof "
（CN101245128A）Patented technology, the iron or the metal oxide sol presoma of cobalt or nickel prepared with sol-gal process,
Stir 3 ~ 10 hours, be subsequently placed in evaporator under the conditions of 40 ~ 85 DEG C, is added in the phenolic resin diluted with absolute ethyl alcohol
Carry out phenol-formaldehyde resin modified；Cheng Feng etc.（Cheng Feng, Wang Junkai, Tan grasp with Fe2O3For catalyst preparation magnesia crystal whisker .. silicate
Report, 2017,45（3）:459~466）The magnesia powder of uniform load ferric nitrate is made using equi-volume impregnating.It is prepared by this method
Catalyst be to rely on dinectly bruning product Fe2O3As catalyst, the property of calcined product is unstable, and its catalytic action is same
It is unstable.
The content of the invention
It is contemplated that overcome prior art defect, it is therefore an objective to provide that a kind of technique is simple, cost is low and reaction is easy to control
The preparation method of the catalyst of the Mo doped ferric oxides of system, the catalyst particle size of Mo doped ferric oxides is controllable made from this method
And excellent catalytic effect.
For with realizing above-mentioned mesh, the technical solution adopted by the present invention is：By molysite: the mass ratio of molybdate is（50~99）∶
（1~50）, the molysite and the molybdate are dissolved in deionized water respectively, obtain iron salt solutions and molybdate solution；Stirring
The iron salt solutions are homogeneously added into the molybdate solution under the conditions of mixing, obtain mixed solution；Institute is adjusted with ammoniacal liquor
The pH value of mixed solution is stated to 4 ~ 8, is filtered, is produced sediment, the sediment is washed with deionized to neutrality, then at
Dried under the conditions of 110 DEG C, obtain front axle shell；Then the front axle shell is calcined into 0.5 ~ 9h under the conditions of 400 DEG C ~ 900 DEG C, be made
The catalyst of Mo doped ferric oxides；The catalyst particle size of the Mo doped ferric oxides is 0.1 ~ 3.6 μm.
The molysite is one or more of iron chloride, ferric nitrate and ferric sulfate.
The molybdate is one or more of ammonium molybdate and sodium molybdate.
The purity of the molysite is more than technical pure.
The purity of the molybdate is more than technical pure.
The atmosphere of the calcining is air, nitrogen, argon gas, CO2One or both of atmosphere.
Due to there is following good effect compared with prior art using above-mentioned technical proposal, the present invention：
The present invention using molysite and molybdate as raw material, by changing molysite: the mass ratio of molybdate and calcining heat are controlled
The size of system gained catalyst particle size, as a result shows, with the rise of calcining heat, obtains catalyst particle size and becomes big.Catalyst
Particle size energy diameter influence the diameter of growth whisker, so adding the different catalyst energy of particle diameter in carbon containing refractory
Its high-temperature behavior is directly affected, the present invention can efficiently control Fe by way of changing technological parameter2O3Particle size, can
Improve the catalytic effect of the catalyst of Mo doped ferric oxides.
Instant invention overcomes the catalyst of obtained iron oxide under the conditions of no molybdenum easily to occur powder reuniting and very
The problem of iron oxide catalytic effect being inhibited in big degree.The present invention introduces Mo in preparation process, makes transition element molybdenum
Fe can preferably be suppressed2O3The phenomenon of particle agglomeration, good dispersion effect is played, iron oxide is played its catalysis well
Effect, while transition element molybdenum equally has catalytic action, this also makes the catalyst of the Mo doped ferric oxides of the invention prepared
Catalytic effect be better than pure iron oxide catalyst.
The present invention prepares front axle shell using coprecipitation, and preparation process does not have Toxic generation, and technique is simple, and reaction is easy to
Control.
The particle diameter of the catalyst of Mo doped ferric oxides prepared by the present invention is 0.1 ~ 3.6 μm.
Therefore, the present invention is with technique is simple, cost is low and reacts urging for easily controllable, obtained Mo doped ferric oxides
Agent size tunable and excellent catalytic effect.
Brief description of the drawings
Fig. 1 is a kind of SEM image of Mo doped ferric oxides catalyst prepared by the present invention.
Embodiment
The invention will be further described with reference to the accompanying drawings and detailed description, not to the scope of the present invention
Restriction.
It is first that the raw materials used Unify legislation of present embodiment is as follows to avoid repeating, repeated no more in example.
The purity of the molysite is more than technical pure.
The purity of the molybdate is more than technical pure.
Embodiment 1
A kind of catalyst of Mo doped ferric oxides and preparation method thereof.Preparation method is described in the present embodiment：By molysite: molybdate
Mass ratio be（50~70）∶（30~50）, the molysite and the molybdate are dissolved in deionized water respectively, it is molten to obtain molysite
Liquid and molybdate solution；The iron salt solutions are homogeneously added into the molybdate solution under agitation, mixed
Close solution；The pH value for adjusting the mixed solution with ammoniacal liquor filters to 4 ~ 6, sediment is produced, by the sediment deionization
Water washing is dried under the conditions of 110 DEG C to neutrality, obtains front axle shell；Then by the front axle shell under the conditions of 400 ~ 700 DEG C
6 ~ 9h is calcined, the catalyst of Mo doped ferric oxides is made.
The molysite is iron chloride.
The molybdate is ammonium molybdate.
The atmosphere of the calcining is CO2Atmosphere.
For the catalyst of Mo doped ferric oxides manufactured in the present embodiment by scanning electron microscopic observation, particle diameter is 0.1 ~ 1.2 μ
m。
Embodiment 2
A kind of catalyst of Mo doped ferric oxides and preparation method thereof.For preparation method described in the present embodiment in addition to following, remaining is same
Embodiment 1：
The molysite is the mixture of ferric nitrate and ferric sulfate.
The molybdate is sodium molybdate.
The atmosphere of the calcining is air atmosphere.
For the catalyst of Mo doped ferric oxides manufactured in the present embodiment by scanning electron microscopic observation, particle diameter is 0.3 ~ 1.2 μ
m。
Embodiment 3
A kind of catalyst of Mo doped ferric oxides and preparation method thereof.Preparation method is described in the present embodiment：By molysite: molybdate
Mass ratio be（65~85）∶（15~35）, the molysite and the molybdate are dissolved in deionized water respectively, it is molten to obtain molysite
Liquid and molybdate solution；The iron salt solutions are homogeneously added into the molybdate solution under agitation, mixed
Close solution；The pH value for adjusting the mixed solution with ammoniacal liquor filters to 5 ~ 7, sediment is produced, by the sediment deionization
Water washing is dried under the conditions of 110 DEG C to neutrality, obtains front axle shell；Then by the front axle shell under the conditions of 500 ~ 800 DEG C
3 ~ 7h is calcined, the catalyst of Mo doped ferric oxides is made.
The molysite is ferric nitrate.
The molybdate is sodium molybdate.
The atmosphere of the calcining is nitrogen atmosphere.
For the catalyst of Mo doped ferric oxides manufactured in the present embodiment by scanning electron microscopic observation, particle diameter is 1.3 ~ 2.6 μ
m。
Embodiment 4
A kind of catalyst of Mo doped ferric oxides and preparation method thereof.For preparation method described in the present embodiment in addition to following, remaining is same
Embodiment 3：
The molysite is the mixture of iron chloride and ferric sulfate.
The molybdate is ammonium molybdate.
The atmosphere of the calcining is argon gas and CO2Mixed atmosphere.
For the catalyst of Mo doped ferric oxides manufactured in the present embodiment by scanning electron microscopic observation, particle diameter is 1.6 ~ 2.4 μ
m。
Embodiment 5
A kind of catalyst of Mo doped ferric oxides and preparation method thereof.Preparation method is described in the present embodiment：By molysite: molybdate
Mass ratio be（80~99）∶（1~20）, the molysite and the molybdate are dissolved in deionized water respectively, it is molten to obtain molysite
Liquid and molybdate solution；The iron salt solutions are homogeneously added into the molybdate solution under agitation, mixed
Close solution；The pH value for adjusting the mixed solution with ammoniacal liquor filters to 6 ~ 8, sediment is produced, by the sediment deionization
Water washing is dried under the conditions of 110 DEG C to neutrality, obtains front axle shell；Then by the front axle shell under the conditions of 600 ~ 900 DEG C
0.5 ~ 5h is calcined, the catalyst of Mo doped ferric oxides is made.
The molysite is ferric sulfate.
The molybdate is the mixture of ammonium molybdate and sodium molybdate.
The atmosphere of the calcining is argon gas.
For the catalyst of Mo doped ferric oxides manufactured in the present embodiment by scanning electron microscopic observation, particle diameter is 2.6 ~ 3.2 μ
m。
Embodiment 6
A kind of catalyst of Mo doped ferric oxides and preparation method thereof.For preparation method described in the present embodiment in addition to following, remaining is same
Embodiment 5：
The molysite is the mixture of iron chloride, ferric nitrate and ferric sulfate.
The atmosphere of the calcining is nitrogen and CO2Mixed atmosphere.
For the catalyst of Mo doped ferric oxides manufactured in the present embodiment by scanning electron microscopic observation, particle diameter is 2.6 ~ 3.6 μ
m。
Present embodiment has following good effect compared with prior art：
Present embodiment uses molysite and molybdate as raw material, by changing molysite: the mass ratio of molybdate and calcining
Temperature controls the size of gained catalyst particle size, as a result shows, with the rise of calcining heat, obtains catalyst particle size change
Greatly.The particle size energy diameter of catalyst influences the diameter of growth whisker, so it is different that particle diameter is added in carbon containing refractory
Catalyst can directly affect its high-temperature behavior, present embodiment can be efficiently controlled by way of changing technological parameter
Fe2O3Particle size, it is possible to increase the catalytic effect of the catalyst of Mo doped ferric oxides.
Powder easily occurs for the catalyst that present embodiment overcomes obtained iron oxide under the conditions of no molybdenum
The problem of reuniting and inhibiting iron oxide catalytic effect.Present embodiment introduces in preparation process
Mo, transition element molybdenum is set preferably to suppress Fe2O3The phenomenon of particle agglomeration, good dispersion effect is played, enables iron oxide
Its catalytic effect is played well, while transition element molybdenum equally has catalytic action, this also makes present embodiment system
The catalytic effect of the catalyst of standby Mo doped ferric oxides is better than pure iron oxide catalyst.
Present embodiment prepares front axle shell using coprecipitation, and preparation process does not have Toxic generation, and technique is simple,
React easily controllable.
The particle diameter of the catalyst of Mo doped ferric oxides prepared by present embodiment is 0.1 ~ 3.6 μm.Fig. 1 is this implementation
A kind of SEM image of the catalyst of Mo doped ferric oxides prepared by example 3；The grain of the catalyst of Mo doped ferric oxides as can be seen from Figure 1
Footpath is 800nm ~ 1 μm.It can be seen that ferric oxide particles are uniformly dispersed in figure.
Therefore, present embodiment has technique is simple, cost is low and reacts easily controllable, obtained Mo to adulterate oxygen
Change iron catalyst particle size is controllable and excellent catalytic effect.
Claims (5)
1. the preparation method of the catalyst of the Mo doped ferric oxides of a kind of size tunable, it is characterised in that the preparation method is：
By molysite: the mass ratio of molybdate is（50~99）∶（1~50）, the molysite and the molybdate are dissolved in deionized water respectively
In, obtain iron salt solutions and molybdate solution；The iron salt solutions are homogeneously added into the molybdate under agitation
In solution, mixed solution is obtained；The pH value for adjusting the mixed solution with ammoniacal liquor filters to 4 ~ 8, produces sediment, by described in
Sediment is washed with deionized to neutrality, is dried under the conditions of 110 DEG C, is obtained front axle shell；Then the front axle shell is existed
0.5 ~ 9h is calcined under the conditions of 400 DEG C ~ 900 DEG C, the catalyst of Mo doped ferric oxides is made；
The molysite is one or more of iron chloride, ferric nitrate and ferric sulfate；
The molybdate is one or more of ammonium molybdate and sodium molybdate.
2. the preparation method of the catalyst of Mo doped ferric oxides according to claim 1, it is characterised in that the molysite it is pure
Spend to be more than technical pure.
3. the preparation method of the catalyst of Mo doped ferric oxides according to claim 1, it is characterised in that the molybdate
Purity is more than technical pure.
4. the preparation method of the catalyst of Mo doped ferric oxides according to claim 1, it is characterised in that the gas of the calcining
Atmosphere is air, nitrogen, argon gas, CO2One or both of atmosphere.
5. a kind of catalyst of Mo doped ferric oxides, it is characterised in that the catalyst of the Mo doped ferric oxides is will according to right
Ask the catalysis of the Mo doped ferric oxides any one of 1 ~ 4 prepared by the preparation method of the catalyst of Mo doped ferric oxides
Agent；
The catalyst particle size of the Mo doped ferric oxides is 0.1 ~ 3.6 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710834168.6A CN107537510A (en) | 2017-09-15 | 2017-09-15 | A kind of catalyst of Mo doped ferric oxides and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710834168.6A CN107537510A (en) | 2017-09-15 | 2017-09-15 | A kind of catalyst of Mo doped ferric oxides and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107537510A true CN107537510A (en) | 2018-01-05 |
Family
ID=60964217
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710834168.6A Pending CN107537510A (en) | 2017-09-15 | 2017-09-15 | A kind of catalyst of Mo doped ferric oxides and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107537510A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109967736A (en) * | 2019-03-21 | 2019-07-05 | 武汉科技大学 | A kind of Fe2O3@Ni composite granule and preparation method thereof with core-shell structure |
| CN112645731A (en) * | 2021-01-08 | 2021-04-13 | 武汉科技大学 | Lightweight spinel-corundum-carbon refractory material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105457648A (en) * | 2014-09-09 | 2016-04-06 | 中国石油化工股份有限公司 | Iron-molybdenum method formaldehyde synthesis catalyst, and preparation method thereof |
| CN106423182A (en) * | 2016-09-12 | 2017-02-22 | 中南大学 | Preparation method of iron-molybdenum compositely doped oxide |
| CN106495229A (en) * | 2016-10-26 | 2017-03-15 | 武汉科技大学 | The synthetic method of molybdic acid iron powder |
| CN106669705A (en) * | 2016-12-26 | 2017-05-17 | 阳泉煤业（集团）有限责任公司 | Catalyst used for methanol ammoxidation and preparation and forming method thereof |
-
2017
- 2017-09-15 CN CN201710834168.6A patent/CN107537510A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105457648A (en) * | 2014-09-09 | 2016-04-06 | 中国石油化工股份有限公司 | Iron-molybdenum method formaldehyde synthesis catalyst, and preparation method thereof |
| CN106423182A (en) * | 2016-09-12 | 2017-02-22 | 中南大学 | Preparation method of iron-molybdenum compositely doped oxide |
| CN106495229A (en) * | 2016-10-26 | 2017-03-15 | 武汉科技大学 | The synthetic method of molybdic acid iron powder |
| CN106669705A (en) * | 2016-12-26 | 2017-05-17 | 阳泉煤业（集团）有限责任公司 | Catalyst used for methanol ammoxidation and preparation and forming method thereof |
Non-Patent Citations (1)
| Title |
|---|
| SHAODONG QIN ET AL.: "Fe-Mo interactions and their influence on Fischer-Tropsch synthesis performance", 《APPLIED CATALYSIS A: GENERAL》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109967736A (en) * | 2019-03-21 | 2019-07-05 | 武汉科技大学 | A kind of Fe2O3@Ni composite granule and preparation method thereof with core-shell structure |
| CN112645731A (en) * | 2021-01-08 | 2021-04-13 | 武汉科技大学 | Lightweight spinel-corundum-carbon refractory material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US8278240B2 (en) | Method of production of transition metal nanoparticles | |
| CN106587010B (en) | A kind of carbon nano-tube material and preparation method thereof using carbon-clad metal catalyst preparation | |
| Dong et al. | The synthesis of composite powder precursors via chemical processes for the sintering of oxide dispersion-strengthened alloys | |
| JP6369048B2 (en) | Method for producing catalyst for carbon nanotube synthesis and method for producing aggregate of carbon nanotubes | |
| KR20140037441A (en) | Metal catalyst for producing carbon nanotubes and method for preparing carbon nanotubes using thereof | |
| CN109371308B (en) | The method for preparing multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end | |
| CN103695691B (en) | A kind of method preparing refractory foam metal tungsten | |
| CN109731574A (en) | A kind of preparation method of catalyst complex carrier, the catalyst based on the carrier and catalyst | |
| Li et al. | Catalytic preparation of graphitic carbon spheres for Al2O3-SiC-C castables | |
| CN109574081A (en) | One kind having Nanocrystaline spherical molybdic acid iron powder body and preparation method thereof | |
| CN107537510A (en) | A kind of catalyst of Mo doped ferric oxides and preparation method thereof | |
| CN109574082A (en) | A kind of original position core-shell structure molybdic acid iron powder body and preparation method thereof | |
| JP5544503B2 (en) | Marimo carbon and method for producing the same | |
| Ming et al. | A new strategy for finely controlling the metal (oxide) coating on colloidal particles with tunable catalytic properties | |
| CN113798504B (en) | Preparation method of rare earth oxide dispersion-reinforced tungsten powder for 3D printing | |
| Shen et al. | Preparation and characterization of amorphous Cr2O3 nanoparticles obtained by solution plasma discharge | |
| CN108452816A (en) | A kind of small particle metal phosphide nano-particle/reduced form graphene composite material and preparation method thereof | |
| KR20230104343A (en) | Method for manufacturing tungsten carbide particles and tungsten carbide particles prepared therefrom | |
| JP2013103143A (en) | METHOD FOR PRODUCING Co3O4/CeO2 COMPOSITE CATALYST FOR EXHAUST GAS PURIFICATION AND CATALYST OBTAINED BY THE SAME | |
| Fouad et al. | Microwave irradiation assisted growth of Cu, Ni, Co metals and/or oxides nanoclusters and their catalytic performance | |
| Pal et al. | Dipentaerythritol: a novel additive for the precipitation of dispersed Ni particles in polyols | |
| CN109465464A (en) | A method of preparing alumina-based ceramic metal nano composite powder | |
| CN114655945A (en) | Carbon nano tube surface coated amorphous or crystalline chromium oxide nano functional coating and preparation method and application thereof | |
| KR101515065B1 (en) | Method for producing oxide dispersion mixed powder using polyvinyl alcohol and oxide dispersion mixed powder thereby | |
| CN108722414B (en) | Preparation method of thin-wall graphitized carbon-coated metal core-shell structure material |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180105 |