CN105274577A - High purity metal preparation electrolysis bath and use method thereof - Google Patents
High purity metal preparation electrolysis bath and use method thereof Download PDFInfo
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- CN105274577A CN105274577A CN201410232316.3A CN201410232316A CN105274577A CN 105274577 A CN105274577 A CN 105274577A CN 201410232316 A CN201410232316 A CN 201410232316A CN 105274577 A CN105274577 A CN 105274577A
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Abstract
The invention relates to a high purity metal preparation electrolysis bath and a use method thereof. According to the high purity metal preparation electrolysis bath, a material inlet pipe is arranged on the upper portion of the electrolysis bath, the inlet of the material inlet pipe is externally connected to a liquid storage groove, the side surface of the upper portion of the electrolysis bath is provided with an overflow port communicated to an overflow zone, the bottom portion of the overflow zone is provided with an overflow hole, the overflow hole is externally connected to a regeneration groove, a flow baffle is arranged inside the electrolysis bath, the electrolysis bath is isolated into a flow baffle zone and an electrolysis zone through the flow baffle, paired groups of snapping groove plates are arranged inside the electrolysis zone, the outlet end of the material inlet pipe is arranged or toward the flow baffle zone, the outer portion of the electrolysis bath is additionally provided with a heatable water bath groove, the electrolysis bath is positioned in the water bath groove and is isolated from the water bath groove, and the bottom portion of the water bath groove is provided with a water inlet hole and a water outlet hole. According to the present invention, during the use, the water bath groove is heated by the heater, the electrolyte enters through the gap on the bottom portion of the flow baffle zone and is gradually filled into the electrolyte bath from bottom to top, and when the liquid level achieves the overflow plate interface, the electrolyte flows into the overflow zone and flows into the externally-connected regeneration groove through the overflow hole; and the problems of unsmooth transmission, unbalanced concentration, sticking on the bag and the like of the electrolyte in the traditional technology can be overcome.
Description
Technical field
The invention belongs to correlative technology field prepared by high pure metal, particularly one prepares high pure metal electrolyzer.
Background technology
Along with the development of new and high technology, high pure metal due to the application in modern material Science and engineering field of the performance of its uniqueness more and more extensive, market demand constantly increases.
The technique that the preparation of high pure metal needs the method such as pyrogenic process, wet method to combine can prepare colory high pure metal.The preparation method of current high pure metal has extraction process, ion exchange method, electrolytic process and vacuum melting method etc.
Aqueous electrolysis in electrolysis occupies main status in high pure metal preparation technology.Feed liquid after purification carries out electrolytic deposition again, can remove the electromotive force metallic impurity more negative than purifying metals further.
The multiplex diaphragm sell of electrolyzer of modern aqueous electrolysis.The minimizing of the electrode surface area in the unit volume caused by the use adopting the technology such as diffusion anodes, modified diaphragm to reduce barrier film, barrier film penetrates, barrier film glues bag, interpole gap increases and the problem such as bath voltage rising, to improve the production intensity of electrolyzer, improve current efficiency.
The electrolytic process of some metals needs to control electrolysis temperature.Usually the electrolytic solution by adding certain temperature in electrolyzer realizes (adopting certain mode, pour electrolyzer after being heated in advance by electrolytic solution again into or heat electrolytic solution in external circulation groove), because electrolyzer itself does not have heating design, so the electrolyte temperature entering electrolyzer cannot keep constant, the instability of electrolyte temperature in electrolytic process will be caused like this.The old liquid of electrolysis is got back in stoste without cycle for the treatment of and is recycled together, easily causes the accumulative precipitation of the difference of concentration of electrolyte and some foreign ions, reduces current efficiency, affects the purity of product.
At present, the preparation abroad for high pure metal cobalt mainly adopts ion exchange method to remove most of impurity in solution, then obtains cobalt metal by electrolysis, then is purified further by methods such as district's melting, electron beam meltings.Domestic main in ion-exchange and electrorefining.Wherein electrolysis adopts aqueous electrolysis.Therefore, being optimized design to cell construction, choose reasonable electrode, diaphragm material, is the key improving current efficiency, reduce bath voltage and saving energy consumption.
Summary of the invention
The object of this invention is to provide one and prepare high pure metal electrolyzer, it is the improvement made for the deficiency preparing high pure metal electrolyzer adopted at present.
For achieving the above object, the present invention takes following design:
One prepares high pure metal electrolyzer, comprise an electrolyzer body, the top of electrolyzer is provided with a feed-pipe, the external electrolytic solution reservoir of inlet end of this feed-pipe, upper part of the electrolytic cell side has overflow port and communicates with flooded zonevvv, opens overflow weir bottom this district, the external regeneration tank of overflow weir, the bottom of flooded zonevvv has an overflow weir, and this overflow weir is communicated with external regeneration tank;
Described electrolyzer built with vertical directly to flow-stopping plate, by this flow-stopping plate, electrolyzer is isolated into baffle district and electrolysis zone; The paired group of clamping groove plate for putting some electrodes is installed in the electrolysis zone of electrolyzer;
The exit end of described feed-pipe is located in baffle district or towards baffle district;
Add a heatable water bath in the outside of electrolyzer, this electrolyzer to be seated in water bath and to separate with water bath, is provided with prosopyle and posticum bottom this water bath.
Describedly prepare in high pure metal electrolyzer, described electrolyzer is separated by the back up pad of bottom and water bath.
Describedly to prepare in high pure metal electrolyzer, well heater is housed to form heatable water bath in the water-bath interlayer formed between electrolyzer and water bath.
Describedly prepare in high pure metal electrolyzer, the upper edge of described flow-stopping plate is concordant with electrolyzer, and the left and right end of flow-stopping plate is connected with electrolyzer, and lower end and bottom of electrolytic tank leave gap; The gap that shelves stream plate lower end and bottom of electrolytic tank leave is not more than 1cm.
Describedly prepare in high pure metal electrolyzer, in side, baffle district, shelves stream plate is 1-3cm apart from the distance of electrolyzer inwall.
Describedly prepare in high pure metal electrolyzer, described paired group of clamping groove plate comprises the upper and lower clamping groove plate of two couples in the two opposite side walls being arranged on upper part of the electrolytic cell and bottom respectively, each upper and lower clamping groove plate all has same quantity and the draw-in groove with orientation; And preferred version is: the groove depth that described lower bayonet slot plate is offered is 1/3 of cell body height.
Describedly prepare in high pure metal electrolyzer, described in be arranged on electrolyzer internal upper part upper clamping groove plate position be not less than overflow port, lower bayonet slot plate bottom, bottom and shelves stream plate bottom are consistent apart from the distance of bottom of electrolytic tank.Too low, because the distance of shelves stream plate and bottom of electrolytic tank is not more than 1cm, clamping groove plate is low imply that the battery lead plate be stuck in wherein is low, electrode cathode plate bottom margin in electrolytic process will be grown up on the one hand, this grows up likely even to downward-extension (this distance can not more than 0.5cm), also branch shape is likely grown up to, if do not have enough spaces to extend downwards, will crosswisely develop, be easy to be communicated with cathode-anode plate (be spaced apart 1-3cm between cathode-anode plate, once dendrite generates, can grow very fast, rapid conducting anode and cathode, is short-circuited; On the other hand, if lower than shelves stream plate, some is understood by pole plate then in draw-in groove, especially the pole plate in the part draw-in groove of shelves stream plate just loses shelves stream plate to the shock absorption of electrolytic solution, pole plate bottom when being equivalent to electrolysis can be subject to the impact of electrolytic solution too much, pole plate is in the electrolytic solution of fluctuation all the time, can cause the change of electric current like this, makes precipitation product surface uneven; If clamping groove plate flows plate higher than shelves, the liquid level of electrolytic solution uprises, and needs more electrolytic solution that pole plate just can be made to immerse in the electrolytic solution comparatively speaking, easily causes the waste of electrolytic solution.
Another object of the present invention is to provide a kind of using method preparing high pure metal electrolyzer, and its method is as follows:
1) first preparing described above, any one prepares high pure metal electrolyzer;
2) in water bath, add tap water by water inlet pipe, when the water level in water bath arrives flooded zonevvv bottom level, heater heats;
3) start feed process, electrolytic solution joins baffle district by feed-pipe, allows electrolytic solution enter electrolyzer by the breach bottom baffle district;
4) electrolytic solution entering electrolyzer is progressively full of electrolyzer from the bottom to top, and when liquid level of electrolyte arrives overflow plate interface, electrolytic solution flows into flooded zonevvv, and the electrolytic solution of flooded zonevvv flows into external regeneration tank by outlet overflows hole; Electrolytic solution now in electrolyzer reaches equilibrium state, after the electrolyte temperature in electrolyzer also arrives predetermined temperature, is inserted into successively in clamping groove plate by battery lead plate, carries out electrolysis.
Another object of the present invention is to provide a kind of purposes of above-mentioned high pure metal electrolyzer, for realizing the preparation of high-purity cobalt.
Describedly prepare in high pure metal electrolyzer, the electrolytic solution in described electrolyzer adopts one-way circulation.
The present invention is utilized to prepare high pure metal electrolyzer, by the improvement to electrolyte flow, heating and electrolytic solution substitute mode etc., improve the temperature of electrolytic solution, maintain the consistence of concentration of electrolyte, more highly purified metal product can be prepared further, belong to high pure metal field of material preparation.
Advantage of the present invention is:
1. outside water bath heating can improve the temperature of electrolytic solution, is conducive to the transmission of ion, plays good promoter action to raising current efficiency;
2. it is simple, convenient and install compactly that the clamping groove plate in inside groove electrolyzer is beneficial to battery lead plate, and can adjust interpole gap easily as required;
3. the flow-stopping plate in electrolyzer can overcome that the transmission of the electrolytic solution that tradition uses barrier film and diaphragm bag to cause is smooth, density unevenness weighing apparatus and glue the problems such as bag, the existence of shelves stream plate makes electrolytic solution internal stability, efficiently avoid solution and to fluctuate the difference of the concentration of electrolyte brought;
4. the single loop system of electrolytic solution makes concentration of electrolyte maintain balance all the time with the requirement meeting electrolysis tech, effectively prevent that the electrolytic solution in negative and positive district in electrolyzer pollutes mutually, the accumulation of foreign metal separates out, improve current efficiency, reduce bath voltage, save energy consumption and obtain more highly purified product.
Accompanying drawing explanation
Fig. 1 is electrolyzer one embodiment agent structure schematic diagram of the present invention (broken section, A-A to).
Fig. 2 is invention electrolyzer general assembly front view.
Fig. 3 is invention electrolyzer general assembly vertical view.
Fig. 4 is the scheme of installation of invention electrode plate of electrolytic tank in draw-in groove.
In figure: 1-water bath; 2-electrolyzer; The upper clamping groove plate of 3-; 4-lower bayonet slot plate; The water inlet pipe of 5-water bath; 6-flooded zonevvv; 7-back up pad; 8-wash-out hole; 9-overflow weir; 10-feed-pipe; 11-water shoot; The upper clamping groove plate of 12-; 13-lower bayonet slot plate; 14-flow-stopping plate; 15-battery lead plate; 16-well heater; 17-temperature sensor; Bottom 18-flooded zonevvv.
Below in conjunction with drawings and the specific embodiments, the present invention is described in further details.
Embodiment
Consult shown in Fig. 1, Fig. 2 and Fig. 3, the present invention mainly creates and is a little: prepare high pure metal electrolyzer and adopt inside and outside two-layer, skin is heatable water bath 1, and internal layer is with the electrolyzer 2 of purifying further for the preparation of high pure metal.The electrolyzer 2 of internal layer to be seated in water bath 1 by the back up pad 7 of bottom and to separate with water bath.
The bottom of described outer field water bath 1 is provided with prosopyle 5 and posticum 11; Well heater 16 is housed, the regulation and control that can realize well heater 16 working order by temperature control unit in heating interlayer, so that temperature required when the temperature of electrolytic solution in electrolyzer remains on better working order can be maintained; Separately can also be equipped with the temperature sensor 17 that is connected to display panel in electrolyzer, water bath, to realize the real-time monitoring to temperature; Temperature control and display are prior art and can realize, and do not repeat herein.
Another creation point of the present invention is the improvement to electrolyte bath structure:
In electrolyzer of the present invention, electrolytic solution adopts not reusable one-way circulation system, and the top of electrolyzer is provided with a feed-pipe 10, and the external electrolytic solution reservoir of inlet end of feed-pipe, electrolyzer is also provided with wash-out hole 8 and discharges for by cleaning materials.Flow-stopping plate 14 is provided with at electrolyte bath, the upper edge of described flow-stopping plate 14 is concordant with cell body upper end edge, the left and right end of flow-stopping plate 14 is connected with cell wall, thus, electrolyzer is isolated two regions by this flow-stopping plate 14: baffle district A and electrolysis zone B, and see Fig. 3, flow-stopping plate 14 and bottom land do not connect, gap will be left with bottom of electrolytic tank in its lower end, and this gap is greater than 1cm.The exit end of electrolyzer feed pipe 10 is located in baffle district or towards baffle district; Within shelves stream plate 14 is 1-3cm apart from the distance of electrolyzer inwall; In electrolysis zone, being provided with the paired group of clamping groove plate for putting some electrodes, comprising two kinds of clamping groove plates, a kind of is upper clamping groove plate 3,12 logical in draw-in groove, is arranged on electrolyzer internal upper part; Another kind of clamping groove plate is groove depth is that difference is penetrating, the lower bayonet slot plate 4,13 of closed bottom, is arranged on bottom in electrolyzer; The installation of these clamping groove plates divides two groups, one group (clamping groove plate 3,4) is arranged on the avris inwall of electrolyzer 1, another group (clamping groove plate 12,13) is arranged on the shelves stream plate 14 in electrolyzer, two groups of clamping groove plates are on relative two faces, see Fig. 4, each upper and lower clamping groove plate all has same quantity and the draw-in groove with orientation; And preferred version is: the groove depth that described lower bayonet slot plate 4,13 is offered is 1/3 of cell body height.
Preferably, lower bayonet slot plate (the lower bayonet slot plate 4,13 in the figure) bottom of bottom of electrolytic tank and the distance of shelves stream plate bottom distance bottom of electrolytic tank will be consistent.Too low, because the distance of shelves stream plate and bottom of electrolytic tank is not more than 1cm, clamping groove plate is low imply that the battery lead plate be stuck in wherein is low, electrode cathode plate bottom margin in electrolytic process will be grown up on the one hand, this grows up likely even to downward-extension (this distance can not more than 0.5cm), also branch shape is likely grown up to, if do not have enough spaces to extend downwards, will crosswisely develop, be easy to be communicated with cathode-anode plate (being spaced apart 1-3cm between cathode-anode plate), once dendrite generates, can grow very fast, rapid conducting anode and cathode, is short-circuited; On the other hand, if lower than shelves stream plate, some is understood by pole plate then in draw-in groove, especially the pole plate in the part draw-in groove of shelves stream plate just loses shelves stream plate to the shock absorption of electrolytic solution, pole plate bottom when being equivalent to electrolysis can be subject to the impact of electrolytic solution too much, pole plate is in the electrolytic solution of fluctuation all the time, can cause the change of electric current like this, makes precipitation product surface uneven; If clamping groove plate flows plate higher than shelves, the liquid level of electrolytic solution uprises, and needs more electrolytic solution that pole plate just can be made to immerse in the electrolytic solution comparatively speaking, easily causes the waste of electrolytic solution.
See Fig. 2, Fig. 3, for electrolyzer sets up a flooded zonevvv 6, flooded zonevvv (bottom) offers overflow weir 9, and the external regeneration tank of this overflow weir 9, to carry out reprocessing.
Referring to Fig. 4, is the scheme of installation in the upper and lower clamping groove plate of battery lead plate 15 in electrolyzer 2.Battery lead plate 15 passes left and right two draw-in grooves 3,12 in top, is seated in left and right two draw-in grooves 4,13 in bottom.These clamping groove plates secure the position of battery lead plate 15 well, avoid rocking of battery lead plate, and grafting is convenient, easy, according to the requirement to battery lead plate interval, whether select to insert in the groove of each paired group or interval insertion, use more convenient, range of application is wider.
Principle of work of the present invention and working process are:
High pure metal electrolyzer prepared by the present invention to install shown in the overall wiring layout of Fig. 1, tap water joins in water bath by water inlet pipe 5, when the water level in water bath arrives flooded zonevvv bottom level, opens water-bath heating system heats.Electrolytic solution after purification joins baffle district A by recycle pump by feed-pipe 10, and electrolytic solution can make solution be full of the electrolysis zone B of electrolyzer from the bottom to top by the breach bottom shelves stream plate 14 with more stable state by baffle district.When liquid level of electrolyte to electrolyzer side overflow port constantly, electrolytic solution flow into flooded zonevvv 6,18 be the bottom of flooded zonevvv, the electrolytic solution of flooded zonevvv flows into reprocessing in external regeneration tank by outlet overflows hole 9.After the electrolyte temperature in electrolyzer arrives technical requirements temperature, battery lead plate is inserted in clamping groove plate successively, carries out electrolysis.After electrolysis terminates, battery lead plate can be taken out easily in the direction along draw-in groove.The single loop system of the water bath in this electrolyzer, electrolytic solution makes not only to make the temperature of electrolytic solution can require to adjust according to electrolysis tech in electrolytic process, to ensure the stability of electrolyte temperature in electrolytic process, and electrolytic solution is in single loop state, ensure that the purity of electrolytic solution, avoid the accumulation of electrolytic solution foreign ion and affect the purity of product, effectively improve current efficiency and product purity.
The main application that the present invention prepares high pure metal electrolyzer is for the preparation of purification process during high-purity cobalt, the high-purity cobalt chloride solution preparing high-purity cobalt is passed into the present invention to prepare in high pure metal electrolyzer and to carry out single loop electrolytic deposition, concrete electrolyting precipitation process is:
1) first select and standby go out titanium plate cathode, titanium be coated with the high-purity cobalt solution that the anode of ruthenium material and enough pH values are 2.5 ~ 4.5, high-purity cobalt solution is poured into or is introduced in electrolytic solution reservoir;
2) high-purity cobalt solution flows in the electrolyzer of internal layer from bottom to top by flow-stopping plate slowly, at the uniform velocity and in appropriate amount, enters flooded zonevvv and enters waste liquid tank by outlet again, no longer recycle after being full of electrolyzer by the overflow port outflow of upper side;
3) utilize the water in water bath to heat, make the high-purity cobalt solution temperature in electrolyzer remain on 50 ~ 60 DEG C, during electrolysis, electrode current density is 100 ~ 300A/m (referring to that negative plate is immersed in the cathode current density of anolyte portion);
4) insert negative electrode, anode electrode plate, prepare high-purity electrodeposited cobalt.
In the inventive method, the electrolytic solution prepared in high pure metal electrolyzer is in single loop, not reusable measurement circulation, that is the high-purity cobalt solution added in electrolyzer be all fresh, there is no used solution, this feed way can maintain the concentration balance of cobalt liquor in groove, avoids the enrichment of impurity; Electrolyzer can heat as required, to maintain temperature equilibrium in groove, improves current efficiency.
In step 2, high-purity cobalt solution after concentrated can continuously, in right amount, be full of electrolyzer by flow-stopping plate slowly, equably from bottom of electrolytic tank from bottom to up evenly after to be overflow by top and stay mouth to flow out not recirculation to use, there is not large change in volume, the concentration that can maintain electrolytic solution like this, the concentration of cobalt liquor in whole electrolyzer maintains relative balance state, avoids the enrichment of the impurity that circulation of elecrolyte uses the change in concentration brought to cause.Concentration, pH value, solution temperature, single loop speed, flow direction etc. through conservative control cobalt liquor effectively can keep the stable of cobalt liquor concentration in electrolyzer, temperature, foreign matter content, thus ensure the purity of product.
It is emphasized that, the electrolyzer used in electrodeposition process prepared by the present invention and high-purity cobalt involved before the technology of the present invention is very different, the electrolyzer that prior art openly uses substantially all is diaphragm sell and all can not heats, new and old circulation of elecrolyte uses, concentration of electrolyte and temperature instability, these factors bring the reduction of current efficiency and the accumulation of impurity substances to separate out, and affect the purity of product.The present invention is by controlling, adjusting the Recycle design of electrodeposition process such as electrolytic solution, the inserted mode of pole plate, the heating parameters of electrolytic solution etc. keep the balance of concentration of electrolyte, temperature etc., successfully solve the impurity enriched problem that concentration of electrolyte difference band comes, reduce cost, prevent the crossed contamination of electrolytic solution.
The various embodiments described above can not to depart under protection scope of the present invention in addition some changes, thus above explanation to comprise and the structure shown in accompanying drawing should be considered as exemplary, and be not used to the protection domain limiting the present patent application patent.
Claims (10)
1. prepare high pure metal electrolyzer for one kind, comprise an electrolyzer body, the top of electrolyzer is provided with a feed-pipe, the external electrolytic solution reservoir of inlet end of this feed-pipe, upper part of the electrolytic cell one side has the overflow port communicated with flooded zonevvv, have an overflow weir in the bottom of flooded zonevvv, this overflow weir is communicated with external regeneration tank; It is characterized in that:
Inside described electrolyzer, distance side plate 1-3cm place is equipped with one piece of flow-stopping plate parallel with side plate, by this flow-stopping plate, electrolyzer is isolated into baffle district and electrolysis zone; The paired group of clamping groove plate for putting some electrodes is installed in the electrolysis zone of electrolyzer;
The exit end of described feed-pipe is located in baffle district or towards baffle district;
Add a heatable water bath in the outside of electrolyzer, this electrolyzer to be seated in water bath and to separate with water bath, is provided with prosopyle and posticum bottom this water bath.
2. prepare high pure metal electrolyzer as claimed in claim 1, it is characterized in that: described electrolyzer is separated by the back up pad of bottom and water bath.
3. prepare high pure metal electrolyzer as claimed in claim 1, it is characterized in that: described flooded zonevvv is the external groove in electrolyzer one side, and the other side of groove connects with water bath inwall and makes whole regional cross water crossing bathe interlayer.
4. prepare high pure metal electrolyzer as claimed in claim 1, it is characterized in that: the upper edge of described flow-stopping plate is concordant with electrolyzer, the left and right end of flow-stopping plate is connected with electrolyzer, and lower end and bottom of electrolytic tank leave gap.
5. prepare high pure metal electrolyzer as claimed in claim 4, it is characterized in that: in side, baffle district, shelves stream plate is 1-3cm apart from the distance of electrolyzer inwall; The gap that shelves stream plate lower end and bottom of electrolytic tank leave is not more than 1cm.
6. prepare high pure metal electrolyzer as claimed in claim 1, it is characterized in that: described paired group of clamping groove plate comprises the upper and lower clamping groove plate of two couples in the two opposite side walls being arranged on upper part of the electrolytic cell and bottom respectively, each upper and lower clamping groove plate all has the draw-in groove in same quantity and corresponding orientation.
7. prepare high pure metal electrolyzer as claimed in claim 6, it is characterized in that: the groove depth that described lower bayonet slot plate is offered is 1/3 of clamping groove plate height.
8. prepare high pure metal electrolyzer as claimed in claim 1, it is characterized in that: described in be arranged on electrolyzer internal upper part upper clamping groove plate position be not less than overflow mouth region, the bottom of the lower bayonet slot plate of bottom and shelves stream plate bottom are consistent apart from the distance of bottom of electrolytic tank.
9. prepare a using method for high pure metal electrolyzer, it is characterized in that method is as follows::
1) first any one as described in claim 1 to claim 8 of preparation prepares high pure metal electrolyzer;
2) in water bath, add tap water by water inlet pipe, when the water level in water bath arrives flooded zonevvv bottom level, heater heats;
3) start feed process, electrolytic solution joins baffle district by feed-pipe, allows electrolytic solution enter electrolyzer by the breach bottom baffle district;
4) electrolytic solution entering electrolyzer is progressively full of electrolyzer from the bottom to top, and when liquid level of electrolyte arrives overflow plate interface, electrolytic solution flows into flooded zonevvv, and the electrolytic solution of flooded zonevvv flows into external regeneration tank by outlet overflows hole; Electrolytic solution now in electrolyzer reaches equilibrium state, after the electrolyte temperature in electrolyzer also arrives predetermined temperature, is inserted into successively in clamping groove plate by battery lead plate, carries out electrolysis.
10. any one as described in claim 1 to claim 8 prepares a purposes for high pure metal electrolyzer, for realizing the preparation of high-purity cobalt.
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| CN201410232316.3A CN105274577A (en) | 2014-05-28 | 2014-05-28 | High purity metal preparation electrolysis bath and use method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109722676A (en) * | 2019-01-23 | 2019-05-07 | 刘蕊 | Combined electrolysis slot |
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Application publication date: 20160127 |
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| RJ01 | Rejection of invention patent application after publication |