CN113145057A - Acid dissolution reactor, equipment and method for preparing nickel sulfate - Google Patents
Acid dissolution reactor, equipment and method for preparing nickel sulfate Download PDFInfo
- Publication number
- CN113145057A CN113145057A CN202110588297.8A CN202110588297A CN113145057A CN 113145057 A CN113145057 A CN 113145057A CN 202110588297 A CN202110588297 A CN 202110588297A CN 113145057 A CN113145057 A CN 113145057A
- Authority
- CN
- China
- Prior art keywords
- valve
- liquid
- tank body
- acid
- nickel
- 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
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/10—Sulfates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
When dilute sulfuric acid is sprayed out from a nozzle, negative pressure is generated in a tee pipe under the action of jet flow, air is sucked from an air suction pipe, the sucked air is instantly mixed with the dilute sulfuric acid to form a large number of tiny bubbles, and when the bubbles enter the reactor along with sulfuric acid and flow through the surface of metal nickel, a hydrogen layer formed on the surface of the metal nickel when the metal nickel reacts with the sulfuric acid can be damaged due to the expansion and crushing action of the bubbles and the scouring action of the sulfuric acid on the surface of the metal nickel, so that the reaction speed of the metal nickel and the sulfuric acid can be accelerated.
Description
Technical Field
The invention belongs to the technical field of nickel sulfate preparation, and particularly relates to an acid-soluble reactor, equipment and a method for preparing nickel sulfate.
Background
Nickel sulfate is an important raw material for industries such as batteries, electroplating, printing and dyeing, catalysts and the like, and the production of nickel sulfate by utilizing metal nickel is one of common methods. The metal nickel which can be used for preparing the nickel sulfate at present comprises electrolytic nickel, nickel powder, nickel pills, nickel pillows and the like, and the metal nickel needs to be dissolved into nickel sulfate solution by sulfuric acid and then purified. The passivation layer on the surface of the metal nickel and the hydrogen bubbles formed on the surface of the metal nickel during reaction can prevent the reaction of the sulfuric acid and the nickel, so that the dissolution speed of the metal nickel in the sulfuric acid solution is reduced, and the production requirement cannot be met.
Disclosure of Invention
The invention aims to: provides an acid-soluble reactor, equipment and a method for preparing nickel sulfate, which can improve the reaction speed and meet the production requirement.
The technical scheme adopted by the invention is as follows:
an acid-soluble reactor for preparing nickel sulfate comprises a tank body, a tank cover covered on the top of the tank body, a jet flow inflating device and a porous grid plate;
the lower part of the tank body is respectively provided with a drain outlet and a liquid inlet, the drain outlet is provided with a drain valve, the upper part of the tank body is respectively provided with an inflation inlet and a liquid outlet, and the position of the liquid outlet is lower than that of the inflation inlet;
the jet flow inflating device comprises a three-way pipe, and a nozzle, an air suction pipe and a conveying pipe which are connected to the three-way pipe, wherein the nozzle and the conveying pipe are coaxially arranged, and the conveying pipe is connected with the liquid inlet;
the porous grid plate is arranged at the bottom in the tank body and is fixed with the tank body, a gap is formed between the porous grid plate and the inner bottom wall of the tank body, and a plurality of through holes are formed in the porous grid plate at equal intervals;
the liquid inlet is lower than the porous grid plate.
The further technical proposal is that the tank cover is provided with an exhaust pipe.
The technical scheme is that the tank body is provided with an interlayer, and a heat insulation material is arranged in the interlayer.
The further technical proposal is that the air suction pipe is provided with an air suction valve.
The further technical proposal is that the nozzle is provided with a liquid inlet valve.
The technical scheme is that the nozzle is provided with a conical inner hole, the end with the large diameter of the inner hole is an inlet, and the end with the small diameter of the inner hole is an outlet.
An acid-soluble reaction device for preparing nickel sulfate, comprising the acid-soluble reactor for preparing nickel sulfate as claimed in claim 6, and further comprising a storage tank, a pump, a flow meter and a heater which are connected in sequence by means of pipelines; the heater is connected with the nozzle through a pipeline; the storage tank is connected with the liquid outlet by a pipeline; a pump inlet valve is arranged on a pipeline between the storage tank and the pump; a return pipeline is connected between the storage tank and the pump, and a return valve is arranged on the return pipeline; a liquid supply valve is arranged on a pipeline between the pump and the flowmeter; a liquid discharging pipe is arranged on the storage tank, and a liquid discharging valve is arranged on the liquid discharging pipe.
The method for preparing the nickel sulfate by using the acid dissolution reaction equipment for preparing the nickel sulfate comprises the following steps:
step a: closing the drain valve, the liquid supply valve and the liquid discharge valve, and opening the reflux valve, the suction valve, the liquid inlet valve and the pump inlet valve;
step b: filling dilute sulfuric acid in the storage tank, placing the metal nickel on the porous grid plate, and filling displacement gas into the tank body from the gas filling port to discharge air in the tank body;
step d: opening a liquid supply valve, starting a pump, closing a reflux valve, adjusting a liquid inlet valve to enable the liquid level in the reactor to be always maintained at the height of a liquid outlet, adjusting an air suction valve to control the amount of bubbles on the liquid level in the reactor, starting a heater for heating, and then opening the reflux valve;
step e: detecting the content of nickel ions in the solution in the storage tank, opening a liquid discharge valve to discharge part of the solution after the content of the nickel ions meets the requirement, closing the liquid discharge valve after the solution is discharged, and supplementing dilute sulfuric acid into the storage tank;
step f: concentrating and crystallizing the discharged partial solution to generate nickel sulfate crystals.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. when the dilute sulfuric acid is sprayed out from the nozzle, negative pressure is generated in the tee pipe under the action of jet flow, air is sucked from the air suction pipe, the sucked air is instantly mixed with the dilute sulfuric acid to form a large number of tiny bubbles, and the tiny bubbles enter the reactor along with the sulfuric acid, when the bubbles flow through the surface of the metal nickel, a hydrogen layer formed on the surface of the metal nickel when the metal nickel reacts with the sulfuric acid can be damaged due to the expansion and crushing action of the bubbles and the scouring action of the sulfuric acid on the surface of the metal nickel, and the reaction speed of the metal nickel and the sulfuric acid can be accelerated.
2. The valve on the air suction pipe can adjust the air suction amount, and further can control the air bubble amount.
3. The solution adopts an external heating mode, and is heated in the process of conveying the dilute sulfuric acid, so that the structures of the tank body and the storage tank can be simplified, heating devices do not need to be arranged on the tank body and the storage tank, the dilute sulfuric acid can be heated when the dilute sulfuric acid is contacted with the metal nickel, and the reaction speed can be accelerated.
4. Because the air sucked by the jet flow inflating device and the replacement gas are filled, the concentration of the hydrogen in the tank body can be diluted, and the explosion danger is avoided.
5. The tank body has a simple structure, and no moving part such as a stirrer is arranged in the tank body, so that the service life is longer.
6. Because the sulfuric acid flows through the metallic nickel upwards at the lower part of the porous grid plate, the contact area of the sulfuric acid solution and the metallic nickel can be increased, the flowing dead zone is avoided, and the reaction is facilitated.
7. The method for preparing the nickel sulfate by the acid dissolution reaction equipment for preparing the nickel sulfate not only can accelerate the reaction speed of the metal nickel and the sulfuric acid, but also can discharge part of the subsequent dilute sulfuric acid by the nickel ions in the storage tank after reaching the standard as long as the metal nickel put into the tank is enough, so that the operation is repeated, the operation in the whole process is simple, and the preparation efficiency of the nickel sulfate is accelerated.
Drawings
FIG. 1 is a schematic diagram of the structure of an acid-soluble reactor for preparing nickel sulfate according to the present invention;
FIG. 2 is a schematic view of the jet inflator of the present invention;
FIG. 3 is a schematic structural diagram of an acid-soluble reaction apparatus for preparing nickel sulfate according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments.
As shown in fig. 1-3, an acid dissolution reactor for preparing nickel sulfate comprises a tank body 4, a tank cover 9 covering the top of the tank body 4, a jet aeration device 15 and a porous grid plate 17;
the lower part of the tank body 4 is respectively provided with a sewage draining outlet 5 and a liquid inlet 14, the sewage draining outlet 5 is provided with a sewage draining valve 6, the upper part of the tank body 4 is respectively provided with an inflation inlet 7 and a liquid outlet 11, and the position of the liquid outlet 11 is lower than that of the inflation inlet 7;
the jet flow aerating device 15 comprises a three-way pipe 18, and a nozzle 20, an air suction pipe 13 and a delivery pipe 19 which are connected to the three-way pipe 18, wherein the nozzle 20 and the delivery pipe 19 are coaxially arranged, and the delivery pipe 19 is connected with a liquid inlet 14;
the porous grid plate 17 is arranged at the bottom in the tank body 4 and fixed with the tank body, a gap is arranged between the porous grid plate 17 and the inner bottom wall of the tank body 4, a plurality of through holes are arranged on the porous grid plate 17 at equal intervals,
the liquid inlet 14 is positioned below the porous grid plate 17.
The bottom of the tank body 4 is provided with a bracket 1.
The metal nickel is placed on the porous grid plate 17, the nozzle 20 is connected with a pipeline for dilute sulfuric acid, the dilute sulfuric acid is sprayed out from the inside of the nozzle 20, negative pressure is generated in the three-way pipe 18 due to the action of jet flow, air is sucked from the air suction pipe 13, the sucked air is instantly mixed with the dilute sulfuric acid to form a large number of tiny bubbles, the tiny bubbles enter the reactor along with the sulfuric acid, and when the bubbles flow through the surface of the metal nickel, a hydrogen layer formed on the surface of the metal nickel when the metal nickel reacts with the sulfuric acid can be damaged due to the expansion and crushing action of the bubbles and the scouring action of the sulfuric acid on the surface of the metal nickel; and because metal nickel is placed on porous grid plate 17 and can make its contact surface increase with dilute sulfuric acid, dilute sulfuric acid can play the scouring action to metal nickel after coming out from the via hole on porous grid plate 17 moreover.
The tank cover 9 is provided with an exhaust pipe 10 to prevent the gas pressure inside the tank body 4 from being too high.
The tank body 4 is provided with an interlayer, the interlayer is internally provided with a heat insulation material 2, and the heat insulation material 2 is a ceramic fiber blanket, an aluminum silicate felt, alumina, silicon carbide fiber, aerogel felt, glass wool or rock wool and the like, and can achieve the heat insulation effect.
The air suction pipe 13 is provided with an air suction valve 12, and the flow rate can be adjusted through the air suction valve 12.
The nozzle 20 is provided with a liquid inlet valve 16. The amount of dilute sulfuric acid sprayed from the nozzle 20 can be controlled and adjusted by the liquid inlet valve 16.
The nozzle 20 is provided with a conical inner hole 21, one end with the large diameter of the inner hole 21 is an inlet, and the other end with the small diameter of the inner hole is an outlet, so that the nozzle 20 can spray dilute sulfuric acid.
An acid dissolution reaction device for preparing nickel sulfate, comprising the acid dissolution reactor 22 for preparing nickel sulfate according to claim 6, and further comprising a storage tank 23, a pump 24, a flow meter 25 and a heater 26 which are connected in sequence by means of pipelines; the heater 26 is connected with the nozzle 20 through a pipeline; the storage tank 23 is connected with the liquid outlet 11 by a pipeline; a pump inlet valve 27 is arranged on a pipeline between the storage tank 23 and the pump 24; a return pipeline 28 is connected between the storage tank 23 and the pump 24, and a return valve 29 is arranged on the return pipeline 28; a liquid supply valve 30 is arranged on a pipeline between the pump 24 and the flowmeter 25; a liquid discharging pipe 31 is provided on the storage tank 23, and a liquid discharging valve 32 is provided on the liquid discharging pipe 31.
The method for preparing the nickel sulfate by using the acid dissolution reaction equipment for preparing the nickel sulfate comprises the following steps:
step a: closing the blowdown valve, the liquid supply valve 30 and the liquid discharge valve 32, and opening the return valve 29, the suction valve 12, the liquid inlet valve and the pump inlet valve 27;
step b: dilute sulphuric acid is filled in the storage tank 23, the metal nickel is placed on the porous grid plate 17, and replacement gas is filled into the tank body 4 from the charging port 7 to discharge the air in the tank body 4;
step d: opening a liquid supply valve 30, starting a pump 24, closing a return valve 29, adjusting a liquid inlet valve 16 to keep the liquid level in the reactor at the height of a liquid outlet 11 all the time, adjusting an air suction valve 12 to control the amount of bubbles on the liquid level in the reactor, starting a heater 26 to heat, and then opening the return valve 29;
step e: detecting the content of nickel ions in the solution in the storage tank 23, opening the liquid discharge valve 32 to discharge part of the solution after the content of the nickel ions meets the requirement, closing the liquid discharge valve 32 after the solution is discharged, and supplementing dilute sulfuric acid into the storage tank 23;
step f: concentrating and crystallizing the discharged partial solution to generate nickel sulfate crystals.
The above are merely preferred embodiments of the present invention.
Claims (8)
1. An acid-soluble reactor for preparing nickel sulfate comprises a tank body (4) and a tank cover (9) covered on the top of the tank body (4), and is characterized by further comprising a jet aeration device (15) and a porous grid plate (17);
a sewage draining outlet (5) and a liquid inlet (14) are respectively arranged at the lower part of the tank body (4), a sewage draining valve (6) is arranged on the sewage draining outlet (5), an air charging port (7) and a liquid outlet (11) are respectively arranged at the upper part of the tank body (4), and the position of the liquid outlet (11) is lower than that of the air charging port (7);
the jet flow inflating device (15) comprises a three-way pipe (18), a nozzle (20), an air suction pipe (13) and a conveying pipe (19) which are connected to the three-way pipe (18), wherein the nozzle (20) and the conveying pipe (19) are coaxially arranged, and the conveying pipe (19) is connected with the liquid inlet (14);
the porous grid plate (17) is arranged at the bottom in the tank body (4) and fixed with the tank body, a gap is reserved between the porous grid plate (17) and the inner bottom wall of the tank body (4), and a plurality of through holes are formed in the porous grid plate (17) at equal intervals;
the liquid inlet (14) is lower than the porous grid plate (17).
2. An acid-soluble reactor for the production of nickel sulphate according to claim 1 characterised in that the tank lid (9) is provided with a vent pipe (10).
3. The acid-soluble reactor for preparing nickel sulfate as claimed in claim 2, wherein the tank 4 has an interlayer, and the interlayer is filled with the thermal insulation material 2.
4. An acid dissolution reactor for nickel sulphate production as claimed in claim 3, characterised in that the suction pipe (13) is provided with a suction valve (12).
5. An acid dissolution reactor for nickel sulphate production as claimed in claim 4, characterised in that the nozzle (20) is provided with a feed valve (16).
6. An acid dissolution reactor for nickel sulphate production as claimed in claim 5, characterised in that the nozzle (20) has a tapered bore (21), the larger diameter end of the bore (21) being the inlet and the smaller diameter end being the outlet.
7. An acid dissolution reaction device for preparing nickel sulfate, which is characterized by comprising the acid dissolution reactor (22) for preparing nickel sulfate, according to claim 6, and further comprising a storage tank (23), a pump (24), a flow meter (25) and a heater (26) which are connected in sequence through pipelines; the heater (26) is connected with the nozzle (20) through a pipeline; the storage tank (23) is connected with the liquid outlet (11) by a pipeline; a pump inlet valve (27) is arranged on a pipeline between the storage tank (23) and the pump (24); a return pipeline (28) is connected between the storage tank (23) and the pump (24), and a return valve (29) is arranged on the return pipeline (28); a liquid supply valve (30) is arranged on a pipeline between the pump (24) and the flowmeter (25); a liquid discharging pipe (31) is arranged on the storage tank (23), and a liquid discharging valve (32) is arranged on the liquid discharging pipe (31).
8. A method for preparing nickel sulfate by using the acid-soluble reaction equipment for preparing nickel sulfate according to claim 7, which is characterized by comprising the following steps:
step a: closing the drain valve, the liquid supply valve (30) and the liquid discharge valve (32), and opening the return valve (29), the suction valve (12), the liquid inlet valve and the pump inlet valve (27);
step b: dilute sulphuric acid is filled in the storage tank (23), the metallic nickel is placed on the porous grid plate (17), and replacement gas is filled into the tank body (4) from the charging port (7) to discharge the air in the tank body (4);
step d: opening a liquid supply valve (30), starting a pump (24), closing a gate of a return valve (29), adjusting a liquid inlet valve (16) to enable the liquid level in the reactor to be always maintained at the height of a liquid outlet (11), adjusting an air suction valve (12) to control the amount of bubbles on the liquid level in the reactor, starting a heater (26) to heat, and then opening the gate of the return valve (29);
step e: detecting the content of nickel ions in the solution in the storage tank (23), opening the liquid discharging valve (32) to discharge part of the solution after the content of the nickel ions meets the requirement, closing the liquid discharging valve (32) after discharging, and supplementing dilute sulfuric acid into the storage tank (23);
step f: concentrating and crystallizing the discharged partial solution to generate nickel sulfate crystals.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110588297.8A CN113145057A (en) | 2021-05-28 | 2021-05-28 | Acid dissolution reactor, equipment and method for preparing nickel sulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110588297.8A CN113145057A (en) | 2021-05-28 | 2021-05-28 | Acid dissolution reactor, equipment and method for preparing nickel sulfate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113145057A true CN113145057A (en) | 2021-07-23 |
Family
ID=76877957
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110588297.8A Pending CN113145057A (en) | 2021-05-28 | 2021-05-28 | Acid dissolution reactor, equipment and method for preparing nickel sulfate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113145057A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NO20220405A1 (en) * | 2022-04-01 | 2023-10-02 | Glencore Nikkelverk As | Continuous dissolution reactor |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101812585A (en) * | 2009-08-27 | 2010-08-25 | 浙江华友钴业股份有限公司 | Microbubble oxidization and acid dissolution method for copper-cobalt alloy |
| JP2011126757A (en) * | 2009-12-21 | 2011-06-30 | Jgc Catalysts & Chemicals Ltd | Method for producing nickel sulfate aqueous solution |
| CN109850958A (en) * | 2018-12-19 | 2019-06-07 | 浙江科菲科技股份有限公司 | A kind of discarded printed nickel net recovery and treatment method |
| CN110237950A (en) * | 2019-04-11 | 2019-09-17 | 浙江花园新能源有限公司 | A kind of pot for smelted copper gas-liquid mixed nozzle |
| CN111439791A (en) * | 2019-01-17 | 2020-07-24 | 江西核工业兴中新材料有限公司 | Method for producing nickel sulfate by gas-liquid emulsification |
| CN215611604U (en) * | 2021-05-28 | 2022-01-25 | 金川镍钴研究设计院有限责任公司 | Acid dissolution reactor and equipment for preparing nickel sulfate |
-
2021
- 2021-05-28 CN CN202110588297.8A patent/CN113145057A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101812585A (en) * | 2009-08-27 | 2010-08-25 | 浙江华友钴业股份有限公司 | Microbubble oxidization and acid dissolution method for copper-cobalt alloy |
| JP2011126757A (en) * | 2009-12-21 | 2011-06-30 | Jgc Catalysts & Chemicals Ltd | Method for producing nickel sulfate aqueous solution |
| CN109850958A (en) * | 2018-12-19 | 2019-06-07 | 浙江科菲科技股份有限公司 | A kind of discarded printed nickel net recovery and treatment method |
| CN111439791A (en) * | 2019-01-17 | 2020-07-24 | 江西核工业兴中新材料有限公司 | Method for producing nickel sulfate by gas-liquid emulsification |
| CN110237950A (en) * | 2019-04-11 | 2019-09-17 | 浙江花园新能源有限公司 | A kind of pot for smelted copper gas-liquid mixed nozzle |
| CN215611604U (en) * | 2021-05-28 | 2022-01-25 | 金川镍钴研究设计院有限责任公司 | Acid dissolution reactor and equipment for preparing nickel sulfate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NO20220405A1 (en) * | 2022-04-01 | 2023-10-02 | Glencore Nikkelverk As | Continuous dissolution reactor |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN215611604U (en) | Acid dissolution reactor and equipment for preparing nickel sulfate | |
| CN113145057A (en) | Acid dissolution reactor, equipment and method for preparing nickel sulfate | |
| CN109097816A (en) | A kind of molten copper device and its copper dissolving method | |
| CN210826400U (en) | High-efficient copper dissolving tank | |
| CN107973328A (en) | A kind of self-priming nano-calcium carbonate carbonization reactor | |
| CN102250752B (en) | Independent air lifting dual circulation fermentation tank | |
| CN202116539U (en) | Independent airlift double-circulation fermenting tank | |
| CN209173918U (en) | A kind of gas liquid reaction kettle device | |
| CN1242933C (en) | High temperature aerobic digestion device for sludge | |
| CN2601259Y (en) | Water bath heating chemical plating plant | |
| CN203179850U (en) | Wet etching machine | |
| CN214990776U (en) | Ammonia nitrogen wastewater aeration device | |
| CN205676168U (en) | A kind of carburizing reagent system of injection reactor and nano-calcium carbonate | |
| CN210506548U (en) | Microbubble high-oxygen copper dissolving tank | |
| CN213254472U (en) | Flexible body static mixing reaction device special for gas-liquid reaction | |
| CN104406419A (en) | Integration exhaust steam and energy receiving device | |
| CN215028711U (en) | Comprehensive treatment tank equipment for producing high-purity quartz sand | |
| CN113582281A (en) | Energy-saving low-temperature flue gas concentration process and device for desulfurization wastewater | |
| CN208266238U (en) | A kind of biological oxidation gold extraction system circulation whirlwind defoaming device | |
| CN207012766U (en) | A kind of methylamine recovery tower | |
| CN217062029U (en) | Novel nitrogen blowing plate | |
| CN209066045U (en) | A kind of molten copper device | |
| CN214512881U (en) | Continuous defoaming machine of vacuum standing distribution pipe | |
| CN220736983U (en) | Acetylene gas purifying tower | |
| CN108315554A (en) | A kind of biological oxidation gold extraction system circulation whirlwind defoaming device |
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 |