CN112143886A - W-shaped fixed bed leaching device and method - Google Patents
W-shaped fixed bed leaching device and method Download PDFInfo
- Publication number
- CN112143886A CN112143886A CN202010948375.6A CN202010948375A CN112143886A CN 112143886 A CN112143886 A CN 112143886A CN 202010948375 A CN202010948375 A CN 202010948375A CN 112143886 A CN112143886 A CN 112143886A
- Authority
- CN
- China
- Prior art keywords
- tower
- liquid
- fixed bed
- uranium
- way valve
- 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
- 238000002386 leaching Methods 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 78
- 229910052770 Uranium Inorganic materials 0.000 claims abstract description 49
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000011347 resin Substances 0.000 claims abstract description 48
- 229920005989 resin Polymers 0.000 claims abstract description 48
- 239000003480 eluent Substances 0.000 claims abstract description 18
- 238000003860 storage Methods 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 239000013589 supplement Substances 0.000 claims description 10
- 238000005070 sampling Methods 0.000 claims description 9
- 230000001502 supplementing effect Effects 0.000 claims description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052801 chlorine Inorganic materials 0.000 claims description 3
- 239000000460 chlorine Substances 0.000 claims description 3
- YPJKMVATUPSWOH-UHFFFAOYSA-N nitrooxidanyl Chemical group [O][N+]([O-])=O YPJKMVATUPSWOH-UHFFFAOYSA-N 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 4
- 238000000605 extraction Methods 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/02—Apparatus therefor
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacturing & Machinery (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a W-shaped fixed bed leaching device and a method, which comprise a W-shaped tower, an automatic control three-way valve, a liquid distributor, a uranium-rich resin inlet and a liquid inlet. The top of the left side of the tower is provided with a liquid distributor, and the eluent is uniformly distributed in the tower through the liquid distributor. The upper part of the liquid distributor is provided with a liquid inlet. The left side surface of the tower is provided with a uranium-rich resin inlet at the lower part of the liquid distributor. The W-shaped fixed bed leaching device is connected with a plurality of towers in series through an automatic control three-way valve. One outlet of the automatic control three-way valve is connected with another series-connected tower, and the other outlet is connected with a qualified liquid storage tank. The method simplifies the operation flow and control parameters, the resin capacity is high, and the uranium concentration of the uranium enriched liquid obtained by leaching can directly meet the product precipitation standard.
Description
Technical Field
The invention belongs to the technical field of uranium ore in-situ leaching, and particularly relates to a W-shaped fixed bed leaching device and a method.
Background
Ion exchange is an important component of the post-treatment process of the ground leaching solution, and leaching is one of the important processes. The leaching operation is carried out on uranium-rich resin, and the leaching operation can be divided into fixed bed leaching and moving bed leaching according to whether a resin bed layer moves relative to a tower in the ion exchange process.
The uranium-rich resin produced by adsorbing the leachate obtained by the acid method through the adsorption tower has low capacity due to ion competitive adsorption and the like. The enriched liquid leached by the single-tower vertical fixed bed has low uranium concentration, cannot directly precipitate products, needs to be further enriched by methods such as extraction and the like, has long flow and has safety and environmental protection risks. The moving bed leaching is adopted, saturated resin generated by an adsorption tower is required to adsorb the uranium enriched liquid again so as to further improve the resin capacity, the preorder process is complex, and the control parameters are multiple.
Accordingly, there is a need for an improved washing apparatus and method.
Disclosure of Invention
The invention mainly aims to provide a leaching device and a leaching method for a W-shaped fixed bed, which simplify the operation process and control parameters, and enable the uranium concentration of the leached uranium enriched liquid to directly meet the product precipitation standard.
The technical scheme adopted by the invention is as follows:
a W-shaped fixed bed leaching device comprises a tower, a liquid distributor, a uranium-rich resin inlet and a liquid inlet. The top of the left side of the tower is provided with a liquid distributor, and the eluent is uniformly distributed in the tower through the liquid distributor. The upper part of the liquid distributor is provided with a liquid inlet. The left side surface of the tower is provided with a uranium-rich resin inlet at the lower part of the liquid distributor.
The tower is of a W-shaped structure.
An emptying valve is arranged at one side of the liquid inlet at the top of the tower, and a pressure gauge is arranged at the other side of the tower.
The tower is provided with a discharge port at the bottom of each of the left and right sides. The tower is provided with a second resin supplement port at the top of the middle part and a first resin supplement port at the top of the right side of the tower.
The lower part of the resin supplementing port on the right side of the tower is provided with an eluting agent outlet, the lower part of the eluting agent outlet is provided with a liquid collecting tank, and the left side and the right side of the bottom of the liquid collecting tank are respectively provided with a groove.
The W-shaped fixed bed leaching device is also provided with an automatic control three-way valve and a uranium concentration analysis sampling port. The bottoms of the two grooves are connected with each other and then connected with the inlet of the automatic control three-way valve.
The W-shaped fixed bed leaching device is connected with a plurality of towers in series through an automatic control three-way valve. The first outlet of the automatic control three-way valve is connected with another tower connected in series, and the second outlet of the automatic control three-way valve is connected with a qualified liquid storage tank.
The automatic control three-way valve controls the liquid outlet direction of the groove to be a qualified liquid storage tank or another tower connected in series.
The uranium concentration analysis sampling port is arranged at the inlet of the automatic control three-way valve.
The invention also provides a leaching method of the W-shaped fixed bed, which comprises the following steps:
s1: and filling the tower with the uranium-rich resin through a uranium-rich resin inlet, a resin supplementing port I and a resin supplementing port II to ensure that the uranium-rich resin capacity is higher than 14mgU/mLWR, and the total length of a uranium-rich resin bed layer in the W-type fixed bed leaching device is 15-25 m.
S2: introducing an eluting agent through a liquid inlet, and controlling the contact time of the eluting agent to be 16-20 h; and simultaneously opening an eluent outlet to discharge the eluent. The eluting agent is nitrate radical type or chlorine type eluting agent.
S3: the eluting agent is gathered through the collecting tank and gets into the recess to from the recess bottom outflow and converge, sample and carry out concentration analysis through uranium concentration analysis sample connection, it is C1 to record uranium concentration.
S4: setting the concentration of qualified leaching solution as C2,
if C1 is more than or equal to C2, the liquid outlet direction of the three-way valve is automatically controlled to be a qualified liquid storage tank;
if C1 is less than C2, the liquid outlet direction of the three-way valve is automatically controlled to be the other tower connected in series.
S5: and after qualified liquid is discharged, stopping feeding the eluent from the liquid inlet when the C1 is less than 100mgU/mL, and finishing leaching.
The invention has the following technical effects:
1) the operation flow and control parameters are simplified, and the uranium concentration of the uranium enriched liquid obtained by leaching can directly meet the product precipitation standard;
2) realizing the leaching of the low-volume saturated resin by adopting a fixed bed; the qualified uranium liquid does not need to be further enriched by an extraction process, so that an organic phase is prevented from being introduced;
3) the resin capacity is high.
Drawings
FIG. 1 is a schematic view of a W-type fixed bed leaching apparatus.
In the figure: 1 is a liquid distributor; 2 is an emptying valve; 3 is a liquid inlet; 4 is a pressure gauge; 5 is a uranium-rich resin inlet; 6 is a tower; 7 is a discharge port; 8 is a uranium concentration analysis sampling port; 9 is an automatic control three-way valve; 10 is an eluent outlet; 11 is a resin supplement port I; 12 is a liquid collecting tank; 13 is a groove; 14 is a resin supplement port II; 15 is an outlet I; and 16 is an outlet II.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
As shown in figure 1, the invention provides a W-shaped fixed bed leaching device, which comprises a tower 6, a liquid distributor 1, a uranium-rich resin inlet 5 and a liquid inlet 3. The top of the left side of the tower 6 is provided with a liquid distributor 1, and the eluting agent is uniformly distributed in the tower 6 through the liquid distributor 1. The upper part of the liquid distributor 1 is provided with a liquid inlet 3. The left side surface of the tower 6 is provided with a uranium-rich resin inlet 5 at the lower part of the liquid distributor 1.
The tower 6 is of a W-shaped structure.
An emptying valve 2 is arranged at one side of the liquid inlet 3 at the top of the tower 6, and a pressure gauge 4 is arranged at the other side.
The tower 6 is provided at the bottom of the left and right sides with a discharge port 7, respectively. The tower 6 is provided with a second resin supplement port 14 at the top of the middle part, and a first resin supplement port 11 at the top of the right side of the tower 6.
An eluent outlet 10 is arranged at the lower part of the first resin supplementing port 11 on the right side of the tower 6, a liquid collecting tank 12 is arranged at the lower part of the eluent outlet 10, and a groove 13 is respectively arranged at the left side and the right side of the bottom of the liquid collecting tank 12.
The W-shaped fixed bed leaching device is also provided with an automatic control three-way valve 9 and a uranium concentration analysis sampling port 8.
The uranium concentration analysis sampling port 8 is arranged at the inlet of the automatic control three-way valve 9.
The bottoms of the two grooves 13 are connected with each other and then connected with the inlet of the automatic control three-way valve 9.
The W-shaped fixed bed leaching device is connected in series with a plurality of towers 6 through an automatic control three-way valve 9. The first outlet 15 of the automatic control three-way valve 9 is connected with another tower 6 which is connected in series, and the second outlet 16 of the automatic control three-way valve 9 is connected with a qualified liquid storage tank.
The automatic control three-way valve 9 controls the liquid outlet direction of the groove 13 to be a qualified liquid storage tank or another tower 6 connected in series.
The invention also provides a leaching method of the W-shaped fixed bed, which comprises the following steps:
the method comprises the following steps: the tower 6 is filled with the uranium-rich resin through a uranium-rich resin inlet 5, a resin supplementing port I11 and a resin supplementing port II 14, so that the volume of the uranium-rich resin is higher than 14mgU/mLWR, and the total length of a uranium-rich resin bed layer in the W-type fixed bed leaching device is 15-25 m.
Step two: feeding eluting agent through the liquid inlet 3, and controlling the contact time of the eluting agent to be 16-20 h; simultaneously, the eluent outlet 10 is opened to discharge the eluent. The eluting agent is nitrate radical type or chlorine type eluting agent.
Step three: the eluting agent is converged into the groove 13 through the liquid collecting tank 12, flows out from the bottom of the groove 13 and is converged, and is sampled through the uranium concentration analysis sampling port 8 and subjected to concentration analysis, so that the uranium concentration is C1.
Step four: setting the concentration of qualified leaching solution as C2,
if C1 is more than or equal to C2, the liquid outlet direction of the three-way valve 9 is automatically controlled to be a qualified liquid storage tank;
if C1 is less than C2, the liquid outlet direction of the three-way valve 9 is automatically controlled to be another tower connected in series.
Step five: and after qualified liquid is discharged, stopping feeding the eluent into the liquid inlet 3 when the C1 is less than 100mgU/mL, and finishing leaching.
The invention has the following technical effects:
1) the operation flow and control parameters are simplified, and the uranium concentration of the uranium enriched liquid obtained by leaching can directly meet the product precipitation standard;
2) realizing the leaching of the low-volume saturated resin by adopting a fixed bed; the qualified uranium liquid does not need to be further enriched by an extraction process, so that an organic phase is prevented from being introduced;
3) the resin capacity is high.
Claims (10)
1. The utility model provides a W type fixed bed drip washing device which characterized in that: comprises a tower (6), a liquid distributor (1), a uranium-rich resin inlet (5) and a liquid inlet (3); a liquid distributor (1) is arranged at the top of the left side of the tower (6), and the eluting agent is uniformly distributed in the tower (6) through the liquid distributor (1); a liquid inlet (3) is arranged at the upper part of the liquid distributor (1); the left side surface of the tower (6) is provided with a uranium-rich resin inlet (5) at the lower part of the liquid distributor (1).
2. The W-type fixed bed leaching apparatus according to claim 1, wherein: the tower (6) is of a W-shaped structure.
3. The W-type fixed bed leaching apparatus according to claim 2, wherein: an exhaust valve (2) is arranged at one side of the liquid inlet (3) at the top of the tower (6), and a pressure gauge (4) is arranged at the other side of the tower.
4. The W-type fixed bed leaching apparatus according to claim 3, wherein: the bottom of the left side and the bottom of the right side of the tower (6) are respectively provided with a discharge port (7), the top of the middle of the tower (6) is provided with a second resin supplement port (14), and the top of the right side of the tower (6) is provided with a first resin supplement port (11).
5. The W-type fixed bed leaching apparatus according to claim 4, wherein: an eluent outlet (10) is formed in the right side of the tower (6) and below the first resin supplementing port (11), a liquid collecting tank (12) is arranged below the eluent outlet (10), and grooves (13) are formed in the left side and the right side of the bottom of the liquid collecting tank (12) respectively.
6. The W-type fixed bed leaching apparatus according to claim 5, wherein: the W-shaped fixed bed leaching device is also provided with an automatic control three-way valve (9), and the automatic control three-way valve (9) is provided with an inlet, an outlet I (15) and an outlet II (16); the bottoms of the two grooves (13) are connected with each other and then connected with the inlet of the automatic control three-way valve (9).
7. The W-shaped fixed bed leaching apparatus according to claim 6, wherein: the W-type fixed bed leaching device is also provided with a uranium concentration analysis sampling port (8), and the uranium concentration analysis sampling port (8) is arranged at an inlet of an automatic control three-way valve (9).
8. The W-type fixed bed leaching apparatus according to claim 7, wherein: the W-shaped fixed bed leaching device is connected with a plurality of towers (6) in series through an automatic control three-way valve (9); the first outlet (15) of the automatic control three-way valve (9) is connected with the other tower (6) which is connected in series, and the second outlet (16) of the automatic control three-way valve (9) is connected with the qualified liquid storage tank.
9. The W-type fixed bed leaching apparatus according to claim 8, wherein: the bottoms of the two grooves (13) are connected with each other and then connected with an inlet of an automatic control three-way valve (9); the automatic control three-way valve (9) controls the liquid outlet direction of the groove (13) to be a qualified liquid storage tank or another tower (6) connected in series.
10. A W-type fixed bed leaching method using the W-type fixed bed leaching apparatus according to claim 9, wherein: the method comprises the following steps:
the method comprises the following steps: the tower (6) is filled with the uranium-rich resin through a uranium-rich resin inlet (5), a resin supplement port I (11) and a resin supplement port II (14), so that the volume of the uranium-rich resin is higher than 14mgU/mLWR, and the total length of a uranium-rich resin bed layer in the W-type fixed bed leaching device is 15-25 m;
step two: feeding the eluting agent through the liquid inlet (3), and controlling the contact time of the eluting agent to be 16-20 h; simultaneously opening an eluent outlet (10) to discharge eluent; the eluent is nitrate radical type or chlorine type eluent;
step three: the eluting agent is converged into the groove (13) through the liquid collecting tank (12), flows out from the bottom of the groove (13) and is converged, and is sampled through the uranium concentration analysis sampling port (8) and subjected to concentration analysis, so that the uranium concentration is measured to be C1;
step four: setting the concentration of qualified leaching solution as C2,
if C1 is more than or equal to C2, the liquid outlet direction of the three-way valve (9) is automatically controlled to be a qualified liquid storage tank;
if C1 is less than C2, the liquid outlet direction of the three-way valve (9) is automatically controlled to be the other tower connected in series;
step five: and after qualified liquid is discharged, stopping feeding the eluent from the liquid inlet (3) when the C1 is less than 100mgU/mL, and finishing leaching.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010948375.6A CN112143886A (en) | 2020-09-10 | 2020-09-10 | W-shaped fixed bed leaching device and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010948375.6A CN112143886A (en) | 2020-09-10 | 2020-09-10 | W-shaped fixed bed leaching device and method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112143886A true CN112143886A (en) | 2020-12-29 |
Family
ID=73889506
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010948375.6A Pending CN112143886A (en) | 2020-09-10 | 2020-09-10 | W-shaped fixed bed leaching device and method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112143886A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1014948A1 (en) * | 1981-11-06 | 1983-04-30 | Среднеазиатский Научно-Исследовательский И Проектный Институт Цветной Металлургии | Apparatus for continuous leaching |
| CN2530705Y (en) * | 2002-01-17 | 2003-01-15 | 黑龙江省计算中心 | Folding continuous counter-current diffuser |
| CN104531996A (en) * | 2014-12-22 | 2015-04-22 | 核工业北京化工冶金研究院 | Tower-changeable ion exchange process for treating neutral leaching liquid |
| CN111519048A (en) * | 2020-04-24 | 2020-08-11 | 核工业北京化工冶金研究院 | U-shaped structure uranium leaching device and method |
| CN111549222A (en) * | 2020-04-24 | 2020-08-18 | 核工业北京化工冶金研究院 | Intelligent control system and method for U-shaped ion exchange tower |
| CN213739613U (en) * | 2020-09-10 | 2021-07-20 | 核工业北京化工冶金研究院 | W-shaped fixed bed leaching device |
-
2020
- 2020-09-10 CN CN202010948375.6A patent/CN112143886A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1014948A1 (en) * | 1981-11-06 | 1983-04-30 | Среднеазиатский Научно-Исследовательский И Проектный Институт Цветной Металлургии | Apparatus for continuous leaching |
| CN2530705Y (en) * | 2002-01-17 | 2003-01-15 | 黑龙江省计算中心 | Folding continuous counter-current diffuser |
| CN104531996A (en) * | 2014-12-22 | 2015-04-22 | 核工业北京化工冶金研究院 | Tower-changeable ion exchange process for treating neutral leaching liquid |
| CN111519048A (en) * | 2020-04-24 | 2020-08-11 | 核工业北京化工冶金研究院 | U-shaped structure uranium leaching device and method |
| CN111549222A (en) * | 2020-04-24 | 2020-08-18 | 核工业北京化工冶金研究院 | Intelligent control system and method for U-shaped ion exchange tower |
| CN213739613U (en) * | 2020-09-10 | 2021-07-20 | 核工业北京化工冶金研究院 | W-shaped fixed bed leaching device |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN213739613U (en) | W-shaped fixed bed leaching device | |
| CN106669867A (en) | Continuous and automatic ion exchange device | |
| WO2021143434A1 (en) | New lithium-sodium separation method | |
| CN102649544B (en) | Multifunctional nitrogen making machine | |
| EP0004792B1 (en) | Moving bed ion exchange method | |
| CN106422414A (en) | Automatic-column-mounting continuous-operating in-series macroporous resin adsorption and separation device | |
| CN112143886A (en) | W-shaped fixed bed leaching device and method | |
| CN207041972U (en) | A kind of Chinese medicine produces chromatographic column automaton | |
| CN111519048B (en) | U-shaped uranium leaching device and method | |
| CN207221944U (en) | Continuous automatic ion exchanging device | |
| CN201095645Y (en) | Adsorption tower for dense moving bed | |
| US3969243A (en) | Moving bed ion-exchange apparatus and operating method thereof | |
| CN212128272U (en) | Ion exchange system for recovering rhenium from rhenium-containing spraying liquid | |
| US4018677A (en) | Method of stripping solid particles | |
| CN102863054B (en) | Device for classification recycling of ion exchange resins and process thereof | |
| CN111549222A (en) | Intelligent control system and method for U-shaped ion exchange tower | |
| CN210434033U (en) | Integrated device for separating multiple components of traditional Chinese medicine based on macroporous resin adsorption | |
| CN104003476B (en) | Electrolytic manganese wastewater ion exchange treatment system adopting aeration type ion exchange devices | |
| CN109052435B (en) | Adsorption tower group for extracting lithium from salt lake brine | |
| CN208302795U (en) | A kind of flat bed as ion-exchange unit | |
| CN109234529B (en) | In-situ leaching uranium extraction leachate treatment process | |
| CN2172156Y (en) | Self-top-pressure reversing flow regenerating ion exchanger | |
| CN203200327U (en) | Activated-carbon adsorption device | |
| CN220246213U (en) | Automatic control process system for preparing uranium-containing qualified liquid | |
| CN201825993U (en) | Continuous ion exchange device for extracting gallium in Bayer mother liquid |
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 |