CN117361654A - Method for preparing dinitroso diammine platinum - Google Patents
Method for preparing dinitroso diammine platinum Download PDFInfo
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- CN117361654A CN117361654A CN202311132689.9A CN202311132689A CN117361654A CN 117361654 A CN117361654 A CN 117361654A CN 202311132689 A CN202311132689 A CN 202311132689A CN 117361654 A CN117361654 A CN 117361654A
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- potassium chloroplatinate
- preparing
- water
- washing
- filtering
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 25
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 45
- 239000011591 potassium Substances 0.000 claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000001914 filtration Methods 0.000 claims abstract description 28
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims abstract description 28
- 238000005406 washing Methods 0.000 claims abstract description 27
- 239000013078 crystal Substances 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 239000007787 solid Substances 0.000 claims abstract description 22
- 239000000243 solution Substances 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000000725 suspension Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 18
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 17
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 17
- 235000010288 sodium nitrite Nutrition 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 6
- QFFVPLLCYGOFPU-UHFFFAOYSA-N barium chromate Chemical compound [Ba+2].[O-][Cr]([O-])(=O)=O QFFVPLLCYGOFPU-UHFFFAOYSA-N 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims 1
- 238000009713 electroplating Methods 0.000 abstract description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 10
- 235000019441 ethanol Nutrition 0.000 description 6
- 235000011164 potassium chloride Nutrition 0.000 description 5
- 239000001103 potassium chloride Substances 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000007664 blowing Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/50—Electroplating: Baths therefor from solutions of platinum group metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
Abstract
The invention provides a method for preparing dinitroso diammine platinum, which relates to the technical field of cyanide-free electroplating, and comprises the steps of mixing obtained potassium chloroplatinate with water in a reaction kettle to prepare potassium chloroplatinate suspension, then adding sodium nitrite into the potassium chloroplatinate suspension, heating and heating under the condition of stirring, filtering the solution to obtain a mixed solution, introducing ammonia water into the cooled mixed solution under the condition of stirring, standing, filtering out solids in the mixed solution, washing and drying the solids, then placing the solids into water for heating and stirring for dissolving, filtering out crystals separated out after the solution is cooled by a sand core, and filtering and drying the crystals.
Description
Technical Field
The invention relates to the technical field of cyanide-free electroplating, in particular to a method for preparing dinitroso diammine platinum.
Background
The dinitroso diammine platinum, commonly called as P salt, is white powder, is commonly used in cyanide-free electroplating platinating, has the advantages of high plating hardness, small resistance and the like, and the preparation method of the dinitroso diammine platinum comprises the following steps: dissolving metal platinum with aqua regia to obtain chloroplatinic acid, and reacting with potassium chloride solution under heating and stirring to obtain potassium chloroplatinate precipitate. The potassium chloroplatinate is mixed into paste by water, heated on a sand bath, and the solution of sodium nitrite is added into the paste potassium chloroplatinate, and the temperature is controlled at 105 ℃ until the reaction is completed, thus obtaining a yellowish green solution. Cooling, adding ammonia water, bottling, plugging the bottle mouth, shaking, standing overnight, suction filtering, washing for several times, recrystallizing with boiling water, and suction drying to obtain the final product.
The dinitroso diammine platinum prepared by the existing method contains more potassium ions and cannot be removed by a recrystallization method, so that the product quality is affected. Under the condition of high requirements of electroplating coating, the stress on the coating is greatly influenced, and the electroplating effect is obviously influenced.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a method for preparing dinitroso diammine platinum, which solves the problems of larger reagent dosage, more severe reaction conditions, more product impurities and the like in the preparation of dinitroso diammine platinum in the prior art.
Technical proposal
In order to achieve the above purpose, the invention is realized by the following technical scheme: a method for preparing dinitroso diammine platinum comprises the following specific preparation method:
sp1: taking chloroplatinic acid to prepare potassium chloroplatinate, and mixing the obtained potassium chloroplatinate with water in a reaction kettle to prepare potassium chloroplatinate suspension;
sp2: adding sodium nitrite into the potassium chloroplatinate suspension, heating under stirring,
then filtering the solution to obtain a mixed solution;
sp3: ammonia water is introduced into the cooled mixed solution under the stirring condition, and then the mixed solution is kept stand for 2 hours;
sp4: filtering out the solid in the mixed solution, and then washing and drying the solid;
sp5: and (3) putting the solid into water, heating and stirring to dissolve, and then filtering out crystals separated out after the solution is cooled by using a sand core, filtering the crystals and drying the crystals.
Preferably, the heating temperature of the sodium nitrite is at least 80 degrees, and the amount of the nitrous acid is 5 times of the mass of the potassium chloroplatinate.
Preferably, the concentration of the ammonia water is 20%, the content of platinum in the chloroplatinic acid is 37.5%, and the ratio of the volume of ammonia water to the mass of platinum is at most 12:1, the minimum ratio of the volume of ammonia water to the mass of platinum is 12:1.
preferably, the solid and the crystal are washed by cold water and ethanol, the times of the cold water washing are 3 times, the times of the ethanol washing are 2 times, the drying temperature of the solid and the crystal is 80 degrees, and the mass ratio of the chloroplatinic acid to the water in the process of preparing the potassium chloroplatinate by the chloroplatinic acid is 1:8.
Preferably, the potassium chloroplatinate suspension reacts with sodium nitrite, a large amount of small bubbles are continuously generated, brown nitrogen oxide gas is released, and finally yellow potassium chloroplatinate particles disappear, the color of the reaction solution becomes light yellow, and the reaction is stopped.
Preferably, the potassium chloroplatinate suspension contains lemon-yellow precipitated crystals, the supernatant of the potassium chloroplatinate suspension is yellowish, and the washing is separated and washed by a centrifuge or filtered and washed by a sand core.
Advantageous effects
The invention provides a method for preparing dinitroso diammine platinum. The beneficial effects are as follows:
mixing the obtained potassium chloroplatinate with water in a reaction kettle to obtain potassium chloroplatinate suspension, adding sodium nitrite into the potassium chloroplatinate suspension, heating and heating under the condition of stirring, filtering the solution to obtain a mixed solution, introducing ammonia water into the cooled mixed solution under the condition of stirring, standing, filtering out solids in the mixed solution, washing and drying the solids, putting the solids into water, heating and stirring to dissolve the solids, and filtering out crystals separated out after the solution is cooled by a sand core, and filtering and drying the crystals.
Drawings
FIG. 1 is a diagram of a preparation method of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
First embodiment:
as shown in fig. 1, a method for preparing dinitroso diammine platinum is specifically as follows:
sp1: taking chloroplatinic acid to prepare potassium chloroplatinate, and mixing the obtained potassium chloroplatinate with water in a reaction kettle to prepare potassium chloroplatinate suspension;
sp2: adding sodium nitrite into the potassium chloroplatinate suspension, heating under stirring,
then filtering the solution to obtain a mixed solution;
sp3: ammonia water is introduced into the cooled mixed solution under the stirring condition, and then the mixed solution is kept stand for 2 hours;
sp4: filtering out the solid in the mixed solution, and then washing and drying the solid;
sp5: and (3) putting the solid into water, heating and stirring to dissolve, and then filtering out crystals separated out after the solution is cooled by using a sand core, filtering the crystals and drying the crystals.
The heating temperature of the sodium nitrite is 80 degrees at the minimum, and the amount of the nitrous acid is 5 times of the mass of the potassium chloroplatinate. The concentration of ammonia water is 20%, the content of platinum in chloroplatinic acid is 37.5%, and the maximum ratio of the volume of ammonia water to the mass of platinum is 12:1, the minimum ratio of ammonia water volume to platinum mass is 12:1. the solid and the crystal are washed by cold water and ethanol, the times of the cold water washing are 3 times, the times of the ethanol washing are 2 times, the drying temperature of the solid and the crystal is 80 degrees, and the mass ratio of the chloroplatinic acid to the water is 1:8 in the process of preparing the potassium chloroplatinate from the chloroplatinic acid. The potassium chloroplatinate suspension reacts with sodium nitrite, a large amount of small bubbles are continuously generated, brown nitrogen oxide gas is released, finally yellow potassium chloroplatinate particles disappear, the color of the reaction solution becomes light yellow, and the reaction is stopped. The suspension of potassium chloroplatinate contains lemon-yellow precipitated crystals, supernatant of the suspension of potassium chloroplatinate is light yellow, washing is carried out by adopting a centrifugal machine to separate and wash or sand core filtration and wash, 100 g of chloroplatinic acid is taken and dissolved in 800 ml of water, 1 ml of hydrogen peroxide is added, heating is carried out to 80 ℃, then 100 g of potassium chloride is slowly added, stirring is carried out for 20 minutes, at this time, the obtained lemon-yellow precipitated crystals are obtained, supernatant is light yellow, precipitate is filtered out by a sand core funnel, and is washed three times by 10% potassium chloride solution, and is washed twice by using absolute ethyl alcohol, air blast is carried out at 80 ℃, drying is carried out at the constant weight, and 92 g of potassium chloroplatinate is obtained; suspending 92 g of dried potassium chloroplatinate in 500 ml of water, starting stirring, adding 128 g of sodium nitrite, slowly heating to 90 ℃, continuously generating a large amount of small bubbles at the moment, releasing brown nitrogen oxide gas, reacting for 4 hours, wherein the small bubbles are not generated, yellow potassium chloroplatinate particles disappear, the color of the reaction solution becomes light yellow, and stopping the reaction; the solution was then filtered, the filtrate was collected and cooled to room temperature. Introducing the cooled filtrate into a reactor, starting stirring, adding 40 ml of ammonia water, generating a large amount of fluffy light yellow floccules after about 1 minute, stopping stirring for 30 minutes, standing for 2 hours, separating and washing by a centrifugal machine or filtering and washing by a sand core after the standing time is over, adding the washed dinitroso diammine platinum crude product into calculated water, stirring and heating to boil, cooling to room temperature after all P salts are dissolved, filtering and separating out crystals by the sand core, washing for 3 times by cold water, washing for two times by ethanol, and drying by blowing at 80 ℃ to constant weight, thus obtaining the pure dinitroso diammine platinum, wherein the yield of the dinitroso diammine platinum is 77% and the platinum content is 61.02% by measurement.
Specific embodiment II:
500 g of chloroplatinic acid is taken and dissolved in 4000 ml of water, 5 ml of hydrogen peroxide is added, the temperature is raised to 80 ℃, then 500 g of potassium chloride is slowly added, and stirring is carried out for 20 minutes, at this time, lemon-yellow precipitated crystals are obtained, and the supernatant is pale yellow. Filtering out precipitate by using a sand core funnel, washing with 10% potassium chloride solution for three times, washing with absolute ethyl alcohol for two times, drying at 80 ℃ by blowing air, and taking out the precipitate after constant weight to obtain 460 g of potassium chloroplatinate; the dried 460 g potassium chloroplatinate was suspended in 2500 ml water and stirring was started. 640 g of sodium nitrite are added and the temperature is slowly raised to 90 ℃. In this case, a large amount of small bubbles are continuously generated and brown nitrogen oxide gas is released, after the reaction is carried out for 4 hours, the small bubbles are not generated, yellow potassium chloroplatinate particles disappear, the color of the reaction solution becomes light yellow, and the reaction is stopped; the solution was filtered and the filtrate was collected and cooled to room temperature. Introducing the cooled filtrate into a reactor, starting stirring, adding 500 ml of ammonia water, generating a large amount of fluffy light yellow floccules after about 1 minute, stopping stirring for 30 minutes, standing for 2 hours, separating and washing by a centrifuge or filtering and washing by a sand core after the standing time is over, adding the washed crude dinitroso diammine platinum product into calculated water, stirring and heating to boil, cooling to room temperature after all dinitroso diammine platinum is completely dissolved, filtering and separating crystals by the sand core, washing for 3 times by cold water, washing for two times by ethanol, and drying by blowing at 80 ℃ to constant weight, thus obtaining 280.3 g of pure dinitroso diammine platinum, and measuring to obtain 280.3 g of dinitroso, the yield is 85%, and the content of the measured platinum is 60.81%.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising a reference structure" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises an element.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A method for preparing dinitroso diammine platinum, characterized by: the preparation method comprises the following steps:
sp1: taking chloroplatinic acid to prepare potassium chloroplatinate, and mixing the obtained potassium chloroplatinate with water in a reaction kettle to prepare potassium chloroplatinate suspension;
sp2: adding sodium nitrite into the potassium chloroplatinate suspension, heating under the condition of stirring, and then filtering the solution to obtain a mixed solution;
sp3: ammonia water is introduced into the cooled mixed solution under the stirring condition, and then the mixed solution is kept stand for 2 hours;
sp4: filtering out the solid in the mixed solution, and then washing and drying the solid;
sp5: and (3) putting the solid into water, heating and stirring to dissolve, and then filtering out crystals separated out after the solution is cooled by using a sand core, filtering the crystals and drying the crystals.
2. A method for preparing dinitroso diammine platinum according to claim 1, characterized in that: the heating temperature of the sodium nitrite is 80 degrees at the minimum, and the nitrous acid amount is 5 times of the mass of the potassium chloroplatinate.
3. A method for preparing dinitroso diammine platinum according to claim 1, characterized in that: the concentration of the ammonia water is 20%, the content of platinum in the chloroplatinic acid is 37.5%, and the maximum ratio of the volume of the ammonia water to the mass of the platinum is 12:1, the minimum ratio of the volume of ammonia water to the mass of platinum is 12:1.
4. a method for preparing dinitroso diammine platinum according to claim 1, characterized in that: the solid and the crystal are washed by cold water and ethanol, the times of the cold water washing are 3 times, the times of the ethanol washing are 2 times, the drying temperature of the solid and the crystal is 80 degrees, and the mass ratio of chloroplatinic acid to water is 1:8 in the process of preparing potassium chloroplatinate from chloroplatinic acid.
5. A method for preparing dinitroso diammine platinum according to claim 1, characterized in that: the potassium chloroplatinate suspension reacts with sodium nitrite, a large amount of small bubbles are continuously generated, brown nitrogen oxide gas is released, finally yellow potassium chloroplatinate particles disappear, the color of the reaction solution becomes light yellow, and the reaction is stopped.
6. A method for preparing dinitroso diammine platinum according to claim 1, characterized in that: the potassium chloroplatinate suspension contains lemon-yellow precipitated crystals, the supernatant of the potassium chloroplatinate suspension is light yellow, and the washing adopts centrifugal separation washing or sand core filtering washing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311132689.9A CN117361654A (en) | 2023-09-04 | 2023-09-04 | Method for preparing dinitroso diammine platinum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311132689.9A CN117361654A (en) | 2023-09-04 | 2023-09-04 | Method for preparing dinitroso diammine platinum |
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| Publication Number | Publication Date |
|---|---|
| CN117361654A true CN117361654A (en) | 2024-01-09 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202311132689.9A Pending CN117361654A (en) | 2023-09-04 | 2023-09-04 | Method for preparing dinitroso diammine platinum |
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| Country | Link |
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| CN (1) | CN117361654A (en) |
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- 2023-09-04 CN CN202311132689.9A patent/CN117361654A/en active Pending
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