CN110964919A - Preparation method of spongy platinum - Google Patents
Preparation method of spongy platinum Download PDFInfo
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- CN110964919A CN110964919A CN201811139398.1A CN201811139398A CN110964919A CN 110964919 A CN110964919 A CN 110964919A CN 201811139398 A CN201811139398 A CN 201811139398A CN 110964919 A CN110964919 A CN 110964919A
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- 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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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Abstract
The invention discloses a preparation method of spongy platinum, which is implemented according to the following steps: step 1, slurrying crude ammonium chloroplatinate, heating, adding hydrochloric acid and sodium chlorate, and stirring to obtain a mixed solution; step 2, boiling the mixed solution and keeping the mixed solution for a fixed time, adding ammonium chloride, and filtering the mixed solution after the mixed solution is cooled to obtain high-purity ammonium chloroplatinate; step 3, slurrying high-purity chloroplatinic acid ammonium, adjusting the pH value to 8-9, heating, and adding hydrazine hydrate for reduction to obtain platinum elements; step 4, dissolving the platinum element in the step 3 by using hydrogen peroxide hydrochloride to obtain a dissolved solution containing the platinum element; step 5, precipitating the dissolved solution in the step 4 by adopting an ammonium chloride fractional precipitation method to obtain ammonium chloroplatinate, and then calcining the ammonium chloroplatinate obtained by the precipitation in the first step to obtain spongy platinum; the invention adopts an aqueous solution chlorination method to remove impurity elements in crude ammonium chloroplatinate, adopts hydrazine hydrate reduction-hydrochloric acid hydrogen peroxide dissolution-ammonium chloride fractional precipitation method to refine ammonium chloroplatinate to obtain spongy platinum, and has short period of the whole process.
Description
Technical Field
The invention belongs to the technical field of non-ferrous metal smelting, and particularly relates to a preparation method of spongy platinum.
Background
In the traditional platinum refining process, impure crude ammonium chloroplatinate is dissolved by using a solvent (commonly called aqua regia) prepared by one volume of nitric acid and three volumes of hydrochloric acid under the condition of heating and boiling.
In order to completely dissolve ammonium chloroplatinate, more than 5-6 times of aqua regia must be added, and the aqua regia must be prepared at present, its whole dissolving time must be above 6 hr, and in order to remove nitrate radical from dissolved platinum solution, the solution must be completely evaporated to near-dry, and after the solution is viscous like syrup, the operation of adding dilute hydrochloric acid can be repeated for more than three times, and finally the nitrate-free solution can be added into dilute hydrochloric acid, heated and boiled to obtain platinum dissolved solution, and after cooling and filtering, the ammonium chloride can be added to precipitate pure ammonium chloroplatinate.
Because the traditional platinum refining process adopts aqua regia as a solvent, the dissolving process is long in time, each process needs to be heated, the energy consumption is high, and the reagent dosage is large.
Disclosure of Invention
The invention aims to provide a preparation method of spongy platinum, which can reduce the dissolving time and reduce the energy consumption. .
The technical scheme adopted by the invention is that the preparation method of the spongy platinum is implemented according to the following steps:
step 1, slurrying crude ammonium chloroplatinate, heating, adding hydrochloric acid and sodium chlorate, and uniformly stirring to obtain a mixed solution;
step 2, boiling the mixed solution obtained in the step 1 and keeping the mixed solution for a fixed time, then adding ammonium chloride, and filtering the mixed solution after the mixed solution is cooled to obtain high-purity ammonium chloroplatinate;
step 3, slurrying high-purity chloroplatinic acid ammonium, adjusting the pH value to 8-9, heating, and then adding hydrazine hydrate for reduction to obtain platinum elements;
step 4, dissolving the platinum element in the step 3 by using hydrogen peroxide hydrochloride to obtain a dissolved solution containing the platinum element;
and 5, precipitating the dissolved solution in the step 4 by adopting an ammonium chloride fractional precipitation method to obtain ammonium chloroplatinate, calcining the ammonium chloroplatinate obtained by the precipitation in the first step to obtain spongy platinum, and returning the ammonium chloroplatinate obtained by the precipitation in the second step to the step 1.
The present invention is also characterized in that,
the specific method for slurrying crude ammonium chloroplatinate in the step 1 comprises the following steps: mixing pure water according to the proportion of 5-10: 1 volume ratio was added to crude ammonium chloroplatinate for slurrying.
The heating temperature in the step 1 is 80-90 ℃, the adding amount of hydrochloric acid is 10-20% of the volume of the slurried solution, the adding amount of sodium chlorate is 5-10% of the mass of the crude ammonium chloroplatinate, and the stirring time is 1-2 h.
The fixed time in the step 2 is 2-4 h.
In the step 2, the adding amount of the ammonium chloride is 50-100% of the mass of the crude ammonium chloroplatinate.
The liquid-solid ratio of the ammonium chloroplatinate slurrying liquid in the step 3 is 5-10: 1, heating to 60-90 ℃.
In the step 4, hydrogen peroxide hydrochloride is adopted to dissolve the platinum element to obtain a dissolved solution containing the platinum element, and the specific implementation method comprises the following steps:
firstly, washing platinum element with pure water, filtering out platinum black, then adding hydrochloric acid, then adding hydrogen peroxide until the platinum black is completely dissolved, heating and boiling after dissolution to evaporate residual hydrochloric acid, finally diluting with pure water to control the concentration of platinum in the solution to be about 50g/L, cooling and filtering to obtain a dissolved solution.
The volume ratio of the hydrochloric acid to the hydrogen peroxide is 0.8-1.2: 1.
the specific implementation method of the ammonium chloride fractional precipitation method in the step 5 comprises the following steps:
heating the dissolved solution to boil, adding ammonium chloride to precipitate platinum in a first step by using ammonium chloroplatinate to obtain high-purity ammonium chloroplatinate; and adding ammonium chloride into the platinum-containing solution after the first-step precipitation again to completely precipitate the platinum-containing solution to obtain low-purity ammonium chloroplatinate.
The adding amount of the ammonium chloride precipitate in the first step is 1.5-2% of the mass of the dissolving solution, and the adding amount of the ammonium chloride precipitate in the second step is 15-20% of the mass of the dissolving solution.
The method has the beneficial effects that impurity elements in the crude ammonium chloroplatinate are removed by adopting an aqueous solution chlorination method, the ammonium chloroplatinate is refined by adopting a hydrazine hydrate reduction-hydrochloric acid hydrogen peroxide dissolution-ammonium chloride fractional precipitation method to obtain the spongy platinum, the period of the whole process is short, the raw materials are not wasted, and the method is easy to popularize.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a preparation method of spongy platinum, which is implemented according to the following steps:
step 1, according to the ratio of 5-10: 1, pulping the crude ammonium chloroplatinate by using pure water, heating to 80-90 ℃, adding hydrochloric acid and sodium chlorate, and uniformly stirring to obtain a mixed solution;
wherein, the adding amount of the hydrochloric acid is 10-20% of the volume of the slurried solution, the adding amount of the sodium chlorate is 5-10% of the mass of the crude ammonium chloroplatinate, and the stirring time is 1-2 h;
step 2, boiling the mixed solution obtained in the step 1 and keeping the boiled mixed solution for 2-4 hours, then adding ammonium chloride, and filtering the mixed solution after the mixed solution is cooled to obtain high-purity ammonium chloroplatinate; wherein the adding amount of the ammonium chloride is 50-100% of the mass of the crude ammonium chloroplatinate;
step 3, slurrying high-purity ammonium chloroplatinate, adjusting the pH value to 8-9, heating to 60-90 ℃, and then adding hydrazine hydrate for reduction to obtain platinum elements; wherein the liquid-solid ratio of the high-purity ammonium chloroplatinate slurrying liquid is 5-10: 1
Step 4, washing the platinum element by pure water, filtering out platinum black, then adding hydrochloric acid, adding hydrogen peroxide until the platinum black is completely dissolved, heating and boiling after dissolution to evaporate residual hydrochloric acid, finally diluting by pure water to control the concentration of platinum in the solution, cooling and filtering to obtain a dissolved solution; the volume ratio of the hydrochloric acid to the hydrogen peroxide is 0.8-1.2: 1;
step 5, heating the dissolved solution to boil, adding ammonium chloride to enable platinum to be subjected to first-step precipitation by ammonium chloroplatinate, and obtaining high-purity ammonium chloroplatinate; adding ammonium chloride into the platinum-containing solution after the first-step precipitation again to completely precipitate the platinum-containing solution to obtain low-purity ammonium chloroplatinate; and finally, calcining the ammonium chloroplatinate obtained by the first-step precipitation to obtain spongy platinum, and returning the ammonium chloroplatinate obtained by the second-step precipitation to the step 1. The adding amount of the ammonium chloride precipitate in the first step is 1.5-2% of the mass of the dissolving solution, and the adding amount of the ammonium chloride precipitate in the second step is 15-20% of the mass of the dissolving solution.
Compared with the existing preparation method, the invention mainly has the following technical advantages: according to the invention, impurity elements in crude ammonium chloroplatinate are removed by adopting an aqueous solution chlorination method, ammonium chloroplatinate is refined by adopting a hydrazine hydrate reduction-hydrochloric acid hydrogen peroxide dissolution-ammonium chloride fractional precipitation method to obtain spongy platinum, the period of the whole process is short, the waste of raw materials is avoided, and the method is easy to popularize.
Example 1
The embodiment 1 of the invention provides a preparation method of sponge platinum, which is implemented according to the following steps:
adding 10L of water into 1kg of crude ammonium chloroplatinate for slurrying, heating to 85 ℃, adding 1.2L of industrial hydrochloric acid and 70g of sodium chlorate, keeping the temperature and stirring for 1h, boiling the solution for 2h for chlorine removal, adding 800g of ammonium chloride into the solution, cooling the solution, filtering to obtain high-purity ammonium chloroplatinate, adding 7L of water into the high-purity ammonium chloroplatinate for slurrying, adding caustic soda flakes to adjust the pH value to 8, heating to 65 ℃, and adding a proper amount of hydrazine hydrate to obtain platinum element;
washing platinum element with pure water, filtering out platinum black, then adding hydrochloric acid, adding hydrogen peroxide until the platinum black is completely dissolved, heating and boiling after dissolution to evaporate residual hydrochloric acid, finally diluting with pure water to control the concentration of platinum in the solution to be about 50g/L, cooling and filtering to obtain a dissolved solution; the volume ratio of the hydrochloric acid to the hydrogen peroxide is 0.8: 1; heating the dissolved solution to boil, adding ammonium chloride to precipitate platinum in a first step by using ammonium chloroplatinate to obtain high-purity ammonium chloroplatinate; adding ammonium chloride into the platinum-containing solution after the first-step precipitation again to completely precipitate the platinum-containing solution to obtain low-purity ammonium chloroplatinate; wherein the adding amount of the ammonium chloride precipitate in the first step is 1.5% of the mass of the dissolving solution, and the adding amount of the ammonium chloride precipitate in the second step is 15% of the mass of the dissolving solution. (ii) a And finally, calcining the ammonium chloroplatinate obtained by the first-step precipitation to obtain the spongy platinum.
Example 2
The embodiment 2 of the invention provides a preparation method of sponge platinum, which is implemented according to the following steps:
1kg of crude ammonium chloroplatinate was slurried by adding 8L of water, the temperature was raised to 88 ℃ and 1.5L of industrial hydrochloric acid and 60g of sodium chlorate were added, and the mixture was stirred for 1.5 hours while maintaining the temperature. The solution was boiled for 3h to drive off chlorine. Adding 900g of ammonium chloride into the solution, filtering after the solution is cooled to obtain high-purity ammonium chloroplatinate, adding 8L of water into the high-purity ammonium chloroplatinate to perform slurrying, adding caustic soda flakes to adjust the pH value to 8, heating to 70 ℃, and adding a proper amount of hydrazine hydrate to obtain platinum elements;
washing platinum element with pure water, filtering out platinum black, then adding hydrochloric acid, adding hydrogen peroxide until the platinum black is completely dissolved, heating and boiling after dissolution to evaporate residual hydrochloric acid, finally diluting with pure water to control the concentration of platinum in the solution to be about 50g/L, cooling and filtering to obtain a dissolved solution; the volume ratio of the hydrochloric acid to the hydrogen peroxide is 1: 1; heating the dissolved solution to boil, adding ammonium chloride to precipitate platinum in a first step by using ammonium chloroplatinate to obtain high-purity ammonium chloroplatinate; adding ammonium chloride into the platinum-containing solution after the first-step precipitation again to completely precipitate the platinum-containing solution to obtain low-purity ammonium chloroplatinate; wherein the adding amount of the ammonium chloride precipitate in the first step is 1.6% of the mass of the dissolving solution, and the adding amount of the ammonium chloride precipitate in the second step is 16% of the mass of the dissolving solution. (ii) a And finally, calcining the ammonium chloroplatinate obtained by the first-step precipitation to obtain the spongy platinum.
Example 3
The embodiment 3 of the invention provides a preparation method of sponge platinum, which is implemented according to the following steps:
adding 7L of water into 1kg of crude ammonium chloroplatinate for slurrying, heating to 82 ℃, adding 1.8L of industrial hydrochloric acid and 80g of sodium chlorate, keeping the temperature, stirring for 2 hours, and boiling the solution for 4 hours for chlorine removal. Adding 1000g of ammonium chloride into the solution, filtering after the solution is cooled to obtain high-purity ammonium chloroplatinate, adding 8L of water into the high-purity ammonium chloroplatinate to perform slurrying, adding caustic soda flakes to adjust the pH value to 8, heating to 75 ℃, and adding a proper amount of hydrazine hydrate to obtain platinum elements;
washing platinum element with pure water, filtering out platinum black, then adding hydrochloric acid, adding hydrogen peroxide until the platinum black is completely dissolved, heating and boiling after dissolution to evaporate residual hydrochloric acid, finally diluting with pure water to control the concentration of platinum in the solution to be about 50g/L, cooling and filtering to obtain a dissolved solution; the volume ratio of the hydrochloric acid to the hydrogen peroxide is 1.1: 1; heating the dissolved solution to boil, adding ammonium chloride to precipitate platinum in a first step by using ammonium chloroplatinate to obtain high-purity ammonium chloroplatinate; adding ammonium chloride into the platinum-containing solution after the first-step precipitation again to completely precipitate the platinum-containing solution to obtain low-purity ammonium chloroplatinate; wherein the adding amount of the ammonium chloride precipitate in the first step is 1.7% of the mass of the dissolving solution, and the adding amount of the ammonium chloride precipitate in the second step is 17% of the mass of the dissolving solution. (ii) a And finally, calcining the ammonium chloroplatinate obtained by the first-step precipitation to obtain the spongy platinum.
Example 4
Embodiment 4 of the present invention provides a preparation method of spongy platinum, which is specifically implemented according to the following steps:
adding 8L of water into 1kg of crude ammonium chloroplatinate to perform slurrying, heating to 83 ℃, adding 1.2L of industrial hydrochloric acid and 72g of sodium chlorate, keeping the temperature and stirring for 1h, boiling the solution for 2.5h to remove chlorine, adding 800g of ammonium chloride into the solution, cooling the solution, filtering to obtain high-purity ammonium chloroplatinate, adding 7.5L of water into the high-purity ammonium chloroplatinate to perform slurrying, adding caustic soda flakes to adjust the pH value to 8, heating to 82 ℃, and adding a proper amount of hydrazine hydrate to obtain platinum element;
washing platinum element with pure water, filtering out platinum black, then adding hydrochloric acid, adding hydrogen peroxide until the platinum black is completely dissolved, heating and boiling after dissolution to evaporate residual hydrochloric acid, finally diluting with pure water to control the concentration of platinum in the solution to be about 50g/L, cooling and filtering to obtain a dissolved solution; the volume ratio of the hydrochloric acid to the hydrogen peroxide is 1.2: 1; heating the dissolved solution to boil, adding ammonium chloride to precipitate platinum in a first step by using ammonium chloroplatinate to obtain high-purity ammonium chloroplatinate; adding ammonium chloride into the platinum-containing solution after the first-step precipitation again to completely precipitate the platinum-containing solution to obtain low-purity ammonium chloroplatinate; wherein the adding amount of the ammonium chloride precipitate in the first step is 1.6% of the mass of the dissolving solution, and the adding amount of the ammonium chloride precipitate in the second step is 18% of the mass of the dissolving solution. (ii) a And finally, calcining the ammonium chloroplatinate obtained by the first-step precipitation to obtain the spongy platinum.
Example 5
Embodiment 5 of the present invention provides a preparation method of sponge platinum, which is specifically implemented according to the following steps:
1kg of crude ammonium chloroplatinate was slurried with 9L of water, heated to 88 ℃ and added with 1.5L of industrial hydrochloric acid and 60g of sodium chlorate, the temperature was maintained and the mixture was stirred for 1.5 h. The solution was boiled for 4h to drive off chlorine. Adding 900g of ammonium chloride into the solution, filtering after the solution is cooled to obtain high-purity ammonium chloroplatinate, adding 9L of water into the high-purity ammonium chloroplatinate to perform slurrying, adding caustic soda flakes to adjust the pH value to 9, heating to 86 ℃, and adding a proper amount of hydrazine hydrate to obtain platinum elements;
washing platinum element with pure water, filtering out platinum black, then adding hydrochloric acid, adding hydrogen peroxide until the platinum black is completely dissolved, heating and boiling after dissolution to evaporate residual hydrochloric acid, finally diluting with pure water to control the concentration of platinum in the solution to be about 50g/L, cooling and filtering to obtain a dissolved solution; the volume ratio of the hydrochloric acid to the hydrogen peroxide is 0.9: 1; heating the dissolved solution to boil, adding ammonium chloride to precipitate platinum in a first step by using ammonium chloroplatinate to obtain high-purity ammonium chloroplatinate; adding ammonium chloride into the platinum-containing solution after the first-step precipitation again to completely precipitate the platinum-containing solution to obtain low-purity ammonium chloroplatinate; wherein the adding amount of the ammonium chloride precipitate in the first step is 1.8% of the mass of the dissolving solution, and the adding amount of the ammonium chloride precipitate in the second step is 17% of the mass of the dissolving solution. (ii) a And finally, calcining the ammonium chloroplatinate obtained by the first-step precipitation to obtain the spongy platinum.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.
Claims (10)
1. The preparation method of the spongy platinum is characterized by comprising the following steps:
step 1, slurrying crude ammonium chloroplatinate, heating, adding hydrochloric acid and sodium chlorate, and uniformly stirring to obtain a mixed solution;
step 2, boiling the mixed solution obtained in the step 1 and keeping the mixed solution for a fixed time, then adding ammonium chloride, and filtering the mixed solution after the mixed solution is cooled to obtain high-purity ammonium chloroplatinate;
step 3, slurrying high-purity chloroplatinic acid ammonium, adjusting the pH value to 8-9, heating, and then adding hydrazine hydrate for reduction to obtain platinum elements;
step 4, dissolving the platinum element in the step 3 by using hydrochloric acid hydrogen peroxide to obtain a dissolved solution containing the platinum element;
and 5, performing fractional precipitation on the dissolved solution in the step 4 by adopting an ammonium chloride precipitation method to obtain ammonium chloroplatinate, calcining the ammonium chloroplatinate obtained by the first-step precipitation to obtain spongy platinum, and returning the ammonium chloroplatinate obtained by the second-step precipitation to the step 1.
2. The method for preparing spongy platinum according to claim 1, wherein the specific method for slurrying crude ammonium chloroplatinate in the step 1 is as follows: mixing pure water according to the proportion of 5-10: 1 volume ratio was added to crude ammonium chloroplatinate for slurrying.
3. The method for preparing spongy platinum according to any one of claims 1 and 2, wherein the heating temperature in the step 1 is 80-90 ℃, the addition amount of the hydrochloric acid is 10% -20% of the volume of the solution after slurrying, the addition amount of the sodium chlorate is 5% -10% of the mass of the crude ammonium chloroplatinate, and the stirring time is 1-2 hours.
4. The method for preparing spongy platinum as claimed in claim 3, wherein the fixing time in step 2 is 2-4 h.
5. The method for preparing spongy platinum as claimed in claim 4, wherein the amount of ammonium chloride added in step 2 is 50-100% by mass of the crude ammonium chloroplatinate.
6. The method for preparing spongy platinum according to claim 5, wherein the liquid-solid ratio of the ammonium chloroplatinate slurrying solution in the step 3 is 5-10: 1, heating to 60-90 ℃.
7. The preparation method of spongy platinum as claimed in claim 6, wherein the platinum element is dissolved by hydrogen peroxide hydrochloride in the step 4 to obtain a solution containing the platinum element, and the specific implementation method is as follows:
firstly, washing platinum element with pure water, filtering out platinum black, then adding hydrochloric acid, then adding hydrogen peroxide until the platinum black is completely dissolved, heating and boiling after dissolution to evaporate residual hydrochloric acid, finally diluting with pure water to control the concentration of platinum in the solution to be about 50g/L, cooling and filtering to obtain a dissolved solution.
8. The preparation method of spongy platinum as claimed in claim 7, wherein the volume ratio of the hydrochloric acid to the hydrogen peroxide is 0.8-1.2: 1.
9. the method for preparing spongy platinum according to claim 8, wherein the step-by-step ammonium chloride precipitation method in the step 5 is implemented by:
heating the dissolved solution to boil, adding ammonium chloride to precipitate platinum in a first step by using ammonium chloroplatinate to obtain high-purity ammonium chloroplatinate; and adding ammonium chloride into the platinum-containing solution after the first-step precipitation again to completely precipitate the platinum-containing solution to obtain low-purity ammonium chloroplatinate.
10. The method for preparing spongy platinum as claimed in claim 9, wherein the amount of ammonium chloride precipitated in the first step is 1.5-2% by mass of the dissolving solution, and the amount of ammonium chloride precipitated in the second step is 15-20% by mass of the dissolving solution.
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| CN114717418B (en) * | 2022-02-24 | 2024-02-23 | 阳谷祥光铜业有限公司 | Method for extracting high-purity sponge platinum from platinum waste liquid |
| CN114604911A (en) * | 2022-03-08 | 2022-06-10 | 金川集团股份有限公司 | Method for removing potassium and sodium from ammonium chloroplatinate product |
| CN114604911B (en) * | 2022-03-08 | 2023-09-22 | 金川集团股份有限公司 | Method for removing potassium and sodium from ammonium chloroplatinate product |
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