CN115386728A - Recycling treatment process for unqualified products and crushed materials of zirconium alloy material - Google Patents
Recycling treatment process for unqualified products and crushed materials of zirconium alloy material Download PDFInfo
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- CN115386728A CN115386728A CN202210874174.5A CN202210874174A CN115386728A CN 115386728 A CN115386728 A CN 115386728A CN 202210874174 A CN202210874174 A CN 202210874174A CN 115386728 A CN115386728 A CN 115386728A
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- 229910001093 Zr alloy Inorganic materials 0.000 title claims abstract description 50
- 239000000956 alloy Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000004064 recycling Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 title claims description 52
- 238000000498 ball milling Methods 0.000 claims abstract description 30
- 238000001035 drying Methods 0.000 claims abstract description 27
- 238000006356 dehydrogenation reaction Methods 0.000 claims abstract description 21
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000005485 electric heating Methods 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000004806 packaging method and process Methods 0.000 abstract description 4
- 238000005303 weighing Methods 0.000 abstract description 4
- 238000012216 screening Methods 0.000 abstract description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 239000011888 foil Substances 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910000986 non-evaporable getter Inorganic materials 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
-
- 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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
-
- 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
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/14—Obtaining zirconium or hafnium
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a recycling treatment process of unqualified products and crushed aggregates of zirconium alloy materials, which can recycle the unqualified products and crushed aggregates of the zirconium alloy materials through the steps of zirconium alloy (unqualified products and crushed aggregates for physical and chemical detection tests) pretreatment crushing → hydrogenation → ball milling, drying → dehydrogenation → ball milling, screening, drying → particle size detection → weighing and packaging and the like. The method can reduce the production quality cost of the zirconium alloy material and improve the reutilization rate of the zirconium alloy material.
Description
Technical Field
The invention relates to treatment of zirconium alloy materials, in particular to a recycling treatment process for unqualified products and crushed materials of zirconium alloy materials.
Background
The zirconium alloy is a solid solution of zirconium or other metals, the zirconium alloy is mainly used in the technical field of nuclear, and the zirconium alloy has good corrosion resistance, moderate mechanical property, lower atomic thermal neutron absorption cross section (zirconium is 0.18 target en) in high-temperature and high-pressure water and steam at the temperature of 300-400 ℃, and has good compatibility with nuclear fuel, so that the zirconium alloy can be used as a core structure material of a water-cooled nuclear reactor. Zirconium alloys are also used in corrosion resistant parts and pharmaceutical devices, and are also widely used as non-evaporable getters in the electro-vacuum and light bulb industries.
In the production of zirconium alloy materials, a certain amount of unqualified products and broken samples after physical analysis and mechanical property detection are generated. Because zirconium powder is expensive, unqualified products and crushed materials in zirconium alloy material products are recycled in order to reduce quality cost, the reutilization rate of zirconium alloy materials is improved, and the research on the recovery process of zirconium alloy materials is a practical problem which needs to be considered in the production of zirconium alloy materials.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a recycling treatment process for unqualified products and crushed aggregates of zirconium alloy materials, wherein the treatment process is used for recycling the unqualified products and the crushed aggregates of the zirconium alloy materials, and the treatment process can reduce the production quality cost of the zirconium alloy materials and improve the recycling rate of the zirconium alloy materials.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a recycling treatment process for unqualified products and crushed materials of zirconium alloy materials comprises the following steps:
s1, pretreating and crushing unqualified zirconium alloy products and crushed materials;
s2, introducing hydrogen into the hydrogenation furnace to carry out hydrogenation treatment on the pretreated and crushed material;
s3, filling the hydrogenated product into a ball milling tank, adding pure water, carrying out wet ball milling, and drying after ball milling;
s4, carrying out dehydrogenation treatment on the dried material in a dehydrogenation furnace;
s5, putting the materials subjected to dehydrogenation treatment into a ball milling tank, adding pure water for wet ball milling, taking the materials out of the tank after ball milling, sieving the materials in a pure water medium by a 400-mesh sieve, transferring the materials below the mesh into a drying furnace for drying treatment, and transferring the materials above the mesh into the step S3 for treatment;
and S6, detecting chemical components and particle sizes of the dried materials according to batches.
In the step S1, the pretreatment crushing is to polish, remove and clean the bonding materials and foreign matters on the appearance of the spherical or columnar product by using a clamping tool.
Before the step S2, adding 0.5L of industrial alcohol into the polished zirconium alloy material in a pan of 10kg for soaking, stirring and cleaning for 5min; and fishing out the cleaned zirconium alloy material and drying.
In the step S2, the hydrogenation treatment is that the vacuum degree is less than 100Pa when hydrogen is introduced into the hydrogenation furnace, the electric heating temperature is 200 +/-10 ℃, and the hydrogenation time is 2 hours.
In the step S3, the hydrogenated product is subjected to wet ball milling for 1h, the drying temperature is 80 ℃, and the drying time is 24h.
And in the step S4, the dehydrogenation treatment is to place the dried material in a tray in a dehydrogenation furnace, start to vacuumize until the vacuum degree is less than 50Pa, turn on electric heating to heat the dehydrogenation furnace to ensure that the temperature in the dehydrogenation furnace is 500-550 ℃, keep the temperature for 2h, turn off the electric heating, naturally cool to room temperature, and then discharge the dehydrogenation furnace.
In the step S5, the wet ball milling time after the dehydrogenation treatment is 1h, the drying temperature of the material smaller than 400 meshes is 80 ℃, and the drying time is 24h.
The recycling treatment process for the unqualified products and the crushed materials of the zirconium alloy material, which is designed by adopting the technical scheme, can recycle the unqualified products and the crushed materials of the zirconium alloy material through the steps of zirconium alloy (the unqualified products and the crushed materials subjected to the physical and chemical detection test) pretreatment crushing → hydrogenation → ball milling, drying → dehydrogenation → ball milling, screening, drying → granularity detection → weighing and packaging and the like. The method has the advantages of clear process principle, reasonable process flow, simple operation, high treatment efficiency, no need of large-scale equipment and facilities, low cost and high efficiency, and improves the reutilization rate of the zirconium alloy material.
Drawings
FIG. 1 shows a schematic flow diagram of the present invention.
Detailed Description
The recycling treatment process of the rejected products and crushed materials of the zirconium alloy material is specifically described below with reference to the accompanying drawings.
The invention relates to a recycling treatment process for unqualified products and crushed aggregates of zirconium alloy materials, which comprises the following operation steps of:
1. pretreating and crushing zirconium alloy (unqualified products, crushed materials for a pressure resistance test and a physicochemical detection test), and polishing, removing and cleaning spherical or cylindrical products with adhesive and foreign matters on the appearance by using a special clamping tool;
2. adding 0.5L of industrial alcohol into a polished zirconium alloy material according to a pan of 10kg for infiltration, and stirring and cleaning for 5min by using a copper shovel;
3. taking out the cleaned zirconium alloy material, putting the zirconium alloy material into a stainless steel tray, and starting a fan below an axial flow fan to dry the zirconium alloy material;
4. the zirconium alloy material is filled into a plastic bag according to 10kg per bag by an electronic scale, argon gas is filled into the filled plastic bag, and the plastic bag is sealed by a sealing machine. Labels are attached to the plastic bags, and material names, batches, categories, weights, dates and the like are marked. Putting the sealed plastic bags into an iron barrel, and pressing each barrel to 40 kg;
5. introducing hydrogen into a hydrogenation furnace for hydrogenation treatment, opening the packaging bag, taking out the zirconium alloy material, placing the zirconium alloy material in a porcelain plate, and uniformly paving the zirconium alloy material to a thickness not more than 15mm. When hydrogen is introduced into the hydrogenation furnace, the vacuum degree is less than 100Pa, the electric heating temperature is 200 +/-10 ℃, and the hydrogenation time is 2 hours;
6. and (3) ball milling, namely filling the hydrogenated product into a ball milling tank, adding pure water, carrying out wet ball milling for 1h, after the ball milling is finished, putting the discharged material into a material tray for drying, and drying at the temperature of 80 ℃ for 24h. The process is called crushing for short;
7. performing dehydrogenation treatment, namely putting the dried material into a tray and placing the tray in a dehydrogenation furnace, starting to vacuumize until the vacuum degree is less than 50Pa, starting electrical heating to heat the dehydrogenation furnace, keeping the temperature in the furnace between 500 and 550 ℃ for 2 hours, turning off the electrical heating, naturally cooling to room temperature, and discharging the material out of the furnace;
8. ball-milling, screening, the material after will dehydrogenating is packed into and is added the pure water in the ball-milling jar, carries out the wet process ball-milling, and the ball-milling time is no less than 4h, after the ball-milling, goes out the jar with the material and sieves in the pure water medium, chooses for use the accurate copper sieve of 400 targets, and what the mesh was greater than 400 mesh material, places the charging tray with its collection of copper shovel, returns operation step 6 and carries out the ball-milling breakage again. Materials with the meshes smaller than 400 meshes are arranged below the sieve;
9. drying, namely collecting materials with a mesh size smaller than 400 meshes by using a copper shovel, placing the materials in a material tray, transferring the materials into a drying furnace for drying treatment, wherein the drying temperature is 80 ℃ and the drying time is 24 hours;
10. and (4) checking chemical components and particle size detection according to batches. And (4) extracting 50g of dried material samples in each batch, filling the samples into an antistatic sealed bag for inspection, and performing chemical component and particle size detection. The granularity D90 of the zirconium alloy is less than or equal to 45 mu m;
11. weighing and packaging, weighing the qualified zirconium alloy powder by using an electronic scale according to the standard of 2kg per bag, filling the zirconium alloy powder into aluminum foil bags, and sealing the aluminum foil bags by using a sealing machine. And (3) labeling the aluminum foil bags with labels, material names, batches, types, weights, dates and the like. And (3) filling the sealed aluminum foil bags into an iron bucket card according to the weight of 40 kg of each bucket, sealing with lead, and delivering to a warehouse.
Claims (7)
1. A recycling treatment process for unqualified products and crushed materials of zirconium alloy materials is characterized by comprising the following steps:
s1, pretreating and crushing unqualified zirconium alloy products and crushed materials;
s2, introducing hydrogen into the hydrogenation furnace to carry out hydrogenation treatment on the pretreated and crushed material;
s3, filling the hydrogenated product into a ball milling tank, adding pure water, carrying out wet ball milling, and drying after ball milling;
s4, carrying out dehydrogenation treatment on the dried material in a dehydrogenation furnace;
s5, putting the materials subjected to dehydrogenation treatment into a ball milling tank, adding pure water for wet ball milling, taking the materials out of the tank after ball milling, sieving the materials in a pure water medium by a 400-mesh sieve, transferring the materials below the mesh into a drying furnace for drying treatment, and transferring the materials above the mesh into the step S3 for treatment;
and S6, detecting chemical components and particle sizes of the dried materials according to batches.
2. The process of claim 1, wherein the pre-crushing step S1 is to remove and clean the bonding material and foreign material from the appearance of the spherical or cylindrical product by using a clamping tool.
3. The recycling treatment process of the unqualified zirconium alloy materials and the crushed materials according to the claim 2, wherein before the step S2, the zirconium alloy materials after being polished are soaked and stirred and cleaned for 5min by adding 0.5L of industrial alcohol into a pan of 10 kg; and fishing out the cleaned zirconium alloy material and drying.
4. The process of claim 1, wherein the hydrogenation step S2 comprises introducing hydrogen gas into the hydrogenation furnace at a vacuum degree of less than 100Pa, at an electric heating temperature of 200 ℃ ± 10 ℃ and for a hydrogenation time of 2 hours.
5. The process of claim 1, wherein in step S3, the hydrogenated product is subjected to wet ball milling for 1 hour, the drying temperature is 80 ℃, and the drying time is 24 hours.
6. The process of claim 1, wherein in the step S4, the dehydrogenation treatment comprises loading the dried material into a tray, placing the tray into a dehydrogenation furnace, vacuumizing to a vacuum degree of less than 50Pa, heating the dehydrogenation furnace by turning on electric heating to a temperature of 500-550 ℃, keeping the temperature for 2 hours, turning off the electric heating, naturally cooling to room temperature, and discharging.
7. The process of claim 1, wherein in step S5, the wet ball milling time after the dehydrogenation treatment is 1 hour, the drying temperature of the material with a particle size of less than 400 meshes is 80 ℃, and the drying time is 24 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210874174.5A CN115386728A (en) | 2022-07-25 | 2022-07-25 | Recycling treatment process for unqualified products and crushed materials of zirconium alloy material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210874174.5A CN115386728A (en) | 2022-07-25 | 2022-07-25 | Recycling treatment process for unqualified products and crushed materials of zirconium alloy material |
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| Publication Number | Publication Date |
|---|---|
| CN115386728A true CN115386728A (en) | 2022-11-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210874174.5A Withdrawn CN115386728A (en) | 2022-07-25 | 2022-07-25 | Recycling treatment process for unqualified products and crushed materials of zirconium alloy material |
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| Country | Link |
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| CN (1) | CN115386728A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104289709A (en) * | 2014-10-31 | 2015-01-21 | 中南大学 | Preparation method for superfine zirconium powder |
| KR20190044233A (en) * | 2017-10-20 | 2019-04-30 | 한국생산기술연구원 | Method for producing high purity metal powder by repeated hydrogenation-dehydrogenation |
-
2022
- 2022-07-25 CN CN202210874174.5A patent/CN115386728A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104289709A (en) * | 2014-10-31 | 2015-01-21 | 中南大学 | Preparation method for superfine zirconium powder |
| KR20190044233A (en) * | 2017-10-20 | 2019-04-30 | 한국생산기술연구원 | Method for producing high purity metal powder by repeated hydrogenation-dehydrogenation |
Non-Patent Citations (1)
| Title |
|---|
| 中国冶金百科全书总编辑委员会《有色金属冶金》卷编辑委员会等: "中国冶金百科全书 有色金属冶金", 冶金工业出版社, pages: 627 - 628 * |
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Application publication date: 20221125 |