CN111748700A - Titanium chip recovery method - Google Patents
Titanium chip recovery method Download PDFInfo
- Publication number
- CN111748700A CN111748700A CN202010482748.5A CN202010482748A CN111748700A CN 111748700 A CN111748700 A CN 111748700A CN 202010482748 A CN202010482748 A CN 202010482748A CN 111748700 A CN111748700 A CN 111748700A
- Authority
- CN
- China
- Prior art keywords
- acid
- titanium
- recovery method
- drying
- chip recovery
- 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
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 37
- 239000010936 titanium Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000011084 recovery Methods 0.000 title claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 24
- 239000012535 impurity Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000005238 degreasing Methods 0.000 claims abstract description 6
- 238000007885 magnetic separation Methods 0.000 claims abstract description 3
- 238000010298 pulverizing process Methods 0.000 claims abstract description 3
- 239000002253 acid Substances 0.000 claims description 29
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000004140 cleaning Methods 0.000 claims description 13
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- 238000005554 pickling Methods 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 229910004077 HF-HNO3 Inorganic materials 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1204—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent
- C22B34/1213—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent by wet processes, e.g. using leaching methods or flotation techniques
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C19/00—Other disintegrating devices or methods
- B02C19/0056—Other disintegrating devices or methods specially adapted for specific materials not otherwise provided for
- B02C19/0062—Other disintegrating devices or methods specially adapted for specific materials not otherwise provided for specially adapted for shredding scrap metal, e.g. automobile bodies
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/02—Magnetic separation acting directly on the substance being separated
-
- 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
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
- C23G1/106—Other heavy metals refractory metals
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/20—Other heavy metals
- C23G1/205—Other heavy metals refractory metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C2201/00—Codes relating to disintegrating devices adapted for specific materials
- B02C2201/06—Codes relating to disintegrating devices adapted for specific materials for garbage, waste or sewage
-
- 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
Abstract
The invention discloses a titanium chip recovery method, which comprises the following steps: degreasing → washing with clear water → oxide layer removal → impurity removal → primary drying → pulverization → magnetic separation → secondary drying. The titanium chips recovered by the process have low impurity content, the tested quality is equal to that of the three-level titanium sponge, the recovery condition is met, the recovery rate of the titanium chips reaches over 95 percent, and the production cost is greatly reduced.
Description
Technical Field
The invention relates to the technical field of titanium processing, in particular to a titanium chip recovery method.
Background
In the production and processing processes of titanium ingots, oxidized substances, mixed mechanical oil, saponification liquid, dust and other impurities on the surfaces of a large amount of formed scraps and micro parts of equipment enter a molten pool together with titanium scraps if the impurities are not completely removed, so that the quality of the formed ingots is greatly influenced.
The traditional treatment method of the company cannot meet the production requirements, and only can be sold as waste titanium scraps, so that the economic benefit is extremely low, and economic loss exists.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the titanium scrap recovery method is provided, the quality of the titanium scrap recovered and treated by the process is equal to that of three-level titanium sponge, and the recovery and utilization conditions are met.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a titanium chip recovery method comprises the following steps: degreasing → washing with clear water → oxide layer removal → impurity removal → primary drying → pulverization → magnetic separation → secondary drying.
The degreasing step comprises the steps of putting titanium chips into a sodium hydroxide aqueous solution with the mass fraction of 1.5% -2%, completely immersing the titanium chips into the sodium hydroxide aqueous solution, heating to 155 +/-2 ℃, and continuously stirring for at least 15 min.
Washing with water at the temperature of 45-50 ℃; washing until the pH value is 7-7.5.
In the oxidation removal layer, titanium chips are subjected to acid cleaning twice in acid liquor, and the acid liquor adopted in the first cleaning is mixed acid of hydrochloric acid and hydrofluoric acid; the acid solution adopted in the second acid cleaning is a mixed acid of nitric acid and hydrofluoric acid. The HF-HCI solution is adopted for acid cleaning for the first time, and the surface oxide layer is removed as soon as possible, so that the efficiency is improved; second time using HF-HNO3And (4) pickling with the solution to enable the surface of the material to be bright.
The volume ratio of the hydrochloric acid to the hydrofluoric acid is 5: 1, and the concentration of the hydrochloric acid in the mixed acid is 5.5-6 wt%; the volume ratio of the nitric acid to the hydrofluoric acid is 5: 1, and the concentration of the nitric acid in the mixed acid is 5.5-6 wt%; the pickling time is more than 30min, and the pickling temperature is 50-60 ℃.
The primary drying is vacuum drying, the drying temperature is 90-105 ℃, the pressure is 50-80mbar, and the drying time is at least 3 hours.
And crushing to obtain the particle size of 0.83-20 mm.
In the magnetic selection, the field intensity of the used magnetic force is more than 5000 gauss.
And the secondary drying is vacuum drying, the drying temperature is 90-105 ℃, the pressure is 50-80mbar, and the drying is carried out until the water content is less than or equal to 0.5 Wt.%.
Has the advantages that: the titanium chips recovered by the process have low impurity content, the tested quality is equal to that of the three-level titanium sponge, the recovery condition is met, the recovery rate of the titanium chips reaches over 95 percent, and the production cost is greatly reduced.
Detailed Description
The process of the present invention is further illustrated below with reference to examples, but the invention is not limited thereto.
Examples 1 to 3
The titanium chip recovery method comprises the following steps:
1) degreasing, namely putting titanium scraps or titanium alloy scraps into a sodium hydroxide aqueous solution with the mass fraction of 1.5-2% to ensure that the titanium scraps or the titanium alloy scraps are completely immersed in the sodium hydroxide aqueous solution, heating to 155 +/-2 ℃, and continuously stirring for at least 15 min.
2) Cleaning with water: the cleaning temperature is 45-50 ℃; washing until the pH value is 7-7.5.
3) Removing an oxidation layer: carrying out acid cleaning on titanium chips in acid liquor for two times, wherein the acid liquor adopted in the first cleaning is mixed acid of hydrochloric acid and hydrofluoric acid; the acid solution adopted in the second acid cleaning is a mixed acid of nitric acid and hydrofluoric acid. The HF-HCI solution is adopted for acid cleaning for the first time, and the surface oxide layer is removed as soon as possible, so that the efficiency is improved; second time using HF-HNO3And (4) pickling with the solution to enable the surface of the material to be bright.
The volume ratio of the hydrochloric acid to the hydrofluoric acid is 5: 1, and the concentration of the hydrochloric acid in the mixed acid is 5.5-6 wt%; the volume ratio of the nitric acid to the hydrofluoric acid is 5: 1, and the concentration of the nitric acid in the mixed acid is 5.5-6 wt%; the pickling time is more than 30min, and the pickling temperature is 50-60 ℃.
4) Removing impurities and larger impurities.
5) The primary drying is vacuum drying, the drying temperature is 90-105 ℃, the pressure is 50-80mbar, and the drying lasts for at least 3 hours.
6) Crushing to 0.83-20 mm size.
7) In magnetic selection, the field intensity of the used magnetic force is more than 5000 gauss.
8) And (3) secondary drying, namely vacuum drying, wherein the drying temperature is 90-105 ℃, the pressure is 50-80mbar, and the drying is carried out until the water content is less than or equal to 0.5 Wt.%.
After the titanium chips are treated by adopting the process, the performance detection result is as follows:
the titanium chips recovered by the process have low impurity content, the tested quality is equal to that of the three-level titanium sponge, the recovery condition is met, the recovery rate of the titanium chips reaches over 95 percent, and the production cost is greatly reduced.
Claims (9)
1. A titanium chip recovery method comprises the following steps: degreasing → washing with clear water → oxide layer removal → impurity removal → primary drying → pulverization → magnetic separation → secondary drying.
2. A titanium chip recovery method according to claim 1, characterized in that: the degreasing step comprises the steps of putting titanium chips into a sodium hydroxide aqueous solution with the mass fraction of 1.5% -2%, completely immersing the titanium chips into the sodium hydroxide aqueous solution, heating to 155 +/-2 ℃, and continuously stirring for at least 15 min.
3. A titanium chip recovery method according to claim 1, characterized in that: washing with water at the temperature of 45-50 ℃; washing until the pH value is 7-7.5.
4. A titanium chip recovery method according to claim 1, characterized in that: in the oxidation removal layer, titanium chips are subjected to acid cleaning twice in acid liquor, and the acid liquor adopted in the first cleaning is mixed acid of hydrochloric acid and hydrofluoric acid; the acid solution adopted in the second acid cleaning is a mixed acid of nitric acid and hydrofluoric acid.
5. The titanium chip recovery method according to claim 4, wherein: the volume ratio of the hydrochloric acid to the hydrofluoric acid is 5: 1, and the concentration of the hydrochloric acid in the mixed acid is 5.5-6 wt%; the volume ratio of the nitric acid to the hydrofluoric acid is 5: 1, and the concentration of the nitric acid in the mixed acid is 5.5-6 wt%; the pickling time is more than 30min, and the pickling temperature is 50-60 ℃.
6. A titanium chip recovery method according to claim 1, characterized in that: the primary drying is vacuum drying, the drying temperature is 90-105 ℃, the pressure is 50-80mbar, and the drying time is at least 3 hours.
7. A titanium chip recovery method according to claim 1, characterized in that: and crushing to obtain the particle size of 0.83-20 mm.
8. A titanium chip recovery method according to claim 1, characterized in that: in the magnetic selection, the field intensity of the used magnetic force is more than 5000 gauss.
9. A titanium chip recovery method according to claim 1, characterized in that: and the secondary drying is vacuum drying, the drying temperature is 90-105 ℃, the pressure is 50-80mbar, and the drying is carried out until the water content is less than or equal to 0.5 Wt.%.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN202010482748.5A CN111748700A (en) | 2020-06-01 | 2020-06-01 | Titanium chip recovery method |
Applications Claiming Priority (1)
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CN202010482748.5A CN111748700A (en) | 2020-06-01 | 2020-06-01 | Titanium chip recovery method |
Publications (1)
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CN111748700A true CN111748700A (en) | 2020-10-09 |
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Family Applications (1)
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CN202010482748.5A Pending CN111748700A (en) | 2020-06-01 | 2020-06-01 | Titanium chip recovery method |
Country Status (1)
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112458315A (en) * | 2020-11-13 | 2021-03-09 | 禄丰新立钛业有限公司 | Production method for impurity removal, quality improvement and upgrading of titanium sponge |
CN113600818A (en) * | 2021-08-17 | 2021-11-05 | 宁波创润新材料有限公司 | Method for preparing high-purity titanium powder by using high-purity titanium ingot turning scraps and product thereof |
CN117427949A (en) * | 2023-12-19 | 2024-01-23 | 陕西天成航空材料股份有限公司 | Titanium bits belt cleaning device |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5719356A (en) * | 1980-07-08 | 1982-02-01 | Nippon Stainless Steel Co Ltd | Recovering method for metallic titanium from titanium-grinding sludge |
CN103966465A (en) * | 2014-04-24 | 2014-08-06 | 青海聚能钛业有限公司 | Titanium scrap recycling and remelting technology |
CN104109761A (en) * | 2013-12-25 | 2014-10-22 | 浙江五环钛业股份有限公司 | Titanium chip recovery technology |
CN106702160A (en) * | 2015-08-05 | 2017-05-24 | 宁波创润新材料有限公司 | Method for processing ultrahigh purity titanium scraps |
CN106757097A (en) * | 2016-12-26 | 2017-05-31 | 宝纳资源控股(集团)有限公司 | Useless titanium surface degreasing device and useless titanium surface impurity sweep-out method |
-
2020
- 2020-06-01 CN CN202010482748.5A patent/CN111748700A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5719356A (en) * | 1980-07-08 | 1982-02-01 | Nippon Stainless Steel Co Ltd | Recovering method for metallic titanium from titanium-grinding sludge |
CN104109761A (en) * | 2013-12-25 | 2014-10-22 | 浙江五环钛业股份有限公司 | Titanium chip recovery technology |
CN103966465A (en) * | 2014-04-24 | 2014-08-06 | 青海聚能钛业有限公司 | Titanium scrap recycling and remelting technology |
CN106702160A (en) * | 2015-08-05 | 2017-05-24 | 宁波创润新材料有限公司 | Method for processing ultrahigh purity titanium scraps |
CN106757097A (en) * | 2016-12-26 | 2017-05-31 | 宝纳资源控股(集团)有限公司 | Useless titanium surface degreasing device and useless titanium surface impurity sweep-out method |
Non-Patent Citations (1)
Title |
---|
《稀有金属材料加工手册》编写组: "《稀有金属材料加工手册》", 31 March 1984, 冶金工业出版社 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112458315A (en) * | 2020-11-13 | 2021-03-09 | 禄丰新立钛业有限公司 | Production method for impurity removal, quality improvement and upgrading of titanium sponge |
CN113600818A (en) * | 2021-08-17 | 2021-11-05 | 宁波创润新材料有限公司 | Method for preparing high-purity titanium powder by using high-purity titanium ingot turning scraps and product thereof |
CN117427949A (en) * | 2023-12-19 | 2024-01-23 | 陕西天成航空材料股份有限公司 | Titanium bits belt cleaning device |
CN117427949B (en) * | 2023-12-19 | 2024-03-05 | 陕西天成航空材料股份有限公司 | Titanium bits belt cleaning device |
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Application publication date: 20201009 |