CN113333174B - Beneficiation reagent for flotation of tantalum and niobium in tantalum-niobium ore and preparation method thereof - Google Patents
Beneficiation reagent for flotation of tantalum and niobium in tantalum-niobium ore and preparation method thereof Download PDFInfo
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- CN113333174B CN113333174B CN202110521025.6A CN202110521025A CN113333174B CN 113333174 B CN113333174 B CN 113333174B CN 202110521025 A CN202110521025 A CN 202110521025A CN 113333174 B CN113333174 B CN 113333174B
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- tantalum
- niobium
- flotation
- beneficiation reagent
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- RHDUVDHGVHBHCL-UHFFFAOYSA-N niobium tantalum Chemical compound [Nb].[Ta] RHDUVDHGVHBHCL-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000005188 flotation Methods 0.000 title claims abstract description 27
- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 22
- 229910052758 niobium Inorganic materials 0.000 title claims abstract description 18
- 239000010955 niobium Substances 0.000 title claims abstract description 18
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 18
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims description 11
- WRMNZCZEMHIOCP-UHFFFAOYSA-N 2-phenylethanol Chemical compound OCCC1=CC=CC=C1 WRMNZCZEMHIOCP-UHFFFAOYSA-N 0.000 claims abstract description 20
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 20
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 20
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 20
- WLAMNBDJUVNPJU-UHFFFAOYSA-N 2-methylbutyric acid Chemical compound CCC(C)C(O)=O WLAMNBDJUVNPJU-UHFFFAOYSA-N 0.000 claims abstract description 10
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 10
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 10
- 239000000292 calcium oxide Substances 0.000 claims abstract description 10
- 235000012255 calcium oxide Nutrition 0.000 claims abstract description 10
- 239000001632 sodium acetate Substances 0.000 claims abstract description 10
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 10
- UAXOELSVPTZZQG-UHFFFAOYSA-N tiglic acid Natural products CC(C)=C(C)C(O)=O UAXOELSVPTZZQG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002283 diesel fuel Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000012190 activator Substances 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 12
- 238000000967 suction filtration Methods 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 230000003213 activating effect Effects 0.000 claims description 3
- 239000000110 cooling liquid Substances 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 230000005484 gravity Effects 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000006193 liquid solution Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 8
- 229940067107 phenylethyl alcohol Drugs 0.000 abstract description 6
- 239000012141 concentrate Substances 0.000 description 5
- WGQKYBSKWIADBV-UHFFFAOYSA-N benzylamine Chemical compound NCC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-N 0.000 description 2
- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 description 2
- 239000012991 xanthate Substances 0.000 description 2
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 229910000592 Ferroniobium Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005456 ore beneficiation Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/018—Mixtures of inorganic and organic compounds
-
- 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
-
- 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; Specified applications
- B03D2203/02—Ores
- B03D2203/04—Non-sulfide ores
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The beneficiation reagent for flotation of tantalum and niobium in tantalum-niobium ores is prepared from the following raw materials in parts by weight: 10-15 parts of diesel oil, 15-40 parts of sodium carbonate, 20-30 parts of sodium acetate, 15-25 parts of ammonium chloride, 12-18 parts of 2-methylbutyric acid, 1-2 parts of quicklime, 30-60 parts of p-phenylmethylamine, 4-5 parts of an activator and 20-35 parts of phenylethyl alcohol. The method has the characteristics of high sorting efficiency, high yield, small using amount, simple and reliable process flow, easy operation and the like, and is suitable for the application of tantalum-niobium ore flotation.
Description
Technical Field
The invention relates to the technical field of beneficiation, in particular to a beneficiation reagent for flotation of tantalum and niobium of tantalum-niobium ores and a preparation method thereof.
Background
At present, the tantalum-niobium metal raw materials in China mainly comprise niobite, tantalite, ferrocolumbium, rutile and the like. The flotation method is one of the tantalum-niobium ore beneficiation methods, and sometimes, in order to improve the quality of tantalum-niobium ore concentrate and remove impurities, the tantalum-niobium ore concentrate is subjected to chemical beneficiation treatment and then subjected to flotation.
The collecting agents which take the leading position in the flotation process of the tantalum-niobium ore are xanthate, cyanide, phosphate, xanthate and the like, but in actual ore dressing, results mostly cannot meet the design requirements, the tantalum-niobium ore concentrate product contains overproof tantalum and niobium, the tantalum-niobium ore concentrate is low in grade, the ore concentrate recovery rate is low, and the waste of ore resources is caused.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides the beneficiation reagent for the flotation of tantalum and niobium from tantalum-niobium ores, which has the advantages of high efficiency, high yield, small dosage, simple and reliable process flow and easiness in operation, and a preparation method thereof.
The invention relates to a beneficiation reagent for flotation of tantalum and niobium in tantalum-niobium ores, which is prepared from the following raw materials in parts by weight: 10-15 parts of diesel oil, 15-40 parts of sodium carbonate, 20-30 parts of sodium acetate, 15-25 parts of ammonium chloride, 12-18 parts of 2-methylbutyric acid, 1-2 parts of quicklime, 30-60 parts of p-phenylmethylamine, 4-5 parts of an activator and 20-35 parts of phenylethyl alcohol.
A preparation method of a beneficiation reagent for flotation of tantalum and niobium in tantalum-niobium ores comprises the following steps:
A. preparing diesel oil, ammonium chloride and quicklime into an oily solution with the volume percentage of 30-65%;
B. b, adding 2-methylbutyric acid and sodium carbonate into the solution obtained in the step A, reacting for 30-70 min, and stirring at a rotating speed of 75-145 r/min;
C. adding the solution obtained in the step B into phenylmethylamine, an activating agent, phenethyl alcohol and sodium acetate, continuously stirring at the stirring speed of 35-125 rpm, reacting for 0.5-1.5 h, and filtering, wherein the reaction temperature and the filtering temperature are 25-65 ℃; the product is a mixture of oily liquid and aqueous solution, wherein the weight percentage of the oily liquid is 30-70%, and the weight percentage of the aqueous solution is 30-70%;
D. c, evaporating the filtrate obtained by filtering in the step C, wherein the specific gravity of the evaporated solution is 2.16g/cm3~4.39 g/cm3;
E. The cooling adopts gradient cooling, and the cooling temperature is 5-30 ℃;
F. and E, carrying out suction filtration on the cooling liquid in the step E, wherein the suction filtration time is 45-100 min.
In the step B, the reaction time is 30-45 min, and the stirring speed is 75-100 r/min;
in the step C, stirring at a rotating speed of 35-80 rpm, reacting for 0.5-1.25 h, and filtering, wherein the reaction temperature and the filtering temperature are 35-50 ℃;
the cooling temperature of the step E is 8-15 ℃;
in the step F, the suction filtration time is 45 min-65 min.
Compared with the prior art, the invention has the following advantages: the method has the characteristics of high sorting efficiency, high yield, small using amount, simple and reliable process flow, easiness in operation and the like, and is suitable for the application of tantalum-niobium ore flotation.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Embodiment 1, a beneficiation reagent for flotation of tantalum and niobium from tantalum-niobium ores is prepared from the following raw materials in parts by weight: 10-15 parts of diesel oil, 15-40 parts of sodium carbonate, 20-30 parts of sodium acetate, 15-25 parts of ammonium chloride, 12-18 parts of 2-methylbutyric acid, 1-2 parts of quicklime, 30-60 parts of p-phenylmethylamine, 4-5 parts of an activator and 20-35 parts of phenylethyl alcohol. Example 1 is applied to flotation of certain tantalum-niobium ores in northern Xinjiang, and the beneficiation reagent is named LZY-20, and the indexes are as follows:
embodiment 2, a beneficiation reagent for flotation of tantalum and niobium from tantalum-niobium ores is prepared from the following raw materials in parts by weight: 10-15 parts of diesel oil, 15-40 parts of sodium carbonate, 20-30 parts of sodium acetate, 15-25 parts of ammonium chloride, 12-18 parts of 2-methylbutyric acid, 1-2 parts of quicklime, 30-60 parts of p-phenylmethylamine, 4-5 parts of an activator and 20-35 parts of phenylethyl alcohol. Example 2 applied to the flotation of certain tantalum-niobium ores in Sichuan, the beneficiation reagent is named LZY-20, and the indexes are as follows:
embodiment 3, a beneficiation reagent for flotation of tantalum and niobium from tantalum-niobium ores is prepared from the following raw materials in parts by weight: 10-15 parts of diesel oil, 15-40 parts of sodium carbonate, 20-30 parts of sodium acetate, 15-25 parts of ammonium chloride, 12-18 parts of 2-methylbutyric acid, 1-2 parts of quicklime, 30-60 parts of p-phenylmethylamine, 4-5 parts of an activator and 20-35 parts of phenylethyl alcohol. Example 3 applied to flotation of Nemeng certain tantalum niobium ores, the beneficiation reagent is named LZY-20, and the indexes are as follows:
embodiment 4, a beneficiation reagent for flotation of tantalum and niobium from tantalum-niobium ores is prepared from the following raw materials in parts by weight: 10-15 parts of diesel oil, 15-40 parts of sodium carbonate, 20-30 parts of sodium acetate, 15-25 parts of ammonium chloride, 12-18 parts of 2-methylbutyric acid, 1-2 parts of quicklime, 30-60 parts of p-phenylmethylamine, 4-5 parts of an activator and 20-35 parts of phenylethyl alcohol. Example 4 applied to flotation of certain tantalum-niobium ores in the Qinghai, the beneficiation reagent is named as LZY-20, and the indexes are as follows:
embodiment 5, a preparation method of beneficiation reagent for tantalum-niobium ore flotation comprises the following steps: A. preparing diesel oil, ammonium chloride and quicklime into an oily solution with the volume percentage of 30-65%; B. adding the solution obtained in the step A, 2-methylbutyric acid and sodium carbonate into the solution, reacting for 30-70 min, and stirring at the rotating speed of 75-145 r/min; C. adding the solution obtained in the step B into phenylmethylamine, an activating agent, phenethyl alcohol and sodium acetate, continuously stirring at the stirring speed of 35-125 rpm, reacting for 0.5-1 h, and filtering, wherein the reaction temperature and the filtering temperature are 25-65 ℃; the product is a mixture of oily liquid and aqueous solution, wherein the weight percentage of the oily liquid is 30-70%, and the weight percentage of the aqueous solution is 30-70%; D. c, evaporating the filtrate obtained by filtering in the step C, wherein the specific gravity of the evaporated solution is 2.16g/cm3~4.39 g/cm3(ii) a E. The cooling adopts gradient cooling, and the cooling temperature is 5-30 ℃; F. to what is neededAnd E, carrying out suction filtration on the cooling liquid in the step E, wherein the suction filtration time is 45-100 min. In the step B, the reaction time is 30-45 min, and the stirring speed is 75-100 r/min; in the step C, stirring at a rotating speed of 35-80 rpm, reacting for 0.5-1.25 h, and filtering, wherein the reaction temperature and the filtering temperature are 35-50 ℃; the cooling temperature of the step E is 8-15 ℃; and in the step F, the suction filtration time is 45-65 min.
The above description is only for the preferred embodiments of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution of the present invention and the inventive concept thereof within the scope of the present invention.
Claims (5)
1. The beneficiation reagent for flotation of tantalum and niobium in tantalum-niobium ores is characterized in that: the feed is prepared from the following raw materials in parts by weight: 10-15 parts of diesel, 15-40 parts of sodium carbonate, 20-30 parts of sodium acetate, 15-25 parts of ammonium chloride, 12-18 parts of 2-methylbutyric acid, 1-2 parts of quicklime, 30-60 parts of p-phenylmethylamine, 4-5 parts of an activator and 20-35 parts of phenethyl alcohol; the preparation method of the beneficiation reagent for flotation of tantalum and niobium from tantalum-niobium ores comprises the following steps:
A. preparing diesel oil, ammonium chloride and quicklime into an oily solution with the volume percentage of 30-65%;
B. adding 2-methylbutyric acid and sodium carbonate into the solution obtained in the step A, reacting for 30-70 min, and stirring at a rotating speed of 75-145 r/min;
C. b, adding p-phenylmethylamine, an activating agent, phenethyl alcohol and sodium acetate into the solution obtained in the step B, continuously stirring, reacting for 0.5-1.5 h at the stirring speed of 35-125 r/min, and filtering, wherein the reaction temperature and the filtering temperature are 25-65 ℃, the product is a mixture of oily liquid and aqueous solution, the weight percentage of the oily liquid is 30-70%, and the weight percentage of the aqueous solution is 30-70%;
D. c, evaporating the filtrate obtained by filtering in the step C, wherein the specific gravity of the evaporated solution is 2.16g/cm3~4.39 g/cm3;
E. The cooling adopts gradient cooling, and the cooling temperature is 5-30 ℃;
F. and E, carrying out suction filtration on the cooling liquid in the step E, wherein the suction filtration time is 45-100 min.
2. The preparation method of the beneficiation reagent for flotation of tantalum and niobium in tantalum-niobium ores according to claim 1, is characterized by comprising the following steps: in the step B, the reaction time is 30-45 min, and the stirring speed is 75-100 r/min.
3. The preparation method of the beneficiation reagent for flotation of tantalum and niobium from tantalum-niobium ores, according to claim 2, is characterized in that: in the step C, the stirring speed is 35-80 rpm, the reaction is carried out for 0.5-1.25 h, and then the filtration is carried out, wherein the reaction temperature and the filtration temperature are 35-50 ℃.
4. The preparation method of the beneficiation reagent for flotation of tantalum and niobium from tantalum-niobium ores, according to claim 2, is characterized in that: the cooling temperature of the step E is 8-15 ℃.
5. The preparation method of the beneficiation reagent for flotation of tantalum and niobium from tantalum-niobium ores, according to claim 2, is characterized in that: and in the step F, the suction filtration time is 45-65 min.
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CN202110521025.6A CN113333174B (en) | 2021-05-13 | 2021-05-13 | Beneficiation reagent for flotation of tantalum and niobium in tantalum-niobium ore and preparation method thereof |
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CN202110521025.6A CN113333174B (en) | 2021-05-13 | 2021-05-13 | Beneficiation reagent for flotation of tantalum and niobium in tantalum-niobium ore and preparation method thereof |
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CN113333174B true CN113333174B (en) | 2022-05-31 |
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