7N Tellurium Crystal Kukura uye Kucheneswa
I. Raw Material Pretreatment uye Preliminary Kucheneswa
- .Raw Material Sarudzo uye Kupwanya.
- .Zvinhu Zvinodiwa: Shandisa tellurium ore kana anode slime (Te yemukati ≥5%), zviri nani mhangura inonyungudutsa anode slime (ine Cu₂Te, Cu₂Se) seyakabikwa.
- .Pretreatment Process:
- Kupwanya kwakashata kusvika kuhukuru ≤5mm, kuchiteverwa nebhora kugaya kusvika ≤200 mesh;
- Magnetic separation (magnetic field intensity ≥0.8T) kubvisa Fe, Ni, uye mamwe magineti tsvina;
- Froth flotation (pH = 8-9, xanthate vateresi) kuparadzanisa SiO₂, CuO, uye zvimwe zvisiri zvemagnetic tsvina.
- .Zvekungwaririra: Dzivisa kuunza mwando panguva yekunyorova (inoda kuomeswa usati wagocha); kudzora ambient humidity ≤30%.
- .Pyrometallurgical Roasting uye Oxidation.
- .Process Parameters:
- Oxidation yekugocha tembiricha: 350-600 ° C (taged control: yakaderera tembiricha ye desulfurization, yakanyanya tembiricha yeoxidation);
- Nguva yekubika: 6-8 maawa, neO₂ kuyerera kwe5-10 L / min;
- Reagent: Yakaiswa sulfuric acid (98% H₂SO₄), chiyero chehuwandu Te₂SO₄ = 1: 1.5.
- .Chemical Reaction:
Cu2Te+2O2+2H2SO4→2CuSO4+TeO2+2H2OCu2Te+2O2+2H2 SO4→2CuSO4+TeO2+2H2O - .Zvekungwaririra: Chengetedza tembiricha ≤600°C kudzivirira TeO₂ volatilization (boiling point 387°C); gadzirisa gasi rinopedza simba neNaOH scrubbers.
II. Electrorefining uye Vacuum Distillation
- .Electrorefining.
- .Electrolyte System:
- Electrolyte kuumbwa: H₂SO₄ (80–120g/L), TeO₂ (40–60g/L), kuwedzera (gelatin 0.1–0.3g/L);
- Kudzora tembiricha: 30–40°C, kutenderera kuyerera 1.5–2 m³/h.
- .Process Parameters:
- Kuwanda kwezvino: 100–150 A/m², sero voltage 0.2–0.4V;
- Electrode spacing: 80–120mm, cathode deposition ukobvu 2–3mm/8h;
- Kusachena kubvisa kushanda zvakanaka: Cu ≤5ppm, Pb ≤1ppm.
- .Zvekungwaririra: Gara uchisefa electrolyte (kurongeka ≤1μm); mechanically polish anode nzvimbo kudzivirira passivation.
- .Vacuum Distillation.
- .Process Parameters:
- Vacuum level: ≤1×10⁻²Pa, tembiricha yedistillation 600–650°C ;
- Condenser zone tembiricha: 200-250 ° C, Te vapor condensation kunyatsoshanda ≥95%;
- Distillation nguva: 8-12h, single-batch simba ≤50kg .
- .Kuparadzirwa Kwekusachena: Tsvina inofashaira yakaderera (Se, S) inoungana kumberi kwecondenser; tsvina inofashaira yakawanda (Pb, Ag) inoramba iri mumasara .
- .Zvekungwaririra: Pre-pombi vacuum system kusvika ≤5×10⁻³Pa isati yapisa kudzivirira Te oxidation.
III. Crystal Kukura (Directional Crystallization).
- .Equipment Configuration.
- .Crystal Kukura Bira ModelsTDR-70A/B (30kg kugona) kana TRDL-800 (60kg kugona);
- Crucible zvinhu: High-purity graphite (ash content ≤5ppm), zviyero Φ300×400mm;
- Kupisa nzira: Graphite kuramba kupisa, tembiricha yepamusoro 1200 ° C.
- .Process Parameters.
- .Melt Control:
- Kunyunguduka tembiricha: 500–520°C, kunyungudutsa dziva kudzika 80–120mm;
- Gasi rekudzivirira: Ar (kuchena ≥99.999%), kuyerera kwe10-15 L / min.
- .Crystallization Parameters:
- Kudhonza chiyero: 1-3mm / h, crystal rotation speed 8-12rpm;
- Temperature gradient: Axial 30-50 ° C / cm, radial ≤10 ° C / cm;
- Kutonhodza nzira: Mvura-yakatonhodzwa mhangura base (tembiricha yemvura 20–25°C), top radiative cooling .
- .Kudzora Kusachena.
- .Segregation Effect: Kusachena kwakadai seFe, Ni (segregation coefficient <0.1) inoungana pamiganhu yezviyo;
- .Remelting Cycles: 3-5 kutenderera, yekupedzisira yakazara tsvina ≤0.1ppm.
- .Zvekungwaririra:
- Ivhara nzvimbo yakanyunguduka nema graphite mahwendefa kudzvinyirira Te volatilization (kurasikirwa kwehuwandu ≤0.5%);
- Monitor crystal dhayamita munguva chaiyo uchishandisa laser geji (kurongeka ± 0.1mm);
- Dzivisa kushanduka kwetembiricha> ± 2 ° C kudzivirira dislocation density kuwedzera (chinangwa ≤10³/cm²) .
IV. Kuongorora Kwemhando uye Makiyi Metrics
Test Item | Standard Value | Test Method | Kwakabva |
.Kuchena. | ≥99.99999% (7N) | ICP-MS | |
.Total Metallic Impurities. | ≤0.1ppm | GD-MS (Glow Discharge Mass Spectrometry) | |
.Oxygen Content. | ≤5ppm | Inert Gasi Fusion-IR Absorption | |
.Crystal Kuvimbika. | Dislocation Density ≤10³/cm² | X-ray Topography | |
.Resistivity (300K). | 0.1–0.3Ω·cm | Four-Probe Method |
V. Environmental and Safety Protocols
- .Exhaust Gasi Kurapa:
- Kupisa kunopera: Neutralize SO₂ uye SeO₂ neNaOH scrubbers (pH≥10);
- Vacuum distillation exhaust: Condense uye dzorera Te vapor; yasara magasi adsorbed via activated kabhoni.
- .Slag Recycling:
- Anode slime (ine Ag, Au): Dzorera kuburikidza nehydrometallurgy (H₂SO₄-HCl system);
- Electrolysis residues (ine Pb, Cu): Dzokera kune copper smelting systems.
- .Matanho Okuchengetedza:
- Vashandi vanofanira kupfeka masiki egasi (Te vapor ine chepfu); chengetedza mhepo isina kunaka yemhepo (air exchange rate ≥10 cycles / h) .
Maitiro Ekugadzirisa Mazano
- .Raw Material Adaptation: Gadzirisa tembiricha yekugocha uye acid reshiyo zvine simba zvichibva pane anode slime masosi (semuenzaniso, mhangura vs. lead smelting);
- .Crystal Dhonza Rate Matching: Gadzirisa kumhanya kwekudhonza zvinoenderana nekunyunguduka kunyunguduka (nhamba yeReynolds Re≥2000) kudzvanyirira kutonhora kwebumbiro;
- .Kushanda Kwesimba: Shandisa dual-temperature zone kudziyisa (main zone 500°C, sub-zone 400°C) kuderedza mashandisirwo emagetsi egraphite ne30%.
Nguva yekutumira: Mar-24-2025