I-6N Ultra-High-Purity Sulfur Disstillation and Purification Process with Detailed Parameters

Ukukhiqizwa kwe-6N (≥99.9999% ubumsulwa) i-ultra-high-purity sulfur kudinga ukukhishwa kwe-multi-stage, i-adsorption ejulile, nokuhlunga okuhlanzekile kakhulu ukuze kuqedwe izinsimbi zokulandelela, ukungcola okuphilayo, nezinhlayiya. Ngezansi kunenqubo yesikali sezimboni ehlanganisa i-vacuum distillation, ukuhlanzwa okusizwa yi-microwave, kanye nobuchwepheshe obunembayo bangemva kokwelashwa.

I. Ukulungiswa Kwezinto Ezingavuthiwe kanye Nokususwa Kokungcola

1. Ukukhethwa Kwezinto Ezingavuthiwe kanye Nokwelashwa Ngaphambili

• .Izimfuneko‌: Ukuhlanzeka kwesibabule sokuqala ≥99.9% (ibanga le-3N), ukungcola okuphelele kwensimbi ≤500 ppm, okuqukethwe kwekhabhoni ephilayo ≤0.1%.
• .Ukuncibilika Okusizwa Nge-microwave:
  Isibabule esingahluziwe sicutshungulwa ku-reactor ye-microwave (imvamisa engu-2.45 GHz, amandla angu-10–15 kW) ku-140–150°C. Ukujikeleza kwe-dipole eyenziwe nge-Microwave kuqinisekisa ukuncibilika ngokushesha ngenkathi kubola ukungcola okuphilayo (isb., izinhlanganisela zetiyela). Isikhathi sokuncibilika: imizuzu engama-30-45; ukujula kwe-microwave: 10-15 cm
• .Ukugeza Amanzi Okuyi-Deionized:
  Isibabule esincibilikisiwe sixutshwa namanzi akhishwe yi-deionized (ukumelana ≥18 MΩ·cm) ku-1:0.3 mass ratio kureactor enyakaziswayo (120°C, 2 bar pressure) ihora elingu-1 ukuze kukhishwe usawoti oncibilikayo emanzini (isb, ammonium sulfate, sodium chloride). Isigaba se-aqueous sinqanyuliwe futhi siphinde sisetshenziswe emijikelezweni engu-2-3 kuze kube yilapho conductivity ≤5 μS/cm.

2. I-Multi-Stage Adsorption kanye Nokuhlunga

• .I-Diatomaceous Earth/I-activated Carbon Adsorption:
  I-Diatomaceous Earth (0.5-1%) kanye nekhabhoni ecushiwe (0.2–0.5%) yengezwa esibabuleni esincibilikisiwe ngaphansi kokuvikelwa kwe-nitrogen (130°C, ukunyakaziswa kwamahora ama-2) ukuze kukhangiswe izakhi zensimbi nezinto eziphilayo ezisele.
• .Ukuhlunga Okunembe Kakhulu:
  Ukuhlunga okunezigaba ezimbili kusetshenziswa izihlungi ze-titanium sintered (usayizi wembotshana ongu-0.1 μm) kungcindezi yesistimu engu-≤0.5 MPa. Isibalo sezinhlayiya zangemuva kokuhlunga: ≤10 izinhlayiya/L (usayizi >0.5 μm).

II. Inqubo ye-Multi-Stage Vacuum Distillation

1. I-Distillation Eyisisekelo (Ukususwa Kokungcola Kwensimbi).

• .Izisetshenziswa: Ikholomu yokuhlanza i-quartz ehlanzekile kakhulu enensimbi engagqwali engu-316L yokupakishwa okuhlelekile (≥15 amapuleti etiory), vacuum ≤1 kPa .
• .Amapharamitha Okusebenza:
• .Ithempelesha Yokuphakelayo: 250–280°C (isulfure ibilisa ku-444.6°C ngaphansi kwengcindezi ye-ambient; vacuum yehlisa indawo yokubila ibe ngu-260–300°C).
• .Isilinganiso se-Reflux: 5:1–8:1; ukushintshashintsha kwezinga lokushisa kwekholomu ≤±0.5°C.
• .Umkhiqizo: Ukuhlanzeka kwesibabule esijikisiwe ≥99.99% (ibanga le-4N), ukungcola okuphelele kwensimbi (Fe, Cu, Ni) ≤1 ppm.

2. I-Distillation Yengqamuzana Yesibili (Ukususwa Kokungcola Kwezinto Eziphilayo).

• .Izisetshenziswa: I-distiller ye-molecular yendlela emfushane enegebe le-evaporation-condensation elingu-10-20 mm, izinga lokushisa lokuhwamuka 300-320°C, vacuum ≤0.1 Pa.
• .Ukuhlukana Kokungcola:
  Izinto eziphilayo ezibilisa kancane (isb., ama-thioethers, i-thiophene) ziyahwamuka futhi ziyakhishwa, kuyilapho ukungcola okubilayo kakhulu (isb., i-polyaromatics) kusala kuzinsalela ngenxa yomehluko wendlela yamahhala yamangqamuzana.
• .Umkhiqizo: Ukuhlanzeka kwesibabule ≥99.999% (ibanga le-5N), ikhabhoni ephilayo ≤0.001%, izinga lensalela <0.3%.

3. Ukucwengisiswa Kwendawo Ephakeme (Ukuzuza Ukuhlanzeka kwe-6N).

• .Izisetshenziswa: Isicwengisisi sendawo evundlile nesilawula izinga lokushisa ezindaweni eziningi (±0.1°C), isivinini sohambo lwezoni 1–3 mm/h.
• .Ukuhlukaniswa:
  Kusetshenziswa ama-coefficients okuhlukanisa (K=Csolid/CliquidK=Cokuqinile/Cliquid), 20-30 zone kudlula concentrate metals (As, Sb) ekugcineni ingot. I-10-15% yokugcina ye-sulfur ingot iyalahlwa.

III. Ngemuva Kokwelashwa kanye Nokwakheka Okuhlanzekile Kakhulu

1. I-Ultra-Pure Solvent Extraction

• .I-Ether/Carbon Tetrachloride Extraction:
  Isibabule sixutshwe ne-ether ye-chromatographic-grade (1:0.5 volume ratio) ngaphansi kosizo lwe-ultrasonic (40 kHz, 40°C) imizuzu engu-30 ukuze kukhishwe umkhondo wezinto eziphilayo ezipholile.
• .Ukubuyisela I-Solvent:
  I-adsorption ye-molecular sieve kanye ne-vacuum distillation kunciphisa izinsalela ze-solvent ibe ngu-≤0.1 ppm.

2. I-Ultrafiltration kanye ne-Ion Exchange

• .I-PTFE Membrane Ultrafiltration:
  Isibabule esincibilikisiwe sihlungwa ngolwelwesi lwe-PTFE lwe-0.02 μm ku-160–180°C kanye nomfutho we-≤0.2 MPa.
• .I-Ion Exchange Resins:
  Ama-resin acwebileyo (isb, i-Amberlite IRC-748) asusa ama-ion ensimbi eleveli ye-ppb (Cu²⁺, Fe³⁺) ngamanani okugeleza angu-1–2 BV/h.

3. Ukwakhiwa Kwendawo Ehlanzekile Kakhulu

• .Inert Gas Atomization:
  Egumbini lokuhlanza le-Class 10, isibabule esincibilikisiwe sine-athomu ye-nitrogen (0.8–1.2 MPa pressure) ibe yizinhlayiyana eziyindilinga ezingu-0.5–1 mm (umswakama <0.001%).
• .Vacuum Packaging:
  Umkhiqizo wokugcina uvalwe nge-vacuum-sealed kufilimu eyinhlanganisela ye-aluminium ngaphansi kwe-ultra-pure argon (≥99.9999% ubumsulwa) ukuze kuvinjelwe i-oxidation.

IV. Amapharamitha wenqubo engukhiye

V. Ukulawula Ikhwalithi Nokuhlola

1. .Ukuhlaziya Ukungcola Kokulandelela:

• .I-GD-MS (Glow Discharge Mass Spectrometry): Ithola izinsimbi kokuthi ≤0.01 ppb.
• .I-TOC Analyzer: Ikala i-organic carbon ≤0.001 ppm.

1. .Ukulawula Usayizi Wezinhlayiyana:
   I-laser diffraction (Mastersizer 3000) iqinisekisa ukuchezuka kwe-D50 ≤±0.05 mm.
2. .Ukuhlanzeka kwendawo:
   I-XPS (i-X-ray Photoelectron Spectroscopy) iqinisekisa ukujiya kwe-oxide engaphezulu ≤1 nm .

VI. Ukuphepha Nokuklanywa Kwemvelo

1. .Ukuvimbela Ukuqhuma:
   Izitholi ze-infrared flame kanye nezinhlelo zokukhukhula kwe-nitrogen zigcina amazinga e-oxygen <3%
2. .Ukulawula Ukukhipha Isisu:

• .Amagesi ane-Acid: Ukukhuhla kwe-NaOH kwezigaba ezimbili (20% + 10%) kususa ≥99.9% H₂S/SO₂.
• .Ama-VOC: Irotha ye-Zeolite + RTO (850°C) yehlisa ama-non-methane hydrocarbons ukuze afike ku-≤10 mg/m³ .

1. .Waste Recycling:
   Ukunciphisa izinga lokushisa eliphezulu (1200°C) kubuyisela izinsimbi; insalela yokuqukethwe kwesibabule <0.1%.

VII. I-Techno-Economic Metrics

• .Ukusetshenziswa kwamandla: 800–1200 kWh ugesi kanye namathani angu-2–3 ngesitimu ngethani le-6N sulphur.
• .Veza: Ukutholwa kwesibabule ≥85%, izinga lezinsalela <1.5%.
• .Izindleko: Izindleko zokukhiqiza ~120,000–180,000 CNY/ton; intengo yemakethe 250,000–350,000 CNY/ton (ibanga le-semiconductor) .

Le nqubo ikhiqiza i-6N sulphur ye-semiconductor photoresist, i-III-V compound substrates, nezinye izinhlelo zokusebenza ezithuthukisiwe. Ukuqapha kwesikhathi sangempela (isb, ukuhlaziya okuyisisekelo kwe-LIBS) kanye nokulinganisa kwegumbi le-ISO Class 1 kuqinisekisa ikhwalithi engaguquki.

Imibhalo yaphansi

1. Ireferensi 2: Amazinga Okuhlanza Isibabule Sezimboni
2. Ireferensi 3: Amasu Okuhlunga Athuthukile Kunjiniyela Wamakhemikhali
3. Ireferensi 6: Ibhuku Lencwadi Yokucubungula Izinto Ezihlanzekile Kakhulu
4. Reference 8: I-Semiconductor-Grade Chemical Production Protocols
5. Ireferensi yesi-5: Ukwenziwa Kwe-Vacuum Distillation