6N Ultra-High-Purity Sulfur Distillation thiab purification txheej txheem nrog cov ncauj lus kom ntxaws

Kev tsim tawm ntawm 6N (≥99.9999% purity) ultra-high-purity sulfur yuav tsum muaj ntau theem distillation, sib sib zog nqus adsorption, thiab ultra-ntxuav pom kom tshem tawm cov kab hlau, organic impurities, thiab particulates. Hauv qab no yog cov txheej txheem kev lag luam ua ke nrog lub tshuab nqus tsev distillation, microwave-pab purification, thiab precision tom qab kho technologies.

Kuv. Raw Material Pretreatment thiab Impurity Tshem Tawm

1. Raw Material Selection thiab Pretreatment

• covKev xav tauInitial sulfur purity ≥99.9% (3N qib), tag nrho hlau impurities ≤500 ppm, organic carbon ntsiab lus ≤0.1%.
• covMicrowave-Assisted Melting:
  Crude sulfur yog ua tiav nyob rau hauv lub microwave reactor (2.45 GHz zaus, 10-15 kW zog) ntawm 140-150 ° C. Microwave-induced dipole rotation xyuas kom ceev melting thaum decomposing organic impurities (xws li, tar compounds). Lub sij hawm melting: 30-45 feeb; microwave qhov tob: 10-15 cm
• covDeionized dej ntxuav:
  Molten sulfur yog tov nrog dej deionized (resistivity ≥18 MΩ·cm) ntawm 1:0.3 huab hwm coj piv nyob rau hauv ib tug stirred reactor (120 ° C, 2 bar siab) rau 1 teev kom tshem tawm cov dej-soluble ntsev (xws li ammonium sulfate, sodium chloride). Theem aqueous yog decanted thiab rov siv dua rau 2-3 cycles kom txog thaum conductivity ≤5 μS / cm.

2. Multi-Stage Adsorption thiab Lim

• covDiatomaceous Earth / Activated Carbon Adsorption:
  Diatomaceous ntiaj teb (0.5-1%) thiab activated carbon (0.2-0.5%) yog ntxiv rau molten sulfur nyob rau hauv kev tiv thaiv nitrogen (130 ° C, 2-teev stirring) rau adsorb hlau complexes thiab residual organics
• covUltra-Precision Lim:
  Ob-theem pom siv titanium sintered lim (0.1 μm pore loj) ntawm ≤0.5 MPa system siab. Post-filtration particulate suav: ≤10 particles/L (loj> 0.5 μm).

II. Multi-Stage Nqus Distillation Txheej txheem

1. Primary Distillation (Metal Impurity Tshem Tawm).

• covKhoom siv: High-purity quartz distillation kem nrog 316L stainless hlau qauv ntim (≥15 theoretical daim hlau), lub tshuab nqus tsev ≤1 kPa.
• covKev khiav hauj lwm Parameters:
• covPub kub: 250-280 ° C (sulfur boils ntawm 444.6 ° C nyob rau hauv ambient siab; lub nqus tsev vacuum txo boiling point rau 260-300 ° C).
• covReflux Ratio: 5:1–8:1; Sab saum toj kub hloov pauv ≤ ± 0.5 ° C.
• covKhoom: Condensed sulfur purity ≥99.99% (qib 4N), tag nrho cov hlau impurities (Fe, Cu, Ni) ≤1 ppm.

2. Secondary Molecular Distillation (Organic Impurity Tshem Tawm).

• covKhoom siv: Short-path molecular distiller nrog 10-20 mm evaporation-condensation kis, evaporation kub 300-320 ° C, nqus ≤0.1 Pa.
• covKev sib cais impurity:
  Tsawg-boiling organics (piv txwv li, thioethers, thiophene) yog vaporized thiab evacuated, thaum high-boiling impurities (piv txwv li, polyaromatics) tseem nyob rau hauv residues vim qhov sib txawv ntawm molecular dawb txoj kev.
• covKhoom: Sulfur purity ≥99.999% (5N qib), organic carbon ≤0.001%, residue tus nqi <0.3%.

3. Tertiary Zone Refining (Ua tiav 6N Purity).

• covKhoom siv: Kab rov tav refiner nrog ntau cheeb tsam kub tswj (± 0.1 ° C), cheeb tsam mus ncig ceev 1-3 mm / h.
• covKev cais:
  Siv cov coefficients sib cais (K = Csolid/CliquidK=Ckhoom /Ckua), 20-30 cheeb tsam dhau cov concentrates hlau (As, Sb) ntawm qhov kawg ingot. Qhov kawg 10-15% ntawm sulfur ingot yog muab pov tseg.

III ib. Tom qab Kev Kho Mob thiab Ultra-Clean Forming

1. Ultra-Ntshiab Solvent Extraction

• covEther / Carbon Tetrachloride Extraction:
  Sulfur yog tov nrog chromatographic-qib ether (1: 0.5 ntim piv) nyob rau hauv kev pab ultrasonic (40 kHz, 40 ° C) rau 30 feeb kom tshem tawm cov kab polar organics.
• covSolvent Recovery:
  Molecular sieve adsorption thiab nqus distillation txo cov kuab tshuaj residues rau ≤0.1 ppm.

2. Ultrafiltration thiab Ion Exchange

• covTom ntej: PTFE Membrane Ultrafiltration:
  Molten sulfur yog lim los ntawm 0.02 μm PTFE membranes ntawm 160-180 ° C thiab ≤0.2 MPa siab.
• covIon txauv Resins:
  Chelating resins (piv txwv li, Amberlite IRC-748) tshem tawm ppb-theem hlau ions (Cu²⁺, Fe³⁺) ntawm 1-2 BV / h txaus tus nqi.

3. Ultra-Clean Ib puag ncig tsim

• covInert Gas Atomization:
  Hauv Chav Kawm 10, molten sulfur yog atomized nrog nitrogen (0.8-1.2 MPa siab) rau hauv 0.5-1 mm spherical granules (puab <0.001%).
• covNqus Ntim:
  Cov khoom kawg yog lub tshuab nqus tsev kaw nyob rau hauv aluminium composite zaj duab xis nyob rau hauv ultra-ntshiab argon (≥99.9999% purity) los tiv thaiv oxidation.

IV. Cov Txheej Txheem Tseem Ceeb

V. Kev Tswj Xyuas Zoo thiab Kev Xeem

1. covTrace Impurity Analysis:

• covGD-MS (Glow Discharge Mass Spectrometry): Pom cov hlau ntawm ≤0.01 ppb.
• covTOC Analyzer: Ntsuas cov organic carbon ≤0.001 ppm.

1. covParticle Loj Tswj:
   Laser diffraction (Mastersizer 3000) kom D50 sib txawv ≤ ± 0.05 hli.
2. covNto huv huv:
   XPS (X-ray Photoelectron Spectroscopy) lees paub qhov chaw oxide thickness ≤1 nm.

VI. Kev Nyab Xeeb thiab Environmental Design

1. covTiv thaiv tawg:
   Infrared nplaim taws detectors thiab nitrogen dej nyab system tswj cov pa oxygen <3%
2. covEmission tswj:

• covAcid Gases: Ob-theem NaOH txhuam (20% + 10%) tshem tawm ≥99.9% H₂S/SO₂.
• covVOCs: Zeolite rotor + RTO (850 ° C) txo cov non-methane hydrocarbons rau ≤10 mg / m³.

1. covPov tseg Recycling:
   Kev kub siab txo (1200 ° C) rov ua cov hlau; residue sulfur cov ntsiab lus <0.1%.

VII. Techno-Economic Metrics

• covKev siv hluav taws xob: 800-1200 kWh hluav taws xob thiab 2-3 tons chav rau ib tuj ntawm 6N sulfur.
• covYield: Sulfur rov ≥85%, residue tus nqi <1.5%.
• covNqi: Tus nqi tsim khoom ~ 120,000-180,000 CNY / tuj; tus nqi lag luam 250,000-350,000 CNY / tuj (qib semiconductor).

Cov txheej txheem no tsim 6N sulfur rau semiconductor photoresists, III-V compound substrates, thiab lwm yam kev siv siab heev. Kev saib xyuas lub sijhawm tiag tiag (piv txwv li, LIBS lub ntsiab lus tsom xam) thiab ISO Class 1 cleanroom calibration kom zoo ib yam.

Cov ntawv hauv qab

1. Siv 2: Muaj Sulfur Purification Standards
2. Reference 3: Advanced Filtration Techniques in Chemical Engineering
3. Siv 6: Phau Ntawv Qhia Ua Cov Khoom Siv Siab Purity
4. Siv 8: Semiconductor-Grade Chemical Production Protocols
5. Siv 5: Nqus Distillation Optimization