Kugadzirwa kwe6N (≥99.9999% kuchena) ultra-high-purity sulfur inoda multi-stage distillation, deep adsorption, uye ultra-clean filtration kubvisa trace metal, organic tsvina, uye zvikamu. Pazasi pane maindasitiri-mwero maitiro ekubatanidza vacuum distillation, microwave-inobatsira kucheneswa, uye chaiyo mushure mekurapa tekinoroji.
I. Raw Material Pretreatment uye Kubvisa Kusachena
1. Raw Material Sarudzo uye Pretreatment
- ,Zvinodiwa: Yekutanga sarufa kuchena ≥99.9% (3N giredhi), yakazara simbi tsvina ≤500 ppm, organic kabhoni yemukati ≤0.1%.
- ,Microwave-Inobatsira Kunyungudika:
Crude sulfur inogadziriswa mumicrowave reactor (2.45 GHz frequency, 10–15 kW simba) pa140–150°C. Microwave-induced dipole rotation inova nechokwadi chekunyunguduka nekukurumidza ichiora organic tsvina (semuenzaniso, tar makomisheni). Nguva yekunyunguduka: 30-45 maminitsi; microwave kupinda kudzika: 10-15 cm - ,Deionized Water Washing:
Sarufa yakanyungudutswa inosanganiswa nemvura yakasvibiswa (resistivity ≥18 MΩ · cm) pa 1: 0.3 mass ratio mune yakamutswa reactor (120 ° C, 2 bar pressure) kweawa imwe kubvisa munyu unonyungudika mumvura (semuenzaniso, ammonium sulfate, sodium chloride). The aqueous phase is decanted and used again for 2-3 cycles kusvika conductivity ≤5 μS/cm.
2. Multi-Stage Adsorption uye Filtration
- ,Diatomaceous Earth/Activated Carbon Adsorption:
Diatomaceous Earth (0.5-1%) uye activated kabhoni (0.2-0.5%) inowedzerwa kune yakanyungudutswa sarufa pasi pe nitrogen kuchengetedzwa (130 ° C, 2-awa inomutsa) kushambadza simbi yakaoma uye yakasara organics. - ,Ultra-Precision Sefa:
Kusefa kwematanho maviri uchishandisa titanium sintered filters (0.1 μm pore size) pa ≤0.5 MPa system pressure. Post-filtration particulate count: ≤10 particles / L (saizi> 0.5 μm).
II. Multi-Stage Vacuum Distillation Maitiro
1. Primary Distillation (Metal Impurity Removal).
- ,Equipment: Yakakwirira-kuchena quartz distillation column ine 316L Stainless simbi yakarongeka yakarongedza (≥15 theoretical plates), vacuum ≤1 kPa.
- ,Operational Parameters:
- ,Feed Temperature: 250–280°C (sarufa inofashaira pa444.6°C pasi pekumanikidzwa kwe ambient; vacuum inoderedza kufashaira kusvika pa260–300°C).
- ,Reflux Ratio: 5:1–8:1; mbiru yepamusoro tembiricha kuchinja ≤±0.5°C.
- ,Product: Kuchena kwesarufa yakanyungudutswa ≥99.99% (giredhi re4N), tsvina yese yesimbi (Fe, Cu, Ni) ≤1 ppm.
2. Secondary Molecular Distillation (Organic Impurity Removal).
- ,Equipment: Short-path molecular distiller ine 10–20 mm evaporation-condensation gap, evaporation tembiricha 300–320°C, vacuum ≤0.1 Pa.
- ,Kuparadzana Kusina Kuchena:
Low-boiling organics (semuenzaniso, thioethers, thiophene) inonyungudika uye inobviswa, nepo kusvibiswa kwepamusoro-kubikira (semuenzaniso, polyaromatics) kunoramba kuri mumasara nekuda kwekusiyana kwema molecular free path. - ,Product: Sulfur kuchena ≥99.999% (5N giredhi), organic kabhoni ≤0.001%, residue mwero <0.3%.
3. Kukwenenzvera kwenzvimbo yepamusoro (Kuwana Kuchena kwe6N).
- ,Equipment: Horizontal zone refiner ine multi-zone tembiricha control (±0.1°C), zone yekufamba kumhanya 1–3 mm/h.
- ,Kusarurana:
Kushandisa segregation coefficients (K=Csolid/CliquidK=Cyakasimba/Cliquid), 20-30 zone inopfuura concentrate simbi (As, Sb) kumagumo ingot. Iyo yekupedzisira 10-15% ye sulfur ingot inoraswa.
III. Post-Kurapwa uye Ultra-Yakachena Kugadzira
1. Ultra-Yakachena Solvent Extraction
- ,Ether/Carbon Tetrachloride Extraction:
Sulfur inosanganiswa ne chromatographic-grade ether (1: 0.5 volume ratio) pasi pe ultrasonic rubatsiro (40 kHz, 40 ° C) kwemaminitsi makumi matatu kubvisa trace polar organics. - ,Solvent Recovery:
Molecular sieve adsorption uye vacuum distillation inoderedza masara esolvent kusvika ≤0.1 ppm.
2. Ultrafiltration uye Ion Exchange
- ,PTFE Membrane Ultrafiltration:
Sarufa yakanyungudutswa inosefa kuburikidza ne0.02 μm PTFE membranes pa 160-180 ° C uye ≤0.2 MPa pressure. - ,Ion Exchange Resins:
Chelating resins (semuenzaniso, Amberlite IRC-748) bvisa ppb-level metal ions (Cu²⁺, Fe³⁺) pa1–2 BV/h kuyerera kwemazinga.
3. Ultra-Yakachena Nzvimbo Kugadzira
- ,Inert Gasi Atomization:
Mukirasi yegumi yekuchenesa imba, sarufa yakanyungudutswa yakanyungudutswa ine nitrogen (0.8–1.2 MPa pressure) kuita 0.5–1 mm spherical granules (unyoro <0.001%). - ,Vacuum Packaging:
Chigadzirwa chekupedzisira ndeye vacuum-yakavharwa mualuminium composite firimu pasi pe Ultra-pure argon (≥99.9999% kuchena) kudzivirira oxidation.
IV. Key Process Parameters
Process Stage | Tembiricha (°C). | Pressure | Nguva/Kumhanya | Core Equipment |
Microwave Melting | 140–150 | Ambient | 30–45 min | Microwave Reactor |
Deionized Water Washing | 120 | 2 bha | 1 awa/kutenderera | Stirred Reactor |
Molecular Distillation | 300–320 | ≤0.1 Pa | Continuous | Pfupi-Path Molecular Distiller |
Zone Refining | 115–120 | Ambient | 1–3 mm/h | Horizontal Zone Refiner |
PTFE Ultrafiltration | 160–180 | ≤0.2 MPa | 1–2 m³/h kuyerera | High-Temperature Sefa |
Nitrogen Atomization | 160–180 | 0.8–1.2 MPa | 0.5-1 mamirimita granules | Atomization Tower |
V. Kudzora Hunhu uye Kuedzwa
- ,Trace Impurity Analysis:
- ,GD-MS (Glow Discharge Mass Spectrometry): Inoona simbi pa ≤0.01 ppb.
- ,TOC Analyzer: Inoyera organic kabhoni ≤0.001 ppm.
- ,Particle Saizi Kudzora:
Laser diffraction (Mastersizer 3000) inovimbisa D50 kutsauka ≤± 0.05 mm. - ,Kuchena Kwepamusoro:
XPS (X-ray Photoelectron Spectroscopy) inosimbisa pamusoro peokisidhi ukobvu ≤1 nm.
VI. Chengetedzo uye Magadzirirwo Ezvakatipoteredza
- ,Kudzivirira Kuputika:
Infrared flame detectors uye nitrogen mafashama masisitimu anochengetedza mazinga eokisijeni <3% - ,Emission Control:
- ,Acid magasi: Kukwesha kweNaOH kwematanho maviri (20% + 10%) kunobvisa ≥99.9% H₂S/SO₂.
- ,VOCs: Zeolite rotor + RTO (850°C) inoderedza asiri-methane hydrocarbons kusvika ≤10 mg/m³.
- ,Waste Recycling:
Kuderedza kupisa kwepamusoro (1200 ° C) kunodzorera simbi; zvakasara zvesarufa zvinyorwa <0.1%.
VII. Techno-Economic Metrics
- ,Kushandiswa Kwemagetsi: 800–1200 kWh magetsi uye matani 2–3 chiutsi patani ye6N salfur.
- ,Yield: Sulfur kupora ≥85%, residue rate <1.5%.
- ,Mutengo: Mutengo wekugadzira ~120,000–180,000 CNY/ton; mutengo wemusika 250,000–350,000 CNY/ton (semiconductor giredhi) .
Iyi nzira inogadzira 6N sarufa ye semiconductor photoresists, III-V kommoni substrates, uye mamwe maapplication epamberi. Chaiyo-nguva yekutarisa (semuenzaniso, LIBS yekutanga ongororo) uye ISO Kirasi 1 yekuchenesa mukamuri calibration inovimbisa kuenderana mhando.
Mashoko omuzasi
- Reference 2: Industrial Sulfur Purification Standards
- Reference 3: Yepamberi Filtration Techniques mu Chemical Engineering
- Reference 6: High-Purity Materials Processing Handbook
- Reference 8: Semiconductor-Giredhi Chemical Production Protocols
- Reference 5: Vacuum Distillation Optimization
Nguva yekutumira: Kubvumbi-02-2025