6N Ultra-Yakakwirira-Kuchena Sulfur Distillation uye Kucheneswa Maitiro ane Detailed Parameters

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6N Ultra-Yakakwirira-Kuchena Sulfur Distillation uye Kucheneswa Maitiro ane Detailed Parameters

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

  1. ,Trace Impurity Analysis:
  • ,GD-MS (Glow Discharge Mass Spectrometry): Inoona simbi pa ≤0.01 ppb.
  • ,TOC Analyzer: Inoyera organic kabhoni ≤0.001 ppm.
  1. ,Particle Saizi Kudzora:
    Laser diffraction (Mastersizer 3000) inovimbisa D50 kutsauka ≤± 0.05 mm.
  2. ,Kuchena Kwepamusoro:
    XPS (X-ray Photoelectron Spectroscopy) inosimbisa pamusoro peokisidhi ukobvu ≤1 nm.

VI. Chengetedzo uye Magadzirirwo Ezvakatipoteredza

  1. ,Kudzivirira Kuputika:
    Infrared flame detectors uye nitrogen mafashama masisitimu anochengetedza mazinga eokisijeni <3%
  2. ,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.
  1. ,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

  1. Reference 2: Industrial Sulfur Purification Standards
  2. Reference 3: Yepamberi Filtration Techniques mu Chemical Engineering
  3. Reference 6: High-Purity Materials Processing Handbook
  4. Reference 8: Semiconductor-Giredhi Chemical Production Protocols
  5. Reference 5: Vacuum Distillation Optimization

Nguva yekutumira: Kubvumbi-02-2025