6N Ultra-High-Purity Sulfur Distillation ndi Kuyeretsa Njira Yokhala ndi Zambiri Zatsatanetsatane

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6N Ultra-High-Purity Sulfur Distillation ndi Kuyeretsa Njira Yokhala ndi Zambiri Zatsatanetsatane

Kupanga kwa 6N (≥99.9999% kuyeretsedwa) sulfure yapamwamba kwambiri kumafuna distillation yamitundu yambiri, kutsekemera kwambiri, ndi kusefera koyera kwambiri kuti athetse zitsulo, zonyansa zamoyo, ndi ma particulates. Pansipa pali njira yamafakitale yophatikizira kupukutira kwa vacuum, kuyeretsa mothandizidwa ndi ma microwave, komanso matekinoloje olondola pambuyo pochiritsa.


Ine. Kukonzekera Kwambiri Kwazinthu Zopangira ndi Kuchotsa Chidetso

1. Kusankhidwa Kwazinthu Zopangira ndi Kukonzekeratu

  • paZofunikira: Kuyeretsedwa kwa sulfure koyamba ≥99.9% (kalasi ya 3N), zonyansa zonse zachitsulo ≤500 ppm, organic carbon content ≤0.1%.
  • paKusungunuka Mothandizidwa ndi Microwave:
    Sulfure wosakhwima amakonzedwa mu microwave reactor (2.45 GHz pafupipafupi, 10-15 kW mphamvu) pa 140-150 ° C. Kuzungulira kwa dipole kopangidwa ndi ma Microwave kumatsimikizira kusungunuka mwachangu ndikuwola zonyansa zakuthupi (mwachitsanzo, mankhwala a tar). Nthawi yosungunuka: 30-45 mphindi; kuya kwa microwave: 10-15 cm
  • paKutsuka Kwamadzi Kwatsopano:
    Sulfure wosungunuka ndi wothira madzi deionized (resistivity ≥18 MΩ · cm) pa 1: 0.3 misa chiŵerengero mu analimbikitsa riyakitala (120 ° C, 2 bala kuthamanga) kwa 1 ora kuchotsa madzi sungunuka mchere (mwachitsanzo, ammonium sulfate, sodium kolorayidi). Gawo lamadzimadzi limachotsedwa ndipo limagwiritsidwanso ntchito kwa maulendo a 2-3 mpaka conductivity ≤5 μS / cm.

2. Multi-Stage Adsorption ndi kusefera

  • paDiatomaceous Earth/Activated Carbon Adsorption:
    Diatomaceous earth (0.5-1%) ndi activated carbon (0.2-0.5%) amawonjezedwa ku sulfure wosungunuka pansi pa chitetezo cha nayitrogeni (130 ° C, 2-hour stirring) kuti adsorbe zitsulo ndi zinthu zotsalira.
  • paKusefera kolondola kwambiri:
    Kusefera kwa magawo awiri pogwiritsa ntchito zosefera za titaniyamu (0.1 μm kukula kwa pore) pa ≤0.5 MPa system pressure. Kuwerengera kwa tinthu tating'ono tosefedwa: ≤10 particles/L (kukula> 0.5 μm).

II. Multi-Stage Vacuum Distillation process

1. Pulayimale Distillation (Metal Impurity Removal).

  • paZida: Mzere wa distillation wa quartz wapamwamba kwambiri wokhala ndi 316L zitsulo zosapanga dzimbiri zolongedza (≥15 mbale zamaphunziro), vacuum ≤1 kPa .
  • paMa Parameters Ogwira Ntchito:
  • paKutentha kwa chakudya250–280°C (sulfure amawira pa 444.6°C pansi pa kupanikizika kozungulira; vacuum imachepetsa kuwira kufika pa 260–300°C).
  • paReflux Ration: 5:1–8:1; kusinthasintha kwapamwamba kwa kutentha ≤± 0.5°C.
  • paZogulitsa: Kuyeretsedwa kwa sulfure ≥99.99% (kalasi ya 4N), zonyansa zonse zachitsulo (Fe, Cu, Ni) ≤1 ppm.

2. Sekondale Molecular Distillation (Organic Impurity Removal).

  • paZida: Njira yochepa ya molecular distiller yokhala ndi 10-20 mm evaporation-condensation gap, kutentha kwa evaporation 300-320 ° C, vacuum ≤0.1 Pa .
  • paKupatukana kwa Chidebe:
    Zinthu zomwe zimawotcha pang'ono (mwachitsanzo, thioethers, thiophene) zimatenthedwa ndikuchotsedwa, pomwe zonyansa zotentha kwambiri (mwachitsanzo, polyaromatics) zimakhalabe zotsalira chifukwa cha kusiyana kwa mamolekyulu opanda njira.
  • paZogulitsa: Sulfur purity ≥99.999% (5N grade), organic carbon ≤0.001%, mlingo wotsalira <0.3%.

3. Kukonza Zone Yapamwamba (Kukwaniritsa Chiyero cha 6N).

  • paZida: Woyengera zone wopingasa wokhala ndi kuwongolera kutentha kwa madera ambiri (± 0.1°C), liwiro la kuyenda madera 1–3 mm/h.
  • paKusiyanitsa:
    Kugwiritsa ntchito ma coefficients olekanitsa (K=Csolid/CliquidK=Ccholimba/Cliquid), 20-30 zone imadutsa zitsulo zokhazikika (As, Sb) kumapeto kwa ingot. 10-15% yomaliza ya sulfure ingot imatayidwa.

III. Pambuyo pa Chithandizo ndi Kupanga Koyera Kwambiri

1. Ultra-Pure Solvent Extraction

  • paEther/Carbon Tetrachloride Extraction:
    Sulfure ndi wothira chromatographic kalasi etere (1: 0.5 voliyumu chiŵerengero) pansi akupanga thandizo (40 kHz, 40°C) kwa mphindi 30 kuchotsa kufufuza polar organics .
  • paKubwezeretsanso Zosungunulira:
    Ma molecular sieve adsorption ndi vacuum distillation amachepetsa zotsalira za zosungunulira mpaka ≤0.1 ppm.

2. Ultrafiltration ndi Ion Exchange

  • paPTFE Membrane Ultrafiltration:
    Sulfure wosungunuka amasefedwa kudzera mu 0.02 μm PTFE nembanemba pa 160-180 ° C ndi ≤0.2 MPa kuthamanga.
  • paIon Kusinthana Resins:
    Chelating resins (mwachitsanzo, Amberlite IRC-748) amachotsa ma ppb-level zitsulo ma ions (Cu²⁺, Fe³⁺) pa 1–2 BV/h mitengo yotuluka.

3. Kupanga Malo Oyera Kwambiri

  • paInert Gasi Atomization:
    Mu chipinda choyera cha Class 10, sulfure yosungunuka imapangidwa ndi nayitrogeni (0.8-1.2 MPa pressure) kukhala 0.5-1 mm matumba ozungulira (chinyezi <0.001%).
  • paVacuum Packaging:
    Chogulitsa chomaliza chimakhala chosindikizidwa mu filimu yopangidwa ndi aluminiyamu pansi pa ultra-pure argon (≥99.9999% chiyero) kuteteza okosijeni.

IV. Key Process Parameters

Gawo la ndondomeko

Kutentha (°C).

Kupanikizika

Nthawi/Liwiro

Zida Zoyambira

Kusungunuka kwa Microwave

140-150

Wozungulira

30-45 min

Microwave Reactor

Kutsuka Kwamadzi Kwatsopano

120

2 bwalo

1 ola / kuzungulira

Wolimbikitsa Reactor

Molecular Distillation

300-320

≤0.1 Pa

Zopitilira

Short-Path Molecular Distiller

Zone Refining

115–120

Wozungulira

1-3 mm/h

Horizontal Zone Refiner

PTFE Ultrafiltration

160-180

≤0.2 MPa

1–2 m³/h kuyenda

Sefa Yotentha Kwambiri

Nitrogen Atomization

160-180

0.8-1.2 MPa

0.5-1 mm granules

Atomization Tower


V. Kuwongolera Ubwino ndi Kuyesa

  1. paTrace Imprity Analysis:
  • paGD-MS (Glow Discharge Mass Spectrometry): Imazindikira zitsulo pa ≤0.01 ppb.
  • paChithunzi cha TOC Analyzer: Imayezera kaboni organic ≤0.001 ppm.
  1. paParticle Size Control:
    Laser diffraction (Mastersizer 3000) imatsimikizira kupatuka kwa D50 ≤± 0.05 mm.
  2. paUkhondo Pamwamba:
    XPS (X-ray Photoelectron Spectroscopy) imatsimikizira makulidwe a okusayidi pamwamba ≤1 nm.

VI. Chitetezo ndi Mapangidwe Achilengedwe

  1. paKuteteza Kuphulika:
    Zowunikira moto wa infrared ndi makina osefukira a nayitrogeni amasunga milingo ya okosijeni <3%
  2. paEmission Control:
  • paMagesi a Acid: Kukolopa kwa magawo awiri a NaOH (20% + 10%) kumachotsa ≥99.9% H₂S/SO₂.
  • paVOCs: Zeolite rotor + RTO (850°C) amachepetsa ma hydrocarboni omwe si a methane kufika ≤10 mg/m³.
  1. paKubwezeretsanso Zinyalala:
    Kuchepetsa kutentha kwambiri (1200 ° C) kumabwezeretsanso zitsulo; zotsalira za sulfure <0.1%.

VII. Techno-Economic Metrics

  • paKugwiritsa Ntchito Mphamvu: magetsi 800–1200 kWh ndi matani 2–3 nthunzi pa toni ya 6N sulfure.
  • paZotuluka: Kuchira kwa sulfure ≥85%, mlingo wotsalira <1.5%.
  • paMtengo: Mtengo wopangira ~ 120,000–180,000 CNY/ton; mtengo wamsika 250,000–350,000 CNY/ton (kalasi ya semiconductor) .

Izi zimapanga sulfure ya 6N ya semiconductor photoresists, magawo apakati a III-V, ndi ntchito zina zapamwamba. Kuyang'anira nthawi yeniyeni (mwachitsanzo, kusanthula koyambira kwa LIBS) ndi kusanja kwa chipinda choyera cha ISO Class 1 kumatsimikizira kusasinthika.

Mawu a M'munsi

  1. Zolozera 2: Miyezo Yoyeretsa Sulfur Yamafakitale
  2. Buku la 3: Njira Zapamwamba Zosefera mu Chemical Engineering
  3. Buku la 6: Buku Lokonzekera Zinthu Zoyera Kwambiri
  4. Reference 8: Semiconductor-Grade Chemical Production Protocols
  5. Chidziwitso 5: Kukhathamiritsa kwa Vacuum Distillation

Nthawi yotumiza: Apr-02-2025