Isejade ti 6N (≥99.9999% ti nw) olekenka-ga-mimọ imi-ọjọ nilo distillation ọpọ-ipele, jin adsorption, ati olekenka-mimọ ase lati se imukuro wa kakiri awọn irin, Organic impurities, ati particulates. Ni isalẹ jẹ ilana iwọn ile-iṣẹ kan ti n ṣepọ distillation igbale, isọdi-iranlọwọ makirowefu, ati awọn imọ-ẹrọ itọju lẹhin pipe.
Emi. Itọju Ohun elo Aise ati Yiyọkuro Aimọ
1. Yiyan Ohun elo Raw ati Itọju
- oAwọn ibeere: Iwa mimọ imi imi-ọjọ akọkọ ≥99.9% (iwọn 3N), awọn idoti irin lapapọ ≤500 ppm, akoonu erogba Organic ≤0.1%.
- oMakirowefu-Iranlọwọ Yo:
Efin robi ti wa ni ilọsiwaju ni ẹrọ itanna makirowefu (igbohunsafẹfẹ 2.45 GHz, agbara 10–15 kW) ni 140–150°C. Yiyi dipole ti a fa makirowefu ṣe idaniloju yo ni kiakia lakoko ti o npa awọn idoti Organic (fun apẹẹrẹ, awọn agbo ogun tar). Akoko yo: 30-45 iṣẹju; ijinle ilaluja makirowefu: 10-15 cm - oDeionized Omi Fifọ:
Efin didà ti wa ni idapọ pẹlu omi ti a ti sọ diionized (resistivity ≥18 MΩ · cm) ni iwọn 1: 0.3 ni ipin ibi-iṣiro kan (120 ° C, titẹ igi 2) fun wakati 1 lati yọ awọn iyọ ti omi ti n yo kuro (fun apẹẹrẹ, ammonium sulfate, sodium chloride). Ipele olomi ti wa ni idinku ati tun lo fun awọn akoko 2–3 titi iṣe adaṣe ≤5 μS/cm.
2. Ipolowo Ipele Olona-pupọ ati Filtration
- oDiatomaceous Earth/ Mu erogba Adsorption ṣiṣẹ:
Ilẹ Diatomaceous (0.5–1%) ati erogba ti a mu ṣiṣẹ (0.2–0.5%) ni a fi kun sulfur didà labẹ aabo nitrogen (130 ° C, gbigbo wakati 2) lati ṣe adsorb awọn eka irin ati awọn ohun alumọni ti o ku. - oUltra-konge ase:
Asẹ-ipele meji nipa lilo awọn asẹ ti a ti sọ di titanium (iwọn pore 0.1 μm) ni ≤0.5 MPa titẹ eto. Nọmba awọn patikulu lẹhin-filtration: ≤10 patikulu/L (iwọn> 0.5 μm).
II. Ilana Distillation Igbale Olona Ipele
1. Distillation akọkọ (Yiyọ aiṣedeede Metal)
- oOhun elo: Giga-mimọ quartz distillation iwe pẹlu 316L irin alagbara, irin eleto packing (≥15 o tumq si farahan), igbale ≤1 kPa.
- oAwọn paramita isẹ:
- oIfunni iwọn otutu: 250-280 ° C (efin efin ni 444.6 ° C labẹ titẹ ibaramu; igbale dinku aaye gbigbọn si 260-300 ° C).
- oReflux Ratio5:1–8:1; ọwọn oke otutu iyipada ≤±0.5°C.
- oỌja: Ti di mimọ imi-ọjọ ≥99.99% (4N grade), lapapọ irin impurities (Fe, Cu, Ni) ≤1 ppm.
2. Distillation Molecular Secondary (Yiyọkuro Aimọ Egan)
- oOhun elo: Kukuru-ọna molikula distiller pẹlu 10-20 mm evaporation-condensation aafo, evaporation otutu 300-320 ° C, igbale ≤0.1 Pa.
- oIyapa aimọ:
Awọn Organic farabale kekere (fun apẹẹrẹ, thioethers, thiophene) ti wa ni vaporized ati gbejade, lakoko ti awọn idoti ti o ga-fun (fun apẹẹrẹ, polyaromatics) wa ninu awọn iṣẹku nitori awọn iyatọ ninu ọna ọfẹ molikula. - oỌja: Sulfur ti nw ≥99.999% (5N ite), erogba Organic ≤0.001%, aloku oṣuwọn <0.3%.
3. Iṣatunṣe Agbegbe Ile-ẹkọ giga (Ṣiṣe Iwa mimọ 6N)
- oOhun elo: Atunṣe agbegbe petele pẹlu iṣakoso iwọn otutu agbegbe pupọ (± 0.1 ° C), iyara irin-ajo agbegbe 1-3 mm / h.
- oIyapa:
Lilo awọn iye-iye ipinya (K=Csolid/CliquidK=Cti o lagbara /Comi), agbegbe 20–30 kọja awọn irin ifọkansi (As, Sb) ni opin ingot. Ik 10-15% ti imi-ọjọ imi-ọjọ jẹ asonu.
III. Itọju-lẹhin-itọju ati Ultra-Clean Forming
1. Isediwon Ipara-funfun-funfun
- oEteri/ Erogba Tetrachloride isediwon:
Sulfur ti wa ni adalu pẹlu chromatographic-ite ether (1: 0.5 iwọn didun ratio) labẹ ultrasonic iranlowo (40 kHz, 40 ° C) fun 30 iṣẹju lati yọ wa kakiri pola organics . - oImularada Imularada:
Adsorption sieve molikula ati distillation igbale dinku awọn iṣẹku olomi si ≤0.1 ppm.
2. Ultrafiltration ati Iyipada paṣipaarọ
- oPTFE Membrane Ultrafiltration:
Efin didà ti wa ni filtered nipasẹ awọn membran PTFE 0.02 μm ni 160-180 ° C ati ≤0.2 MPa titẹ. - oIon Exchange Resini:
Awọn resini chelating (fun apẹẹrẹ, Amberlite IRC-748) yọ awọn ions irin ipele ppb kuro (Cu²⁺, Fe³⁺) ni awọn iwọn sisan 1–2 BV/h.
3. Ayika Ultra-Mimọ
- oInert Gaasi Atomization:
Ninu yara mimọ ti Kilasi 10, imi-ọjọ didà jẹ atomized pẹlu nitrogen (titẹ 0.8-1.2 MPa) sinu awọn granules iyipo 0.5–1 mm (ọrinrin <0.001%). - oApoti igbale:
Ọja ikẹhin ti wa ni edidi igbale ni fiimu apapo aluminiomu labẹ ultra-pure argon (≥99.9999% mimọ) lati ṣe idiwọ ifoyina.
IV. Awọn paramita Ilana bọtini
Ipele Ilana | Ooru (°C) | Titẹ | Akoko / Iyara | Ohun elo mojuto |
Makirowefu Yo | 140–150 | Ibaramu | 30–45 iṣẹju | Makirowefu riakito |
Deionized Omi Fifọ | 120 | 2 igi | 1 wakati / ọmọ | Aruwo riakito |
Distillation molikula | 300–320 | ≤0.1 Paa | Tesiwaju | Kukuru-Path Molecular Distiller |
Agbegbe Refaini | 115–120 | Ibaramu | 1–3 mm / h | Petele Zone Refiner |
PTFE Ultrafiltration | 160–180 | ≤0.2 MPa | 1–2 m³/h sisan | Ajọ-iwọn otutu |
Nitrogen Atomization | 160–180 | 0.8–1.2 MPa | 0,5-1 mm granules | Atomization Tower |
V. Iṣakoso Didara ati Idanwo
- oItupalẹ Iwa Aimọ:
- oGD-MS (Glow Discharge Mass Spectrometry): Ṣe awari awọn irin ni ≤0.01 ppb.
- oTOC Oluyanju: Awọn iwọn erogba Organic ≤0.001 ppm.
- oPatiku Iwon Iṣakoso:
Diffraction lesa (Mastersizer 3000) ṣe idaniloju iyapa D50 ≤± 0.05 mm. - oDada Cleanliness:
XPS (X-ray Photoelectron Spectroscopy) jẹrisi sisanra ohun elo afẹfẹ ≤1 nm.
VI. Aabo ati Apẹrẹ Ayika
- oIdena bugbamu:
Awọn aṣawari ina infurarẹẹdi ati awọn ọna iṣan omi nitrogen ṣetọju awọn ipele atẹgun <3% - oIṣakoso itujade:
- oAwọn Gas Acid: Fifọ NaOH ipele meji (20% + 10%) yọ ≥99.9% H₂S/SO₂ kuro.
- oAwọn VOCs: Zeolite rotor + RTO (850°C) dinku hydrocarbons ti kii-methane si ≤10 mg/m³.
- oAtunlo Egbin:
Idinku iwọn otutu giga (1200 ° C) gba awọn irin pada; akoonu imi imi <0.1% .
VII. Awọn Metiriki Imọ-ọrọ-ọrọ
- oLilo Agbara: 800-1200 kWh itanna ati 2-3 toonu nya fun pupọ ti 6N sulfur.
- oSo eso: sulfur imularada ≥85%, aloku oṣuwọn <1.5%.
- oIye owo: Iye owo iṣelọpọ ~ 120,000-180,000 CNY / ton; owo oja 250,000–350,000 CNY/ton (semikondokito ite) .
Ilana yii ṣe agbejade imi-ọjọ 6N fun awọn oluyaworan semikondokito, awọn sobusitireti idapọmọra III-V, ati awọn ohun elo ilọsiwaju miiran. Abojuto akoko gidi (fun apẹẹrẹ, itupalẹ ipilẹ LIBS) ati isọdiwọn yara mimọ ISO Kilasi 1 ṣe idaniloju didara ibamu.
Awọn akọsilẹ ẹsẹ
- Reference 2: Industrial Sulfur ìwẹnumọ Standards
- Itọkasi 3: Awọn Imọ-ẹrọ Filtration To ti ni ilọsiwaju ni Imọ-ẹrọ Kemikali
- Itọkasi 6: Iwe-itumọ Awọn Ohun elo Mimo-giga
- Itọkasi 8: Awọn Ilana iṣelọpọ Kemikali-Grade Semiconductor
- Reference 5: Igbale Distillation o dara ju
Akoko ifiweranṣẹ: Oṣu Kẹrin Ọjọ 02-2025