I-Selenium, njengento ebalulekileyo ye-semiconductor kunye ne-industrial raw material, inomsebenzi wayo ochaphazelekayo ngokuthe ngqo kukucoceka kwayo. Ngexesha lenkqubo yokucoca i-vacuum distillation, ukungcola kwe-oksijini yenye yezinto eziphambili ezichaphazela ukucoceka kwe-selenium. Eli nqaku libonelela ngengxoxo ecacileyo yeendlela ezahlukeneyo kunye nobuchule bokunciphisa umxholo we-oxygen ngexesha lokucocwa kwe-selenium nge-vacuum distillation.

I. Ukunciphisa i-Oxygen Content kwi-Raw Material Pretreatment Stage

1. Ukucocwa kwangaphambili kweMpahla ekrwada

Iselenium ekrwada idla ngokuqulatha ubumdaka obahlukeneyo, kubandakanywa iioksidi. Ngaphambi kokungena kwi-vacuum distillation system, iindlela zokucoca iikhemikhali kufuneka zisetyenziswe ukususa ii-oxides ezingaphezulu. Izisombululo zokucoca ezisetyenziswa ngokuqhelekileyo ziquka:

• Nciphisa isisombululo se-hydrochloric acid (i-5-10% yoxinaniso): Unyibilikisa ngokufanelekileyo i-oxides ezifana ne-SeO₂
• I-Ethanol okanye i-acetone: Isetyenziselwa ukususa izinto ezingcolileyo eziphilayo
• Amanzi adiyiniweyo: Iirinse ezininzi zokususa iasidi eshiyekileyo

Emva kokucoca, ukomisa kufuneka kwenziwe phantsi kwegesi ye-inert (umzekelo, i-Ar okanye i-N₂) emoyeni ukukhusela i-oxidation kwakhona.

2. Unyango lwangaphambi kokuNcitshiswa kwezinto eziKhwezi

Ukunciphisa unyango lwemathiriyeli ekrwada phambi kokuba ivacuum distillation inokunciphisa kakhulu umxholo weoksijini:

• Ukunciphisa i-Hydrogen: Yazisa i-hydrogen ecocekileyo (ubunyulu ≥99.999%) kwi-200-300 ° C ukunciphisa i-SeO₂ kwi-elenium elemental
• Ukunciphisa i-Carbothermal: Hlanganisa i-selenium ekrwada kunye ne-carbon powder ephezulu kunye nobushushu ukuya kwi-400-500 ° C phantsi kwe-vacuum okanye i-inert emoyeni, ukukhuthaza ukusabela kwe-C + SeO₂ → Se + CO₂
• Ukunciphisa i-sulfide: Iigesi ezifana ne-H₂S zinokunciphisa i-selenium oxides kumaqondo aphantsi kakhulu.

II. Uyilo kunye nokuPhuculwa kokuSebenza kweNkqubo yeVacuum Distillation

1. Ukukhethwa kunye noLungiselelo lweNkqubo yeVacuum

Indawo enevacuum ephezulu ibalulekile ekunciphiseni umxholo weoksijini:

• Sebenzisa impompo yokusasaza + indibaniselwano yempompo yomatshini, enevacuum yokugqibela efikelela ubuncinane kwi-10⁻⁴ Pa.
• Inkqubo kufuneka ixhotyiswe ngomgibe obandayo ukukhusela umva-ukusasazwa komphunga weoyile
• Zonke iidibansi kufuneka zisebenzise izitywina zetsimbi ukuphepha ukuphuma kwegesi kwiitywina zerabha
• Isixokelelwano kufuneka singene kwi-bake-out degassing eyaneleyo (200-250 ° C, 12-24 iiyure)

2. Ulawulo oluchanekileyo loBushushu beDistillation kunye noxinzelelo

Eyona nkqubo yeparameter indibaniselwano:

• Ubushushu bedistillation: Ilawulwa phakathi koluhlu lwama-220-280°C (ngaphantsi kwendawo yokubila ye-selenium engama-685°C)
• Uxinzelelo lwenkqubo: Igcinwe phakathi kwe-1-10 Pa
• Izinga lokufudumala: 5-10 ° C / min ukunqanda ukuphuphuma kobundlobongela kunye nokungena
• Ubushushu bezowuni yokuxinana: Igcinwe ku-50-80°C ukuqinisekisa ukujiya kweselenium ngokupheleleyo

3. ITekhnoloji ye-Multi-Stage Distillation

I-distillation enamanqanaba amaninzi inokunciphisa ngokuqhubekayo umxholo we-oxygen:

• Inqanaba lokuqala: Idistillation erhabaxa ukususa uninzi lokungcola okuguquguqukayo
• Inqanaba lesibini: Ulawulo oluchanekileyo lobushushu ukuqokelela iqhezu eliphambili
• Inqanaba lesithathu: Ubushushu obuphantsi, ukucotha kwedistillation ukufumana imveliso yococeko oluphezulu
  Amaqondo obushushu obushushu obuhlukeneyo angasetyenziswa phakathi kwezigaba zokondezwana kwamaqhezu

III. Amanyathelo eNkqubo eNcedisayo

1. ITekhnoloji yoKhuseleko lweGesi ye-Inert

Nangona isebenza phantsi kwe-vacuum, ukuqaliswa okufanelekileyo kwegesi ye-inert ecocekileyo inceda ukunciphisa umxholo we-oksijini:

• Emva kokukhupha inkqubo, gcwalisa i-argon ephezulu yokucoca (ubunyulu ≥99.9995%) ukuya kwi-1000 Pa
• Sebenzisa ukhuseleko lokuhamba kwegesi oluguquguqukayo, ngokuqhubekayo ukwazisa inani elincinci le-argon (10-20 sccm)
• Faka izicoci zerhasi ezisebenza kakuhle kakhulu kwiindawo zokungena igesi ukususa intsalela yeoksijini kunye nokufuma

2. Ukongezwa kwe-Oxygen Scavengers

Ukongeza i-oxygen scavenger efanelekileyo kwizinto ezingasetyenziswanga kunokunciphisa ngokufanelekileyo umxholo we-oxygen:

• Intsimbi yeMagnesium: Ubudlelwane obunamandla beoksijini, yenze iMgO
• I-aluminium powder: Iyakwazi ukususa ioksijini kunye nesulfure ngaxeshanye
• Iintsimbi zomhlaba ezinqabileyo: Ezinje ngeY, La, njl., ezineziphumo ezibalaseleyo zokususa ioksijini
  Ubungakanani be-oxygen scavenger ngokuqhelekileyo yi-0.1-0.5 wt% yezinto eziluhlaza; Izixa ezigqithisileyo zinokuchaphazela ubunyulu be-selenium

3. ITekhnoloji yoHlulo olutyhidiweyo

Ukucoca i-selenium enyibilikisiweyo phambi kokucoca:

• Sebenzisa i-quartz okanye izihlungi ze-ceramic ezinobungakanani bepore ye-1-5 μm
• Lawula ubushushu bokucoca kwi-220-250 ° C
• Inokususa amasuntswana eoksidi eqinileyo
• Izihluzi kufuneka zisuswe ngaphambili phantsi kwevacuum ephezulu

IV. Emva koNyango kunye noGcino

1. Ukuqokelelwa kweMveliso kunye nokuPhathwa

• Umqokeleli we-condenser kufuneka aqulunqwe njengesakhiwo esichithwayo ukuze kube lula ukufumana izinto eziphathekayo kwindawo engenzi lutho
• I-selenium ingots eqokelelweyo kufuneka ifakwe kwibhokisi yeglavu ye-argon
• Ukucolwa komphezulu kunokwenziwa ukuba kuyimfuneko ukususa iileya zeoksidi ezinokubakho

2. Ulawulo lwemeko yoGcino

• Indawo yokugcina kufuneka igcinwe yomile (indawo yombethe ≤-60°C)
• Sebenzisa i-double-layer seal packaging ezaliswe yi-high-purity gas inert
• Ubushushu bokugcina obucetyiswayo bungaphantsi kwe20°C
• Kuphephe ukuvezwa kukukhanya ukuthintela ukusabela kwe-photocatalytic oxidation

V. Ulawulo loMgangatho kunye noVavanyo

1. ITekhnoloji yokuJonga kwi-Intanethi

• Faka abahlalutyi berhasi eshiyekileyo (RGA) ukujonga uxinzelelo oluyinxenye lweoksijini ngexesha langempela
• Sebenzisa i-oxygen sensors ukulawula umxholo we-oksijini kwiigesi ezikhuselayo
• Sebenzisa i-infrared spectroscopy ukuchonga incopho zeempawu zokufunxa kwiibhondi ze-Se-O

2. Uhlalutyo lweMveliso egqityiweyo

• Sebenzisa indlela yokufunxa i-inert gas fusion-infrared ukumisela umxholo weoksijini
• I-ion mass spectrometry (SIMS) yesibini ukuhlalutya ukuhanjiswa kwe-oxygen
• I-X-reyi ye-photoelectron spectroscopy (XPS) yokukhangela iimeko zeekhemikhali ezingaphezulu

Ngokusebenzisa amanyathelo abanzi achazwe ngasentla, umxholo we-oksijini unokulawulwa ngaphantsi kwe-1 ppm ngexesha lokucocwa kwe-vacuum distillation ye-selenium, ukuhlangabezana neemfuno zokusetyenziswa kwe-selenium ephezulu. Kwimveliso yangempela, iiparamitha zenkqubo kufuneka ziphuculwe ngokusekelwe kwiimeko zezixhobo kunye neemfuno zemveliso, kwaye inkqubo yokulawula umgangatho engqongqo kufuneka isekwe.