Abstract:i-acetone catalyzed chloride futhi ikhiqizwe yi-solvent crystallization ku-1,1,3-trichloroacetone enobumsulwa obuphakeme obungekho ngaphansi kuka-99.0%,nesivuno esingu-45%o Amagama angukhiye:1,1,3-trichloroacetone;ukuhlanganiswa;ukuhlanzeka okuphezulu
———-. Isandulelo
1,1,3■i-trichloroacetone iyingxenye ebalulekile emaphakathi ekukhiqizweni kwe-folic acid.Okwamanje,1,1,3.i-acetone trihloropacetone,umjikelezo omude wokukhiqiza(amahora angama-48),ukukhetha okubi,isivuno esiphansi,1,1,3- okuqukethwe kwe-trichloropacetone cishe ku-17% kuphela, ngemva kokukhipha amanzi, okuqukethwe kwakho kungu-51.9% kuphela.Futhi izindleko zokukhiqiza ziphezulu, ukulungiswa komkhiqizo kuphansi.Lokhu konke kuholela ezindlekweni eziphezulu zokukhiqiza i-folic acid yasekhaya, kunzima ukuthuthukisa okuqukethwe nokunye. izinkinga.Umbhali ufunde inqwaba yemibhalo yasekhaya neyangaphandle. Ngemuva kokuhlolwa okuningi nezifundo, sengeze i-catalyst kanye nesivinini sokulawula i-fou chlorine, sinciphisa isikhathi sokuphendula sibe yi-1,1,3-3 trichlorropacetone emahoreni angu-24, kanye ne-1,1,3-3 ye-trichloropacetone crystallization ngobumsulwa obungaphezu kuka-99% kanye isivuno esingaphezu kuka-45%.
II. Ingxenye yokuhlola
- ukusabela
0 00
- II.
I-ChaCCa+Cl:—ClCH.2CCH.3+Cl.2I-CHCCH.3+C1CH.2CCH.2C1+
- Izinyathelo zokuhlola
Eflaskini enentamo emine ene-spherical condenser engu-500ml, inani elithile le-acetone kanye ne-catalyst lanyakaziswa futhi lafakwa ku-chlorine ekushiseni okusabelayo okungu-10~30 W.Qala isikhathi, yeka ukudlula ku-chlorine amahora ambalwa ngemva kokusabela, futhi uqhubeke. ukugqugquzela ihora elingu-1. I-solvent ekhethekile efana nempahla yengezwe engxubeni ewumphumela, ivuselelwe ihora elingu-1 ngenkathi ipholile ku-10 ° C crystallization, ikhipha i-1,1,3-trichloroacetone.
- 1,1,3.Ukunqunywa okukhethiwe kokuhlanzeka kwe-trichloroacetone
I-Varin 3700 gas chromatograph,QF・1 ikholomu yokugcwalisa kanye nomtshina we-FID zisetshenziswe ukuze kukhethwe ngokukhetha inzuzo yokuhlanzeka komkhiqizo nesixazululo se-chloride.
- Imiphumela yengxoxo
- Umthelela we-catalyst ekukhetheni kwe-chloride ubonise ukukhetha kwe-acetone chlorination
Ithonya elikhulu,Ithebula 1 libala isethi yemiphumela yokuhlola.Kuthebula 1,ukukhethwa okuncane kwe-1,1,3-trichloroacetone kukhuphuke kakhulu(cishe 19.1%) ngaphandle kwe-catalyst,futhi
I-compound amine catalyst ihamba phambili, ifika ku-57.5%o.Izimo zokuhlola: Innl acetone, 3nr) l chlorine,i-catalyst 0.6g, izinga lokushisa 1030°C,
isikhathi amahora angu-18. Phakathi namahora angu-12 va:3.9 Cao h;2
〜7 amahora,vq:27 Cao h;7〜18 amahora,VQ:3.9 kuya h.Ithebula 1.Imiphumela ye-catalyst ekukhetheni komkhiqizo
- Umthelela wesivinini se- through-chlorine ekuphenduleni
Ukuhlola kuthole ukuthi i-chlorine efanayo yayinokukhethwa komkhiqizo okungalungile, okuthuthukisa kakhulu ukukhetha komkhiqizo kanye nesivuno.
Ithebula 2 libala isethi yedatha yokuhlola.
Ithebula 2 Imiphumela yesivinini se-pass-chlorine ekukhetheni umkhiqizo
Ukuhlolwa^isimo:]Petri dish 1 acetone,catalyst:iklasi eliyinhlanganisela 0.6go
Ucwaningo luthole ukuthi i-fluchlorine yayingaphambi kwesikhathi(amahora angu-12) futhi kamuva(amahora angu-8 24),iningi le-chlorine libalekela ukuthi ukusabela kwakuhamba kancane futhi okuphakathi(28 h) kwakushesha.Lapho igesi ye-chlorine imiswa, ukukhetha komkhiqizo kanye nesivuno. zehliswa kakhulu.Imiphumela ikhombise ukuthi i-1,1,3 ikhiqize kancane kakhulu kune
1,1-dichloroacetone.Ngesikhathi sokusabela nge
i-chloride, i-chloride, i-acetone, i-1,1,4003000,
I-CICH2CCH3
o.
leyoII.I-chlorination eqenjini le-submethyl yayiningi
ngokushesha kunaseqenjini le-methyl.Ngakho-ke, i
Umbhali ukholelwa ukuthi inqubo yokusabela kwesizukulwane se-acetone chloride yile:
Ukusabela kwenziwa nge-V1 1 2-5 njengenqubo eyinhloko.
Ngokwedatha yeThebula 2, ukuhleleka kwesivinini sokusabela kwesinyathelo ngasinye
V2^”3^1 2 5>V4
Kuya ngesivinini sokuphendula sesinyathelo ngasinye,
6 | 57.1% | Ikristalu | I-Xi 9.0% | 45.0% |
Kungabonakala kudatha yeThebula 3 ukuthi, ngenxa yomehluko omncane wamaphuzu abilayo phakathi kwe-1,1,3.trichloroacetone kanye nemikhiqizo, ngokuvamile kunzima ukuhlukanisa ukuchithwa kwamanzi futhi ukuhlukanisa kuyindlela elula. imikhiqizo ingasuswa, ukuhlanzeka kunzima
silawula ijubane lokudlula le-chlorine esigabeni ngasinye,
ukufeza inhloso yokunciphisa isikhathi se-chlorine yokudlula kanye nokuvimbela ukukhetha kokwandisa isivinini sokuphendula sesibili ngo-1,1,3 trichloroacetone.
- Ukuhlanzwa kwekristalu enamanzi Ngokusho kwezincwadi, imvamisa i-
I-acetone chloride liquid ikhishwa noma icwengisiswe ngamanzi ukuze kwandiswe okuqukethwe kwe-1,1,3-trichloroacetone, futhi umbhali usebenzise i-1,1,3-trichloroacetone ukuze i-crystallization kusuka kweminye imikhiqizo.
Ithebula 3 libala ukuhlanzeka komkhiqizo okutholwe ngezindlela ezihlukene zokuhlukanisa.
Ithebula 3.Ukuhlanzeka komkhiqizo okutholwe ezindleleni ezihlukene zokuhlukanisa
ukuze uthuthuke ngokwengeziwe.Ukuhlanzeka komkhiqizo kufinyelela ngaphezu kuka-99%, futhi isivuno sibuye sibe phezulu kakhulu ngezindlela eziningi, kufika ku-45%o.1 Indlela idinga okuqukethwe kwe-1,1,3-trichloroacetone ka-K ngaphezu kuka-50% ku-chloride. isisombululo.
Khetha i-compound amine catalyst efanelekile, lawula ukuvinjwa kwe-chlorine ehamba kancane ekuqaleni nasekupheleni kuka-10~30°C, ingenza i-1,1,3-trichloroacetone chloride, ehlanjululwe ngecrystallization ye-solvent ekhethekile, ithole umkhiqizo wecrystalline ongekho ngaphansi kuka-99.0%, ngesivuno ka-45%, kodwa i-1,1,3-trichloroacetone kusisombululo se-chloride kufanele ibe ngaphezu kuka-50%o.Athena CEO
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ENGEZA: Isifunda saseJiangsu, eChina
Isikhathi sokuthumela: Aug-12-2021