Isifinyezo: i-acetone i-catalyzed chloride futhi ikhiqizwa yi-solvent crystallization ku-1,1,3-trichloroacetone enokuhlanzeka okuphezulu okungenani okungu-99.0%, enesivuno esingu-45%o Amagama ayisihluthulelo: 1,1,3-trichloroacetone; ukwenziwa; ukuhlanzeka okuphezulu

———-. Isandulelo

I-1,1,3■i-trichloroacetone iyinto ebalulekile ekukhiqizweni kwe-folic acid. Njengamanje, i-1,1,3.i-acetone trichloropacetone, umjikelezo wokukhiqiza omude (amahora angu-48), ukukhetha okubi, isivuno esiphansi, okuqukethwe kwe-1,1,3-trichloropacetone kungama-17% kuphela, ngemuva kokukhishwa kwamanzi, okuqukethwe kwayo kungama-51.9% kuphela. Futhi izindleko zokukhiqiza ziphezulu, ukulungiswa komkhiqizo kuphansi. Konke lokhu kuholela ezindleleni eziphezulu zokukhiqiza i-folic acid yasekhaya, kunzima ukuthuthukisa okuqukethwe nezinye izinkinga. Umbhali ufunde inani elikhulu lemibhalo yasekhaya neyangaphandle. Ngemuva kokuhlolwa okuningi nezifundo, sengeze isivinini se-catalyst kanye ne-fou chlorine elawulwayo, sanciphisa isikhathi sokusabela saba yi-1,1,3-3 trichloropacetone emahoreni angama-24, kanye ne-1,1,3-3 trichloropacetone crystallization ngobumsulwa obungaphezu kwama-99% kanye nesivuno esingaphezu kwama-45%.

II. Ingxenye yokuhlola

1. ukusabela

0 0 0 0

1. II.

　　I-CHACCHa+Cl:—ClCH.₂I-CCH.₃+Cl.₂I-CHCCH.₃+C1CH.₂I-CCH.₂C1+

1. Izinyathelo zokuhlola

Ebhodleleni elinezintamo ezine eline-condenser eyindilinga engu-500ml, inani elithile le-acetone kanye ne-catalyst kwavuselelwa futhi kwafakwa i-chlorine ekushiseni kokusabela okungu-10 ~ 30 W. Qala isikhathi, yeka ukudlula i-chlorine emahoreni ambalwa ngemva kokusabela, bese uqhubeka uvuselela ihora eli-1. Kwengezwe into ekhethekile efana nesinyibilikisi engxubeni ephumayo, yavuselelwa ihora eli-1 ngenkathi ipholiswa ku-10°C crystallization, yakhipha i-1,1,3-trichloroacetone.

1. 1,1,3. Ukunqunywa kokukhetha kokuhlanzeka kwe-trichloroacetone

I-Varin 3700 gas chromatograph, ikholomu yokugcwalisa ye-QF・1 kanye ne-FID detector kwasetshenziswa ukunquma ngokukhetha inzuzo yobumsulwa bomkhiqizo kanye nesixazululo se-chloride.

1. Imiphumela yengxoxo
2. Ithonya le-catalyst ekukhetheni i-chloride libonise ukukhetha kwe-acetone chlorination

Ithonya elikhulu, Ithebula 1 libala isethi yemiphumela yokuhlola. Kusukela kuThebula 1, ukukhetha okuncane kwe-1,1,3-trichloroacetone kukhushulwe kakhulu (cishe ngo-19.1%) ngaphandle kwe-catalyst, futhi

　　i-compound amine catalyst iyona engcono kakhulu, kufika ku-57.5%o. Izimo zokuhlola: I-Innl acetone, i-3nr) l chlorine, i-catalyst 0.6g, izinga lokushisa elingu-1030°C,

isikhathi amahora angu-18. Phakathi kwamahora angu-12 va:3.9 Cao h;2

〜Amahora angu-7, vq:27 Cao h;7〜Amahora angu-18, VQ:3.9 kuya ku-h.Ithebula 1.Imiphumela ye-catalyst ekukhetheni komkhiqizo

1. Umphumela wejubane le-through-chlorine ekusabeleni

Ukuhlolwa kwathola ukuthi i-chlorine efanayo yayinokukhetha okubi komkhiqizo, okuthuthukisa kakhulu ukukhetha kanye nokukhiqiza komkhiqizo.

Ithebula 2 libala isethi yedatha yokuhlola.

Ithebula 2 Imiphumela yejubane lokudlula kwe-chlorine ekukhetheni komkhiqizo

Isivivinyo^isimo:]Isidlo sePetri i-acetone engu-1, i-catalyst:iklasi elihlanganisiwe 0.6go

Ukuhlolwa kuthole ukuthi i-fluchlorine yayisekuqaleni (amahora ayi-12) futhi kamuva (amahora ayi-8 kuya kwangu-24), iningi le-chlorine liphuma ukuthi ukusabela kwakuhamba kancane kanti okuphakathi (amahora angama-28) kwakuhamba ngokushesha. Lapho igesi ye-chlorine imiswa, ukukhetha komkhiqizo kanye nesivuno kuncipha kakhulu. Imiphumela ibonise 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.

leyo_II.i-chlorination eqenjini le-submethyl yayiningi kakhulu.

ngokushesha kunaseqenjini le-methyl. Ngakho-ke,

Umbhali ukholelwa ukuthi inqubo yokusabela kwenqubo yokukhiqizwa kwe-acetone chloride yile:

Ukusabela kwenziwa nge-V1 1 2-5 njengenqubo eyinhloko.

Ngokusho kwedatha yeThebula 2, i-oda lejubane lokusabela lesinyathelo ngasinye liyi

　　V2^”3^1 2 5>V4

Kuye ngesivinini sokusabela kwesinyathelo ngasinye,

Kungabonakala kudatha yeThebula 3 ukuthi, ngenxa yomehluko omncane wamaphuzu okubila phakathi kwe-1, 1, 3. i-trichloroacetone kanye nemikhiqizo engaphansi kwayo, ngokuvamile kunzima ukuhlukanisa ukukhishwa kwamanzi futhi ukuhlukaniswa kuyindlela elula. Nakuba imikhiqizo eminingi ye-1 ingasuswa, ubumsulwa bunzima.

silawula isivinini sokudlulisa i-chlorine esigabeni ngasinye,

ukufeza inhloso yokunciphisa isikhathi sokudlula kwe-chlorine nokuvimbela ukukhetha kokwandisa isivinini sokuphendula kwesibili ngo-1,1,3 trichloroacetone.

1. Ukuhlanzwa kwekristalu okumanzi Ngokusho kwezincwadi, ngokuvamile

Uketshezi lwe-acetone chloride lukhishwa noma lucwengisiswa ngamanzi ukuze kwandiswe okuqukethwe yi-1,1,3-trichloroacetone, kanti umbhali usebenzise i-1,1,3-trichloroacetone ukuze kukhiqizwe amakristalu kusuka kweminye imikhiqizo engaphansi kwayo.

Ithebula 3 libala ubumsulwa bomkhiqizo obutholakala ngezindlela ezahlukene zokuhlukanisa.

Ithebula 3. Ubumsulwa bomkhiqizo obutholakala ezindleleni ezahlukene zokuhlukanisa

ukuthuthukisa kakhulu. Ukuhlanzeka komkhiqizo kufinyelela ngaphezu kuka-99%, futhi isivuno siphezulu kakhulu ezindleleni eziningana, kufika ku-45% o.1 Le ndlela idinga okuqukethwe okungu-1,1,3-trichloroacetone okungu-K okungaphezu kuka-50% kusisombululo se-chloride.

Khetha i-compound amine catalyst efanele, lawula ukuvimba kwe-chlorine okuhamba kancane ekuqaleni nasekupheleni kuka-10~30°C, kungenza i-1,1,3-trichloroacetone chloride, ehlanzwa yi-solvent crystallization ekhethekile, ithole umkhiqizo we-crystalline okungenani ongaphansi kuka-99.0%, ngesivuno esingu-45%, kodwa i-1,1,3-trichloroacetone esixazululweni se-chloride kumele ibe ngaphezu kuka-50%o.I-CEO ye-Athena

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