Abstract:i-acetone catalyzed chloride kwaye iveliswe yi-solvent crystallization kwi-1,1,3-trichloroacetone enobunyulu obuphezulu obungekho ngaphantsi kwe-99.0%, kunye nesivuno se-45% o Amagama angundoqo:1,1,3-trichloroacetone;synthesis;ucoceko oluphezulu

———-. Intshayelelo

1,1,3■i-trichloroacetone siphakathi esibalulekileyo kwimveliso ye-folic acid.Okwangoku,1,1,3.i-acetone trichlorropacetone,umjikelo omde wemveliso(iiyure ezingama-48),ukhetho olulambathayo,isivuno esiphantsi,1,1,3- Umxholo we-trichloropacetone umalunga ne-17% kuphela, emva kokutsalwa kwamanzi, umxholo wayo ngu-51.9% kuphela. Kwaye ixabiso lokuvelisa liphezulu, ukulungiswa kwemveliso kuphantsi.Onke oku kukhokelela kwiindleko eziphezulu zokuvelisa i-folic acid yasekhaya, kunzima ukuphucula umxholo kunye nezinye. iingxaki.Umbhali ufunde inani elikhulu lamaxwebhu asekhaya nawangaphandle. Emva kwezilingo ezininzi kunye nezifundo, songeze i-catalyst kunye nokulawula isantya se-chlorine e-fou, sinciphisa ixesha lokuphendula kwi-1,1,3-3 ye-trichloropacetone kwiiyure ze-24, kunye ne-1,1,3-3 ye-trichloropacetone crystallization ngobunyulu obukhulu kune-99% kunye isivuno esingaphezulu kwama-45%.

II. Inxalenye yovavanyo

1. ukusabela

0 0 0 0

1. II.

　　CHACCa+Cl:—ClCH.₂CCH.₃+Cl.₂CHCCH.₃+C1CH.₂CCH.₂C1+

1. Amanyathelo ovavanyo

Kwiflask enentamo emine ene-500ml spherical condenser, isixa esithile se-acetone kunye ne-catalyst yavuselelwa kwaye yondliwa kwi-chlorine kwiqondo lokushisa lokusabela kwe-10 ~ 30 W.Qalisa ixesha, yeka ukudlula kwi-chlorine kwiiyure ezininzi emva kokuphendula, kwaye uqhubeke. ukuvuselela iyure ye-1. I-solvent ekhethekileyo efana neyona nto yongezwa kumxube obangelwayo, ixutywe ngeyure ye-1 ngelixa ipholile kwi-10 ° C crystallization, ikhupha i-1,1,3-trichloroacetone.

1. 1,1,3.Ukuzimisela okukhethiweyo kokucoceka kwe-trichloroacetone

I-Varin 3700 ye-chromatograph yegesi, i-QF ・ Ikholamu yokuzalisa e-1 kunye nesixhobo se-FID zisetyenziselwe ukukhetha ukucoceka kwenzuzo yemveliso kunye nesisombululo sekloridi.

1. Iziphumo zengxoxo
2. Impembelelo ye-catalyst kwi-chloride selectivity ibonise ukukhethwa kwe-acetone chlorination

Impembelelo enkulu, iThebhile 1 idwelisa isethi yeziphumo zovavanyo.Ukusuka kwiThebhile 1, ubuncinci bokukhethwa kwe-1,1,3-trichloroacetone yanda kakhulu (malunga ne-19.1%) ngaphandle kwe-catalyst, kwaye

　　I-compound amine catalyst yeyona nto ingcono, ukuya kuthi ga kwi-57.5% o.Iimeko zovavanyo: Innl acetone, 3nr) l chlorine, catalyst 0.6g, iqondo lobushushu 1030°C,

ixesha 18 iiyure.Ngaphakathi 12 iiyure va:3.9 Cao h;2

〜7 iiyure,vq:27 Cao h;7〜18 iiyure,VQ:3.9 ukuya h.Itheyibhile 1.Iziphumo zecatalyst ekukhetheni imveliso

1. Impembelelo yesantya sokudlula kwiklorin ekuphenduleni

Uvavanyo lwafumanisa ukuba iklorini efanayo yayinokhetho olubi lwemveliso, iphucula kakhulu ukukhethwa kwemveliso kunye nesivuno.

Itheyibhile 2 idwelisa iseti yedatha yovavanyo.

Itheyibhile 2 Iziphumo ze-pass-chlorine velocity ekukhetheni imveliso

Uvavanyo^imeko:]Petri dish 1 acetone,catalyst:composite class 0.6go

Uvavanyo lwafumanisa ukuba i-fluchlorine yayisekuqaleni (iiyure ezili-12) kwaye kamva (8 24 h), uninzi lweklorini lubalekela ukuba ukusabela kwakucotha kwaye okuphakathi (28 h) kwakhawuleza. zincitshiswe kakhulu.Iziphumo zibonise ukuba i-1,1,3 ivelise kade kakhulu kune

1,1-dichloroacetone.Ngexesha lokusabela nge

ikloridi,ikloridi,iacetone,1,1,4003000,

CICH2CCH3

o.

yiyo i_II.I-chlorination kwiqela le-submethyl yayininzi

ngokukhawuleza kunakwiqela le-methyl.Ngoko ke, i

Umbhali ukholelwa ukuba inkqubo yokuphendula i-acetone chloride yile:

Ukusabela kuqhutywa nge-V1 1 2-5 njengeyona nkqubo iphambili.

Ngokutsho kwedatha yeThebhile 2, ulandelelwano lwesantya sokusabela kwinyathelo ngalinye

　　V2^”3^1 2 5>V4

Ngokuxhomekeke kwisantya sokusabela kwinyathelo ngalinye,

Inokubonwa kwidatha yeThebhile 3 ukuba, ngenxa yomahluko omncinci wokubilisa phakathi kwe-1,1,3.trichloroacetone kunye neemveliso, ngokuqhelekileyo kunzima ukwahlula ukutsalwa kwamanzi kunye nokwahlula yindlela elula.Nangona uninzi I iimveliso zinokususwa, ubunyulu bunzima

silawula isantya seklorine yokudlula kwinqanaba ngalinye,

ukufezekisa injongo yokunciphisa ixesha leklorine yokudlula kunye nokuthintela ukhetho lokunyusa isantya sokusabela okwesibini nge-1,1,3 trichloroacetone.

1. Ukucocwa kwekristale eHydrated Ngokutsho koncwadi, ngokuqhelekileyo i

I-acetone chloride liquid ikhutshwe okanye ihlanjululwe ngamanzi ukunyusa umxholo we-1,1,3-trichloroacetone, kwaye umbhali wasebenzisa i-1,1,3-trichloroacetone kwi-crystallization evela kwezinye iimveliso.

Itheyibhile 3 idwelisa ukucoceka kwemveliso efunyenwe ngeendlela ezahlukeneyo zokwahlula.

Itheyibhile 3.Ukucoceka kwemveliso efunyenwe kwiindlela ezahlukeneyo zokwahlula

ukuphucula ngakumbi.Ubusulungeko lwemveliso bufikelela ngaphezu kwe-99%, kwaye isivuno sikwayesona siphezulu kwiindlela ezininzi, ukuya kuthi ga kwi-45%o.1 Indlela ifuna isiqulatho se-1,1,3-trichloroacetone ye-K ngaphezu kwe-50% kwikloridi. isisombululo.

Khetha i-compound amine catalyst efanelekileyo, lawula ukucotha kweklorini ukuvalela kwangethuba nasemva kwexesha nge-10 ~ 30°C, unokwenza i-1,1,3-trichloroacetone chloride, ihlanjululwe ngecrystallization yokunyibilikisa okukhethekileyo, ifumane imveliso yecrystalline engekho ngaphantsi kwe-99.0%, ngesivuno ye-45%, kodwa i-1,1,3-trichloroacetone kwisisombululo sekloridi kufuneka ibe nkulu kune-50%o.Athena CEO

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