Isishwankathelo: i-acetone i-catalyzed chloride kwaye iveliswa yi-solvent crystallization kwi-1,1,3-trichloroacetone enobunyulu obuphezulu obungaphantsi kwe-99.0%, kunye nesivuno se-45% o Amagama angundoqo: 1,1,3-trichloroacetone; ukwenziwa; ubunyulu obuphezulu

———-. Intshayelelo

I-1,1,3■i-trichloroacetone ibaluleke kakhulu kwimveliso ye-folic acid. Okwangoku, i-1,1,3.i-acetone i-trichloropacetone, umjikelo wemveliso omde (iiyure ezingama-48), ukukhetha okungekho semgangathweni, isivuno esiphantsi, umxholo we-1,1,3-trichloropacetone umalunga ne-17% kuphela, emva kokukhupha amanzi, umxholo wayo yi-51.9 kuphela%. Kwaye iindleko zemveliso ziphezulu, ukulungiswa kwemveliso kuphantsi. Zonke ezi zinto zikhokelela kwiindleko eziphezulu zemveliso ye-folic acid yasekhaya, kunzima ukuphucula umxholo kunye nezinye iingxaki. Umbhali ufunde inani elikhulu lamaxwebhu asekhaya nakwamanye amazwe. Emva kovavanyo oluninzi kunye nezifundo, songeze isantya se-catalyst kunye ne-fou chlorine elawulwayo, sinciphisa ixesha lokuphendula ukuya kwi-1,1,3-3 trichloropacetone kwiiyure ezingama-24, kunye ne-1,1,3-3 trichloropacetone crystallization ngobumsulwa obungaphezulu kwe-99% kunye nesivuno esingaphezulu kwe-45%.

II. Inxalenye yovavanyo

1. impendulo

0 0 0 0

1. II.

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

1. Amanyathelo ovavanyo

Kwiflaski enentamo ezine ene-condenser eyi-500ml, inani elithile le-acetone kunye ne-catalyst zivuselelwe zaza zafakwa kwi-chlorine kubushushu be-reaction obuyi-10 ~ 30 W. Qala ixesha, yeka ukudlula kwi-chlorine emva kweeyure ezimbalwa emva kwe-reaction, kwaye uqhubeke uvuselela iyure e-1. Kongezwa into ekhethekileyo efana nesinyibilikisi kumxube ophumayo, yavuselelwa iyure e-1 ngelixa ipholisiwe ukuya kwi-10°C crystallization, ikhupha i-1,1,3-trichloroacetone.

1. 1,1,3. Ukumisela ngokukhetha ubunyulu be-trichloroacetone

I-Varin 3700 gas chromatograph, i-QF・1 filling column kunye ne-FID detector zisetyenzisiwe ukumisela ngokukhetha inzuzo yobumsulwa bemveliso kunye nesisombululo se-chloride.

1. Iziphumo zengxoxo
2. Impembelelo ye-catalyst ekukhetheni i-chloride ibonise ukukhetha kwe-acetone chlorination

Impembelelo enkulu, iTheyibhile 1 idwelisa iseti yeziphumo zovavanyo. Ukusuka kwiTheyibhile 1, ukhetho oluncinci lwe-1,1,3-trichloroacetone lunyuswe kakhulu (malunga ne-19.1%) ngaphandle kwe-catalyst, kwaye

　　I-compound amine catalyst yeyona ilungileyo, ukuya kuthi ga kwi-57.5% o. Iimeko zovavanyo: I-Innl acetone, i-3nr) l chlorine, i-catalyst 0.6g, ubushushu obuyi-1030°C,

ixesha ziiyure ezili-18. Ngaphakathi kweeyure ezili-12 va:3.9 Cao h;2

〜iiyure ezisi-7, vq:27 Cao h;7〜iiyure ezili-18, VQ:3.9 ukuya ku h. Itheyibhile 1. Iziphumo ze-catalyst ekukhetheni imveliso

1. Impembelelo yesantya se-through-chlorine kwimpendulo

Olu vavanyo lufumanise ukuba i-chlorine efanayo yayinokukhetha imveliso kakubi, nto leyo eyaphucula kakhulu ukukhetha imveliso kunye nesivuno sayo.

Itheyibhile 2 idwelisa iseti yedatha yovavanyo.

Itheyibhile 2 Imiphumo yesantya se-pass-chlorine ekukhetheni imveliso

Uvavanyo^imeko:]Isitya sePetri i-acetone eyi-1, i-catalyst: iklasi ye-composite 0.6go

Olu vavanyo lufumanise ukuba i-fluchlorine yayisekuqaleni (iiyure ezili-12) kwaye kamva (iiyure ezisi-8 ukuya kwezingama-24), uninzi lwe-chlorine luphuma apho impendulo yayicotha kwaye i-medium (iiyure ezingama-28) yayikhawuleza. Xa igesi ye-chlorine imisiwe, ukukhetha imveliso kunye nemveliso kuncitshiswa kakhulu. Iziphumo zibonise ukuba i-1,1,3 ivelise kancinci kakhulu kune-1,1,3.

1,1-dichloroacetone. Ngexesha lokuphendula nge

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

I-CICH2CCH3

o.

yiyo i_II.i-chlorination kwiqela le-submethyl yayininzi kakhulu.

ngokukhawuleza kunakwiqela le-methyl. Ke ngoko,

Umbhali ukholelwa ukuba inkqubo yokusabela kwenkqubo yokuvelisa i-acetone chloride yile:

I-reaction yenziwa nge-V1 1 2-5 njengenkqubo ephambili.

Ngokwedatha yeTheyibhile 2, ulungelelwaniso lwesantya sokusabela kwenyathelo ngalinye

　　V2^”3^1 2 5>V4

Kuxhomekeke kwisantya sokusabela kwenyathelo ngalinye,

Kuyabonakala kwidatha yeTheyibhile 3 ukuba, ngenxa yomahluko omncinci weqondo lokubila phakathi kwe-1, 1, 3. i-trichloroacetone kunye neemveliso ezingaphantsi, kunzima kakhulu ukwahlula ukukhupha amanzi kwaye ukwahlula yindlela elula. Nangona uninzi lweemveliso ze-1 zinokususwa, ubumsulwa bunzima.

silawula isantya se-chlorine kwinqanaba ngalinye,

ukufezekisa injongo yokunciphisa ixesha le-chlorine elidlulayo kunye nokuthintela ukukhetha kokunyusa isantya sempendulo yesibini nge-1,1,3 trichloroacetone.

1. Ukuhlanjululwa kwekristale emanzi Ngokutsho kweencwadi, ngokuqhelekileyo

Ulwelo lwe-acetone chloride lukhutshwa okanye lucocwe ngamanzi ukuze kwandiswe umxholo we-1,1,3-trichloroacetone, kwaye umbhali usebenzise i-1,1,3-trichloroacetone ukwenza i-crystallization evela kwezinye iimveliso ezingaphantsi kwayo.

Itheyibhile 3 idwelisa ubunyulu bemveliso obufunyenwe ngeendlela ezahlukeneyo zokwahlulahlula.

Itheyibhile 3. Ubumsulwa bemveliso obufunyenwe kwiindlela ezahlukeneyo zokwahlulahlula

ukuphucula ngakumbi. Ubumsulwa bemveliso bufikelela ngaphezulu kwe-99%, kwaye isivuno sikwaphezulu kwiindlela ezahlukeneyo, ukuya kuthi ga kwi-45% o.1 Le ndlela ifuna umxholo we-1,1,3-trichloroacetone we-K ngaphezulu kwe-50% kwisisombululo se-chloride.

Khetha i-compound amine catalyst efanelekileyo, lawula ukuvinjwa kwe-chlorine kancinci ekuqaleni nasemva kwexesha kwi-10~30°C, ingenza i-1,1,3-trichloroacetone chloride, ecociweyo yi-solvent crystallization ekhethekileyo, ifumane imveliso ye-crystalline engaphantsi kwe-99.0%, enemveliso ye-45%, kodwa i-1,1,3-trichloroacetone kwisisombululo se-chloride kufuneka ibe ngaphezulu kwe-50%o.I-CEO yase-Athena

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