Pfupiso: acetone yakakonzera chloride uye inogadzirwa ne solvent crystallization pa 1,1,3-trichloroacetone ine kuchena kwakanyanya kweisingasviki 99.0%, ine goho re 45% o Mazwi makuru: 1,1,3-trichloroacetone; synthesis; kuchena kwakanyanya

———-. Mashoko Ekutanga

1,1,3■trichloroacetone chinhu chakakosha pakugadzirwa kwefolic acid. Parizvino, 1,1,3.acetone trichloropacetone, kugadzirwa kwenguva refu (maawa 48), kusasarudza zvakanaka, goho diki, 1,1,3-trichloropacetone huwandu hunenge 17% chete, mushure mekutorwa kwemvura, huwandu hwayo hunongova 51.9%. Uye mutengo wekugadzira wakakwira, kugadziriswa kwechigadzirwa kwakaderera. Izvi zvese zvinotungamira kumitengo yepamusoro yekugadzira folic acid yemuno, zvakaoma kuvandudza huwandu hwezvinhu nezvimwe zvinetso. Munyori akaverenga magwaro akawanda emuno neekunze. Mushure mekuedza kwakawanda nezvidzidzo, takawedzera catalyst uye controlled fou chlorine speed, tichideredza nguva ye reaction kusvika 1,1,3-3 trichloropacetone mumaawa 24, uye 1,1,3-3 trichloropacetone crystallization nekuchena kwakapfuura 99% uye goho rinopfuura 45%.

II. Chikamu chekuedza

1. maitiro

0 0 0 0

1. II.

　　CHACCHa+Cl:—ClCH.₂CCH. (Chikamu cheCCH).₃+Cl.₂CHIKAMU.₃+C1CH.₂CCH. (Chikamu cheCCH).₂C1+

1. Matanho ekuyedza

Muchirongo chine mitsipa mina chine 500ml spherical condenser, huwandu hwakati hweacetone necatalyst zvakasanganiswa ndokuiswa muchlorine patembiricha ye reaction ye10 ~ 30 W. Tanga nguva, rega kupfuura nechlorine maawa akati wandei mushure me reaction, uye ramba uchikurunga kweawa imwe. Chinhu chakafanana nechinonyungudutsa chakawedzerwa kumusanganiswa wakabuda, chakakurunga kweawa imwe uku chichitonhodzwa kusvika ku10°C crystallization, chichiburitsa 1,1,3-trichloroacetone.

1. 1,1,3. Kusarudza kuchena kwetrichloroacetone

Varin 3700 gas chromatograph, QF・1 filling column uye FID detector zvakashandiswa kusarudza purofiti yechinhu ichi ne chloride solution.

1. Mhedzisiro yehurukuro
2. Simba re catalyst pakusarudza chloride rakaratidza kusarudza kwe acetone chlorination

Simba guru, Tafura 1 inonyora seti yemhedzisiro yekuyedza. Kubva paTafura 1, sarudzo shoma ye1,1,3-trichloroacetone yakawedzera zvakanyanya (inenge 19.1%) pasina catalyst, uye

　　Chinhu chinobatsira mukugadzira amine catalyst ndicho chakanakisa, kusvika ku57.5%o. Mamiriro ekuyedza: Innl acetone, 3nr) l chlorine, catalyst 0.6g, tembiricha 1030°C,

nguva maawa gumi nemasere. Mukati memaawa gumi nemaviri va:3.9 Cao h;2

〜7 maawa, vq:27 Cao h;7〜18 maawa, VQ:3.9 kusvika h. Tafura 1. Mhedzisiro ye catalyst pakusarudza chigadzirwa

1. Mhedzisiro yekumhanya kwe through-chlorine pane reaction

Kuedza uku kwakawana kuti chlorine yakafanana yakanga isina sarudzo yakanaka yezvigadzirwa, zvichiita kuti sarudzo yezvigadzirwa ive nani uye goho rayo riwedzere.

Tafura 2 inoratidza ruzivo rwekuyedza.

Tafura 2 Mhedzisiro yekumhanya kwepasi-chlorine pakusarudza chigadzirwa

Muedzo^mamiriro:]Petri dish 1 acetone, catalyst: composite class 0.6go

Kuedza kwacho kwakawana kuti fluchlorine yakanga iri mangwanani (maawa gumi nemaviri) uye gare gare (maawa masere nemakumi maviri nemana), chlorine yakawanda yakabuda ichitaura kuti reaction yacho yakanga iri kunonoka uye pakati (maawa makumi maviri nemasere) yakanga iri nekukurumidza. Kana gasi rechlorine rikamiswa, kusarudza kwechigadzirwa uye goho zvinodzikira zvakanyanya. Zvakabuda zvakaratidza kuti 1, 1, 3 yakaburitsa zvishoma nezvishoma kupfuura

1,1-dichloroacetone. Munguva yekuita ne

kloridhi, chloride, acetone, 1,1,4003000,

CICH2CCH3

o.

ndizvozvo_II.chlorination paboka re submethyl yaive yakawanda.

nekukurumidza kupfuura paboka remethyl. Nokudaro,

Munyori anotenda kuti maitiro ekuita maitiro ekugadzira acetone chloride ndeekuti:

Maitiro acho anoitwa neV1 1 2-5 senzira huru.

Zvichienderana nedata reTafura 2, kurongeka kwekumhanya kwekuita kwedanho rega rega ndiko

　　V2^”3^1 2 5>V4

Zvichienderana nekumhanya kwekuita kwedanho rega rega,

Zvinogona kuonekwa kubva mudata riri muTafura 3 kuti, nekuda kwemusiyano mudiki wekubikira pakati pe1,1,3.trichloroacetone nezvinobva muzvinhu, zvinowanzova zvakaoma kupatsanura kuburitsa mvura uye kupatsanura inzira iri nyore. Kunyangwe zvigadzirwa zvakawanda zvichigona kubviswa, kuchena kwacho kwakaoma.

tinodzora kumhanya kwe chlorine padanho rega rega,

kuzadzisa chinangwa chekuderedza nguva ye chlorine inodarika uye kudzivirira kusarudza kwekuwedzera kumhanya kwechipiri kwekuita ne 1,1,3 trichloroacetone.

1. Kucheneswa kwekristaro kwakanyorova. Sekureva kwemabhuku, kazhinji

Mvura yeacetone chloride inobviswa kana kunatswa nemvura kuti iwedzere huwandu hwe1,1,3-trichloroacetone, uye munyori akashandisa 1,1,3-trichloroacetone kugadzira kristalllization kubva kune zvimwe zvigadzirwa.

Tafura 3 inoratidza kuchena kwechigadzirwa chinowanikwa nenzira dzakasiyana-siyana dzekuparadzanisa.

Tafura 3. Kuchena kwechigadzirwa kunowanikwa kubva munzira dzakasiyana dzekuparadzanisa

kuti zviwedzere kuvandudzwa. Kuchena kwechigadzirwa kunosvika pamusoro pe99%, uye goho racho rakanyanyawo kuwanikwa munzira dzakasiyana-siyana, kusvika ku45% o.1 Nzira iyi inoda 1,1,3-trichloroacetone yeK inopfuura 50% mu chloride solution.

Sarudza compound amine catalyst yakakodzera, dzora chlorine blocking inononoka pakutanga uye kunonoka pa10~30°C, inogona kugadzira 1,1,3-trichloroacetone chloride, inocheneswa ne solvent crystallization chaiyo, kuwana chigadzirwa che crystalline chisina pasi pe99.0%, negoho re45%, asi 1,1,3-trichloroacetone mu chloride solution inofanira kunge iri pamusoro pe50%o.CEO weAthena

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