Abstract: acetone catalyzed chloride thiab tsim los ntawm cov kuab tshuaj crystallization ntawm 1,1,3-trichloroacetone nrog kev ntshiab siab tsis tsawg dua 99.0%, nrog rau cov txiaj ntsig ntawm 45% o Cov lus tseem ceeb: 1,1,3-trichloroacetone; synthesis; kev ntshiab siab

———-. Lus Qhia Ua Ntej

1,1,3■trichloroacetone yog ib qho tseem ceeb hauv kev tsim cov folic acid. Tam sim no, 1,1,3.acetone trichloropacetone, lub voj voog tsim khoom ntev (48 teev), kev xaiv tsis zoo, cov txiaj ntsig qis, cov ntsiab lus 1,1,3-trichloropacetone tsuas yog li 17%, tom qab rho tawm dej, nws cov ntsiab lus tsuas yog 51.9%. Thiab tus nqi tsim khoom siab, kev kho cov khoom qis. Cov no ua rau cov nqi tsim khoom folic acid hauv tsev siab, nyuaj rau txhim kho cov ntsiab lus thiab lwm yam teeb meem. Tus sau tau nyeem ntau cov ntaub ntawv hauv tsev thiab txawv teb chaws. Tom qab ntau qhov kev sim thiab kev tshawb fawb, peb tau ntxiv catalyst thiab tswj plaub chlorine ceev, txo lub sijhawm teb rau 1,1,3-3 trichloropacetone hauv 24 teev, thiab 1,1,3-3 trichloropacetone crystallization nrog kev ntshiab ntau dua 99% thiab cov txiaj ntsig ntau dua 45%.

II. Ib feem sim

1. kev ua xua

0 0 0 0

1. II.

　　CHAcHa+Cl:—ClCH₂.₂CCH.₃+Cl.₂CHCCH.₃+C1CH.₂CCH.₂C1+

1. Cov kauj ruam sim

Hauv lub raj mis plaub-caj dab nrog 500ml spherical condenser, ib qho me me ntawm acetone thiab catalyst tau do thiab pub rau chlorine ntawm qhov kub ntawm 10 ~ 30 W. Pib lub sijhawm, tsis txhob hla dhau chlorine ob peb teev tom qab qhov tshuaj tiv thaiv, thiab txuas ntxiv do rau 1 teev. Ib qho khoom siv tshwj xeeb zoo li cov kuab tshuaj tau ntxiv rau qhov sib tov, do rau 1 teev thaum txias rau 10 ° C crystallization, rho tawm 1,1,3-trichloroacetone.

1. 1,1,3. Kev txiav txim siab xaiv ntawm trichloroacetone purity

Cov roj chromatograph Varin 3700, QF ・ 1 kab sau thiab FID detector tau siv los txiav txim siab qhov purity ntawm cov khoom thiab cov tshuaj chloride.

1. Cov txiaj ntsig ntawm kev sib tham
2. Qhov cuam tshuam ntawm catalyst rau chloride selectivity qhia tau qhov kev xaiv ntawm acetone chlorination

Kev cuam tshuam loj, Rooj 1 teev cov txheej txheem ntawm cov txiaj ntsig sim. Los ntawm Rooj 1, qhov kev xaiv tsawg kawg nkaus ntawm 1,1,3-trichloroacetone tau nce ntxiv ntau (kwv yees li 19.1%) yam tsis muaj catalyst, thiab

　　cov tshuaj amine catalyst yog qhov zoo tshaj plaws, txog li 57.5% o. Cov xwm txheej xeem: Innl acetone, 3nr) l chlorine, catalyst 0.6g, kub 1030 ° C,

lub sijhawm 18 teev. Hauv 12 teev va: 3.9 Cao h; 2

~7 teev, vq: 27 Cao h; 7 ~ 18 teev, VQ: 3.9 rau h. Rooj 1. Cov teebmeem ntawm cov catalyst rau kev xaiv khoom

1. Cov nyhuv ntawm qhov ceev ntawm chlorine los ntawm kev sib xyaw ua ke

Qhov kev sim pom tau tias cov tshuaj chlorine sib xws muaj kev xaiv khoom tsis zoo, ua rau kev xaiv khoom thiab cov txiaj ntsig zoo dua.

Rooj 2 teev cov ntaub ntawv sim.

Rooj 2 Cov teebmeem ntawm qhov ceev ntawm pass-chlorine rau kev xaiv khoom

Kev Ntsuas ^ mob:] Lub tais Petri 1 acetone, catalyst: chav kawm sib xyaw 0.6go

Qhov kev sim pom tau tias cov fluchlorine tau tawm thaum ntxov (12 teev) thiab tom qab ntawd (8 txog 24 teev), feem ntau cov chlorine tawm uas cov tshuaj tiv thaiv qeeb thiab cov nruab nrab (28 teev) ceev. Thaum cov pa chlorine raug tso tseg, qhov kev xaiv khoom thiab cov txiaj ntsig tau txo qis heev. Cov txiaj ntsig tau qhia tias 1,1,3 tsim tawm qeeb dua li

1,1-dichloroacetone. Thaum lub sijhawm ua tshuaj nrog

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

CICH2CCH3

o.

uas yog_II.chlorination ntawm submethyl pawg yog ntau

sai dua li ntawm pawg methyl. Yog li ntawd, tus

Tus sau ntseeg tias cov txheej txheem tsim cov acetone chloride yog:

Cov tshuaj tiv thaiv yog ua nrog V1 1 2-5 ua tus txheej txheem tseem ceeb.

Raws li cov ntaub ntawv hauv Rooj 2, qhov kev txiav txim siab ntawm txhua kauj ruam yog

　　V2^”3^1 2 5>V4

Nyob ntawm qhov ceev ntawm txhua kauj ruam,

Nws tuaj yeem pom los ntawm cov ntaub ntawv ntawm Rooj 3 tias, vim yog qhov sib txawv me me ntawm qhov kub ntawm 1,1,3.trichloroacetone thiab cov khoom lag luam, feem ntau nws nyuaj rau cais cov dej rho tawm thiab kev sib cais yog ib txoj hauv kev yooj yim. Txawm hais tias feem ntau cov khoom I tuaj yeem tshem tawm, qhov huv si yog qhov nyuaj

peb tswj qhov ceev ntawm cov tshuaj chlorine ntawm txhua theem,

kom ua tiav lub hom phiaj ntawm kev txo lub sijhawm dhau chlorine thiab inhibiting qhov kev xaiv ntawm kev nce qhov ceev ntawm cov tshuaj tiv thaiv thib ob los ntawm 1,1,3 trichloroacetone ..

1. Hydrated crystal purification Raws li cov ntaub ntawv, feem ntau yog

Cov kua acetone chloride raug rho tawm lossis ua kom huv los ntawm dej kom nce cov ntsiab lus ntawm 1,1,3-trichloroacetone, thiab tus sau tau siv 1,1,3-trichloroacetone los ua kom cov khoom siv los ntawm lwm cov khoom siv.

Rooj 3 teev cov khoom purity tau los ntawm ntau txoj kev sib cais.

Rooj 3. Kev huv ntawm cov khoom tau los ntawm ntau txoj kev sib cais sib txawv

kom txhim kho ntxiv. Cov khoom purity ncav cuag tshaj 99%, thiab cov txiaj ntsig kuj yog qhov siab tshaj plaws hauv ntau txoj kev, txog li 45% o.1 Txoj kev xav tau 1,1,3-trichloroacetone cov ntsiab lus ntawm K ntau dua 50% hauv cov tshuaj chloride.

Xaiv cov tshuaj amine catalyst uas tsim nyog, tswj kev thaiv chlorine qeeb thaum ntxov thiab lig ntawm 10 ~ 30 ° C, tuaj yeem ua 1,1,3-trichloroacetone chloride, purified los ntawm cov kuab tshuaj tshwj xeeb crystallization, tau txais cov khoom crystalline nrog tsis tsawg dua 99.0%, nrog cov txiaj ntsig ntawm 45%, tab sis 1,1,3-trichloroacetone hauv cov tshuaj chloride yuav tsum ntau dua 50% o.Athena CEO

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