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

———-.Lus qhuab ntuas

1,1,3■trichloroacetone yog ib qho tseem ceeb nruab nrab ntawm kev tsim cov folic acid.Tam sim no, 1,1,3.acetone trichloropacetone, ntev ntau lawm voj voog (48 teev), tsis zoo xaiv, tsis tshua muaj yield, 1,1,3- cov ntsiab lus trichloropacetone tsuas yog li 17%, tom qab dej rho tawm, nws cov ntsiab lus tsuas yog 51.9% thiab cov nqi tsim khoom yog siab, cov khoom kho yog tsawg.Cov no ua rau cov nqi siab hauv tsev folic acid ntau lawm, nyuaj rau kev 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 ntxiv catalyst thiab tswj fou chlorine ceev, txo cov tshuaj tiv thaiv lub sij hawm rau 1,1,3-3 trichloropacetone nyob rau hauv 24 teev, thiab 1,1,3-3 trichloropacetone crystallization nrog purity ntau dua 99% thiab cov yield ntau tshaj 45%.

II.Kev sim ib feem

1. tshuaj tiv thaiv

000 0

1. II.

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

1. Kev sim cov kauj ruam

Nyob rau hauv ib lub khob plaub-caj dab nrog 500ml spherical condenser, ib qho nyiaj ntawm acetone thiab catalyst tau nplawm thiab pub rau cov tshuaj chlorine ntawm qhov kub thiab txias ntawm 10 ~ 30 W. Pib lub sij hawm, nres dhau ntawm cov tshuaj chlorine ob peb teev tom qab cov tshuaj tiv thaiv, thiab txuas ntxiv mus. nplawm rau 1 teev.Ib cov kuab tshuaj tshwj xeeb zoo li cov khoom raug ntxiv rau qhov sib xyaw ua ke, stirred rau 1 teev thaum txias rau 10 ° C crystallization, rho tawm 1,1,3-trichloroacetone.

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

Varin 3700 gas chromatograph, QF・1 sau kem thiab FID detector tau siv los xaiv los txiav txim siab purity profit ntawm cov khoom thiab tshuaj chloride.

1. Cov txiaj ntsig ntawm kev sib tham
2. Kev cuam tshuam ntawm catalyst ntawm chloride selectivity pom qhov kev xaiv ntawm acetone chlorination

Kev cuam tshuam loj, Table 1 teev cov txiaj ntsig ntawm kev sim. Los ntawm Table 1, qhov tsawg kawg nkaus xaiv ntawm 1,1,3-trichloroacetone yog nce ntau (li 19.1%) yam tsis muaj catalyst, thiab

　　compound amine catalyst yog qhov zoo tshaj plaws, mus txog 57.5% o.Test mob: Innl acetone, 3nr) l chlorine, catalyst 0.6g, kub 1030 ° C,

Sijhawm 18 teev.In 12 teev va: 3.9 Cao h; 2

~ 7 teev, vq: 27 Cao h; 7 ~ 18 teev, VQ: 3.9 rau h.Table 1.Qhov cuam tshuam ntawm catalyst ntawm cov khoom xaiv

1. Cov nyhuv ntawm cov tshuaj chlorine tshaj tawm ntawm cov tshuaj tiv thaiv

Qhov kev sim pom tias cov tshuaj chlorine tsis zoo muaj cov khoom tsis zoo xaiv, ua kom cov khoom xaiv tau zoo thiab tawm los.

Table 2 teev cov ntaub ntawv xeem.

Table 2 Qhov cuam tshuam ntawm pass-chlorine tshaj tawm ntawm cov khoom xaiv

Test^condition:] Petri phaj 1 acetone, catalyst: composite class 0.6go

Qhov kev sim pom tias cov tshuaj fluchlorine yog ntxov (12 teev) thiab tom qab ntawd (8 24 teev), feem ntau cov tshuaj chlorine khiav tawm uas cov tshuaj tiv thaiv qeeb thiab qhov nruab nrab (28 h) tau nrawm.Thaum cov roj chlorine nres, cov khoom xaiv thiab cov khoom tawm los. raug txo qis.Cov txiaj ntsig tau pom tias 1,1,3 ua tau qeeb qeeb dua

1,1-dichloroacetone.Thaum cov tshuaj tiv thaiv nrog

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

TXC2CCH3

o.

uas yog_II.chlorination ntawm submethyl pawg tau ntau

sai dua ntawm methyl pawg.Yog li ntawd, cov

Tus kws sau ntawv ntseeg tias acetone chloride tiam txheej txheem cov txheej txheem tshuaj tiv thaiv yog:

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

Raws li cov ntaub ntawv Table 2, cov tshuaj tiv thaiv tshaj tawm ntawm txhua kauj ruam yog

　　V2^”3^1 2 5>V4

Nyob ntawm cov tshuaj tiv thaiv ceev ntawm txhua kauj ruam,

Nws tuaj yeem pom los ntawm cov ntaub ntawv ntawm Table 3 uas, vim yog qhov sib txawv me me ntawm qhov sib txawv ntawm 1,1,3.trichloroacetone thiab cov khoom los ntawm cov khoom, feem ntau nyuaj rau kev cais cov dej extraction thiab kev sib cais yog ib qho yooj yim txhais tau tias.Txawm tias feem ntau kuv cov khoom tuaj yeem raug tshem tawm, qhov purity yog qhov nyuaj

peb tswj cov tshuaj chlorine ceev ntawm txhua theem,

kom ua tiav lub hom phiaj ntawm kev txo cov chlorine dhau lub sij hawm thiab inhibiting qhov kev xaiv ntawm kev nce cov tshuaj tiv thaiv theem nrab los ntawm 1,1,3 trichloroacetone..

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

acetone chloride kua yog muab rho tawm los yog refined los ntawm dej kom nce cov ntsiab lus ntawm 1,1,3-trichloroacetone, thiab tus sau siv 1,1,3-trichloroacetone crystallization los ntawm lwm yam khoom los ntawm cov khoom.

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

Table 3.Product purity tau los ntawm kev sib cais sib txawv

txhawm rau txhim kho ntxiv.Product purity ncav cuag ntau dua 99%, thiab cov txiaj ntsig kuj yog qhov siab tshaj plaws hauv ntau txoj kev, mus txog 45% o.1 Txoj kev yuav tsum muaj 1,1,3-trichloroacetone cov ntsiab lus ntawm K ntau tshaj 50% hauv cov tshuaj chloride. daws.

Xaiv cov khoom tsim nyog amine catalyst, tswj cov tshuaj 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 cov khoom siv lead ua tsis muaj tsawg dua 99.0%, nrog yield ntawm 45%, tab sis 1,1,3-trichloroacetone hauv cov tshuaj chloride yuav tsum ntau dua 50% o.Athena CEO

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