Ntawm ib sab tes, qhov kev tsim kho tshiab no muab txoj kev ntxuav 1,1, 3-trichloroacetone, qhov twg txoj kev no muaj cov kauj ruam hauv qab no

Flash:

(1) Cov roj av 1,1, 3-trichloroacetone sib xyaw nrog dej;

(2) Recrystallization ntawm cov tshuaj sab saud tom qab sawv ntsug; Ib yam li ntawd

(3) cov khoom siv lead ua los ntawm cov khoom siv recrystallized raug lim tawm thiab ntxuav nrog dej;

Qhov twg, hauv Kauj Ruam (1), qhov hnyav piv ntawm cov khoom nyoos 1,1, 3-trichloroacetone rau qhov ntau ntawm cov dej yog 10.1-2).

Zoo dua, hauv Kauj Ruam (1), qhov hnyav piv ntawm 1,1, 3-trichloroacetone cov khoom nyoos rau qhov ntau ntawm cov dej tuaj yeem yog 1:

(0.4-0.6), ntxiv rau qhov zoo tshaj plaws li 1:0.5; Hauv kev tsim kho tshiab, qhov ntau npaum li cas ntawm 1,1, 3-trichloroacetone cov khoom nyoos thiab dej raug tswj hwm hauv qhov saum toj no

Qhov ntau ntawm cov purity siab 1,1, 3-trichloroacetone tuaj yeem tau txais.

Raws li qhov kev tsim kho tshiab no, hauv kauj ruam (1), cov khoom siv raw 1,1, 3-trichloroacetone thiab dej tuaj yeem npaj tau ntawm qhov kub ntawm 10-50 ℃

Sib tov rau 10-30 feeb nyob rau hauv cov xwm txheej, thiab tom qab ntawd cia sawv rau 10-30 feeb; Qhov zoo tshaj plaws, hauv Kauj Ruam (1), hais tias 1,1, 3-trichloropropyl

Cov ketone nyoos tau sib xyaw nrog dej ntawm qhov kub ntawm 30-35 ℃ rau 25-30 feeb, thiab tom qab ntawd sawv rau 10-15 feeb; Hauv kev tsim kho tshiab tam sim no

, siv 1,1, 3-trichloroacetone nyoos ua cov khoom siv raw, hauv lub lauj kaub tshuaj tiv thaiv, sib xyaw nrog dej, do ntawm qee qhov kub tom qab sawv ntsug

Kev Ua Kom Tawm. Tom qab ua kom tawm, txheej roj qis dua raug tshem tawm, feem ntau yog los ntawm kev tshem tawm cov tshuaj chlorine ntau thiab tawm hauv cov tshuaj sab saud rau kev siv tom qab.

Raws li qhov kev tsim kho tshiab, hauv kauj ruam (1), cov roj crude 1,1, 3-trichloroacetone yog sib xyaw nrog dej thiab kuj tuaj yeem sib xyaw ua ke.

Cov xwm txheej, uas tsis muaj kev txwv tshwj xeeb rau cov xwm txheej thiab cov khoom siv sib xyaw, tsuav yog 1,1, 3-trichloroacetone tuaj yeem ntxhib

Cov khoom no tuaj yeem sib tov nrog dej kom sib npaug. Qhov zoo tshaj plaws yog tias qhov nrawm sib tov yog 100-300r/min.

Hauv kev tsim kho tshiab no, cov dej zoo dua yog cov dej deionized.

Raws li qhov kev tsim kho tshiab, hauv kauj ruam (2), cov xwm txheej recrystallization yuav yog: kub ntawm 0 txog 35 ℃, lub sijhawm ntawm 0.5 -

10 teev, qhov zoo tshaj plaws, qhov recrystallization yog ua tiav ntawm qhov nrawm ntawm 50-300 RPM; Qhov zoo tshaj plaws, qhov reknot

Dej kuj tseem ntxiv rau hauv cov txheej txheem crystallization, qhov twg cov dej ntxiv rau ntawm tus nqi ntawm 200-600 ml / min; Nyob rau hauv cov xwm txheej no, recrystallization efficiency

Txiv hmab txiv ntoo zoo.

[0034] Ntxiv mus, qhov zoo tshaj plaws, cov xwm txheej recrystallization yog: qhov kub ntawm 10-15 ℃, lub sijhawm ntawm 2-3 teev, thiab cov xwm txheej recrystallization

Cov siv lead ua ke raug do ntawm tus nqi ntawm 100-200 RPM thiab cov dej raug ntxiv ntawm tus nqi ntawm 300-500 ml / feeb.

Nyob rau hauv cov xwm txheej no, qhov recrystallization effect zoo dua.

Hauv kev tsim kho tshiab no, qhov kub ntawm recrystallization piav qhia hauv kauj ruam (2) qis dua li ntawm 1,1, 3-trichloroacetone hauv kauj ruam (1)

Qhov kub uas cov khoom sib xyaw nrog dej.

Raws li qhov kev tsim kho tshiab, hauv Kauj Ruam (3), cov tshuaj sib xyaw tom qab Kauj Ruam (2) tuaj yeem lim tawm los ntawm kev nias kaw, lossis tuaj yeem ua tau

Cov siv lead ua khov kho tau los ntawm kev nias ncaj qha los ntawm lub phaj sieve hauv qab ntawm lub reactor. Hauv kev tsim kho tshiab no, cua thiab/lossis nitrogen zoo dua yog siv.

Kev lim dej siab, nws zoo dua los siv nitrogen rau kev lim dej siab, thiab qhov siab tuaj yeem yog 0.1-0.2MPa, zoo dua 0.12 -

0.18 mpa.

Raws li qhov kev tsim kho tshiab, cov siv lead ua los ntawm cov dej tom qab lim dej siab raug ntxuav nrog dej, qhov twg cov dej hais tau ntxuav

Tsis muaj kev txwv tshwj xeeb, piv txwv li, koj tuaj yeem xaiv 1-2kg ntawm cov dej tsuag ntxuav hauv qab qhov kub ntawm 2-25 ℃, thiab tsuag

Tsis muaj qhov txwv ceev tshwj xeeb.

Raws li qhov kev tsim kho tshiab, qhov huv ntawm cov khoom nyoos 1,1, 3-trichloroacetone yuav yog 50-65% los ntawm qhov hnyav.

Nplooj ntawv 3/6 ntawm cov lus qhia

5

CN 109516908 A

5

Qhov kev tsim kho tshiab no, ntawm qhov tod tes, kuj muab cov folic acid uas tau npaj los ntawm ib qho ntawm cov txheej txheem piav qhia saum toj no.

Ib qho kua dej ntawm 1,1, 3-trichloroacetone yog siv ncaj qha los npaj cov folic acid.

Kev ua haujlwm ntawm txoj kev ntxuav ntawm qhov kev tsim kho tshiab, xws li stratified extraction, crystallization filtration thiab lwm yam, tuaj yeem ua tiav hauv lub kaw lus kaw.

Ib puag ncig-phooj ywg, thiab txo qhov tsim cov dej khib nyiab, tsis muaj cov kuab tshuaj organic pov tseg thiab cov pa roj khib nyiab organic; Tsis tas li ntawd, txoj kev ntxuav kom huv si

Tsis muaj cov organic solvents raug qhia, thiab cov chlorine impurities siab raug tshem tawm thaum lub sijhawm ua kom huv, yog li tsis muaj kev pheej hmoo zoo rau qhov zoo ntawm folic acid.

Txoj kev siv dej ua cov tshuaj crystallization, thiab cov kua dej ntshiab ntawm 1,1, 3-trichloroacetone yog siv ncaj qha rau kev tsim cov folic acid.

Tag nrho cov txiaj ntsig ntawm folic acid tuaj yeem nce ntxiv 5% los ntawm qhov hnyav, thiab qhov huv si yog siab dua 99.2% los ntawm qhov hnyav, uas tuaj yeem tau txais cov khoom zoo

Ua los ntawm folic acid.

Qhov kev tsim kho tshiab tau piav qhia meej los ntawm cov qauv hauv qab no.

[0042] Hauv cov qauv thiab cov feem pua ​​hauv qab no, tshwj tsis yog teev tseg lwm yam, cov ntaub ntawv siv tau los ntawm kev yuav khoom lag luam, tshwj tsis yog teev tseg lwm yam

Txoj kev siv yog txoj kev ib txwm muaj nyob rau hauv daim teb no.

Tus qauv roj chromatography yog GC-2014, yuav los ntawm Shimadzu Company.

Tus 1,1, 3-trichloroacetone npaj los ntawm txoj kev ntxuav ntawm qhov kev tsim kho tshiab no [0047] yog ntxuav hauv lub tshuab hluav taws xob 50-litre uas muaj lub phaj lim dej hauv qab [0048] Ua ntej, qhov huv ntawm 1,1 yog 65% los ntawm qhov hnyav, 3-trichloroacetone 20Kg thiab dej 10Kg hauv lub lauj kaub tshuaj sib xyaw ua ke hauv 24 teev do rau 12 feeb, qhov twg qhov nrawm yog 200r / min, hauv cov txheej txheem do kom ntxiv dej, dej ntawm tus nqi ntawm 300 ml / min, thiab tom qab ntawd cov khoom sib xyaw sawv rau 10 feeb, sib cais los ntawm cov roj txheej qis dua, tshem tawm cov tshuaj chlorine siab; Qhov thib ob, qhov kub ntawm cov kua txheej sab saud tau txo qis rau 5 thiab do rau 2 teev ntawm qhov nrawm ntawm 100r / min. Tom qab ntawd, cov khoom siv lead ua tau txais ncaj qha los ntawm lub phaj sieve hauv qab ntawm lub lauj kaub tshuaj tiv thaiv los ntawm kev lim dej nitrogen ntawm qhov siab ntawm 0.1 MPa, thiab tom qab ntawd txau thiab ntxuav nrog 2 kg dej txias. Qhov hnyav ntub ntawm 1,1, 3-trichloroacetone yog 9.8 kg, thiab cov chromatographic ntshiab (GC) yog 96.8 wt% [0051] Kev ua haujlwm koom nrog hauv txoj kev ntxuav no, xws li kev faib tawm zoo li qub, tshem tawm cov tshuaj chlorine siab, crystallization, lim thiab ntxuav dej, tuaj yeem nqa tawm hauv lub cev kaw, uas yog tus phooj ywg ib puag ncig, thiab txo qis qhov tsim cov dej khib nyiab thiab tsis tsim cov kuab tshuaj organic thiab cov roj khib nyiab organic [0052]. Ntxiv mus, vim tias txoj kev ntxuav tsis tau qhia txog cov kuab tshuaj organic, thiab cov tshuaj chlorine siab kom tshem tawm cov khoom tsis huv hauv cov txheej txheem ntxuav, tsis muaj kev pheej hmoo zoo rau qhov zoo ntawm folic acid, tab sis kuj los ntawm qhov piv txwv ntawm kev npaj 1, 1, 3 - folic acid cross-linked nrog acetone dej yaj ncaj qha siv hauv kev tsim khoom, ua rau folic acid txhim kho tag nrho cov txiaj ntsig 5 qhov hnyav%, qhov huv ntawm 99 5 qhov hnyav% Piv txwv 2 [0054] Qhov kev siv no hais tias 1,1, 3-trichloroacetone npaj los ntawm txoj kev ntxuav ntawm qhov kev tsim kho tam sim no [0055] yog ntxuav hauv 50-litre reactor nruab nrog lub phaj lim dej hauv qab [0056] Ua ntej, 1,1 nrog qhov huv ntawm 50%, 3-trichloroacetone 20Kg thiab dej 4Kg sib xyaw hauv lub reactor, do rau 15 feeb ntawm 45, qhov sib tov ntawm 300r / min, hauv cov txheej txheem sib tov kom ntxiv dej, dej ntawm tus nqi ntawm 300 ml / min, thiab tom qab ntawd qhov sib tov sawv rau 15 feeb, sib cais los ntawm cov roj txheej qis dua, tshem tawm cov tshuaj chlorine siab; Qhov thib ob, qhov kub ntawm cov tshuaj txheej sab saud tom qab stratification tau txo qis rau 20, thiab qhov nrawm yog 200r / min rau 0.5 teev. Tom qab ntawd, cov khoom siv lead ua tau txais ncaj qha los ntawm lub phaj sieve hauv qab ntawm lub reactor los ntawm nitrogen siab lim ntawm qhov siab ntawm 0. 2MPa. Tom qab ntawd, cov khoom siv lead ua tau txau thiab ntxuav nrog 1Kg ntawm 25 dej txias, thiab qhov hnyav ntub ntawm 1,1, 3-trichloroacetone yog 8.2kg los ntawm txoj kev txo qis Txoj kev ntxuav kom huv si uas koom nrog kev tshem tawm cov tshuaj chlorine siab, kev siv lead ua, kev lim dej thiab kev ntxuav dej tuaj yeem ua tiav hauv Lub kaw lus kaw, qhov chaw ua haujlwm zoo, thiab txo qhov tsim cov dej khib nyiab, tsis muaj cov kuab tshuaj organic pov tseg thiab cov roj khib nyiab organic [0060] Tsis tas li ntawd, txij li thaum txoj kev tsis qhia cov kuab tshuaj organic thiab tshem tawm cov tshuaj chlorine siab thaum lub sijhawm ntxuav kom huv si, tsis muaj kev pheej hmoo zoo rau qhov zoo ntawm folic acid, thiab 1,1, 3-trichloroacetone npaj los ntawm Piv txwv 2 yog yaj hauv dej thiab siv ncaj qha rau hauv kev tsim cov folic acid, ua rau tag nrho cov txiaj ntsig ntawm folic acid los ntawm 4.9% los ntawm qhov hnyav thiab ua tiav qhov huv ntawm 99 Qhov kev siv no hais tias 1,1, 3-trichloroacetone npaj los ntawm txoj kev ntxuav ntawm qhov kev tsim kho tam sim no [0063] yog ntxuav hauv 50-litre lub reactor uas muaj lub phaj lim dej hauv qab [0064] Ua ntej, 1,1 nrog qhov huv ntawm 60%, 3-trichloroacetone 20Kg sib xyaw nrog dej 40Kg hauv lub lauj kaub tshuaj tiv thaiv, do rau 30 feeb ntawm 15, qhov nrawm ntawm 100r / min, hauv cov txheej txheem do kom ntxiv dej, dej ntawm tus nqi ntawm 500 ml / min, thiab tom qab ntawd cov khoom sib xyaw sawv rau 30 feeb, sib cais los ntawm cov roj txheej qis dua, tshem tawm cov tshuaj chlorine siab; Qhov thib ob, qhov kub ntawm cov tshuaj txheej sab saud tom qab stratification tau qis dua rau 10, thiab qhov nrawm ntawm 100r / min rau 10 teev. Tom qab ntawd, cov khoom siv lead ua tau txais ncaj qha los ntawm lub phaj lim dej hauv qab ntawm lub reactor los ntawm kev lim dej nitrogen ntawm qhov nrawm ntawm 0.2MPa, thiab tom qab ntawd txau thiab ntxuav nrog 1Kg ntawm 5 dej txias. Qhov hnyav ntub ntawm 1,1, 3-trichloroacetone yog 6.9kg, thiab cov chromatographic ntshiab (GC) yog 98.3% los ntawm qhov hnyav [0067] Kev ua haujlwm koom nrog hauv txoj kev ntxuav no, xws li kev faib tawm zoo li qub, tshem tawm cov chlorine tsis huv siab, crystallization, lim dej thiab ntxuav dej, tuaj yeem nqa tawm hauv lub cev kaw, uas muaj ib puag ncig ua haujlwm zoo, thiab txo qhov tsim cov dej khib nyiab thiab tsis tsim cov kuab tshuaj organic thiab cov roj khib nyiab organic [0068]. Ntxiv mus, vim tias txoj kev ntxuav tsis tau qhia txog cov organic solvent, thiab chlorine siab kom tshem tawm cov khoom tsis huv hauv cov txheej txheem ntxuav, tsis muaj kev pheej hmoo zoo rau qhov zoo ntawm folic acid, thiab yuav piv txwv li 3 kev npaj ntawm 1, 1, 3 - cross-linked nrog acetone, dej kom yaj, siv ncaj qha rau hauv kev tsim cov folic acid, ua rau folic acid los txhim kho tag nrho cov txiaj ntsig 5. 3 qhov hnyav%, qhov huv ntawm 99. 2 qhov hnyav% Rau qhov sib piv 1 [0070] purified 1,1, 3-trichloroacetone raws li txoj kev ntawm embodiment 1, tshwj tsis yog tias hauv kauj ruam (1), dej tsis siv, Hloov chaw, cov organic solvents tau siv. Yog li ntawd, qhov npaj 1,1, 3-trichloroacetone tau yaj hauv dej thiab siv ncaj qha rau hauv kev tsim cov folic acid. Tag nrho cov txiaj ntsig ntawm folic acid tsuas yog nce 2% los ntawm qhov hnyav thiab qhov huv yog 95% los ntawm qhov hnyav. Ntxiv rau, vim yog kev qhia txog cov organic solvents hauv txoj kev ntxuav no, muaj kev pheej hmoo zoo rau qhov zoo ntawm folic acid [0071] hauv qhov sib piv 2 [0072]. 1,1, 3-trichloroacetone raug ntxuav raws li txoj kev hauv Piv txwv 1. Qhov sib txawv yog tias hauv Kauj Ruam (1), qhov ntau ntawm cov dej yog 50Kg, ua rau muaj kev nce ntxiv ntawm cov dej khib nyiab thiab txo qis ntawm 1. Cov txiaj ntsig ntawm 1,1, 3-trichloroacetone crystals tau yaj hauv dej thiab siv ncaj qha rau hauv kev tsim cov folic acid, yog li tag nrho cov txiaj ntsig ntawm folic acid tsuas yog nce ntxiv 5.6% los ntawm qhov hnyav thiab qhov huv si yog 99.6% los ntawm qhov hnyav [0073] tawm tsam qhov sib piv ntawm 3 [0074]. 1,1 tau raug ntxuav los ntawm txoj kev Piv txwv 1, 3-trichloroacetone, qhov sib txawv yog tias hauv kauj ruam (1), cov chlorine heteroplastid siab tsis raug tshem tawm, qhov tshwm sim ntawm kev npaj ntawm 1,1, 3-trichloroacetone muaj ntau cov tshuaj chlorinated, qhov zoo ntawm folic acid pheej hmoo [0075] Raws li qhov piv txwv saum toj no 1-3 thiab yog qhov tshwm sim ntawm qhov ntsuas ntawm 1-3: txoj kev ntxuav suav nrog cia sawv ntsug layered crystal lim kom tshem tawm cov chlorine siab impurities ntxuav kev ua haujlwm xws li txhua yam tab sis hauv lub kaw lus airtight, ib puag ncig ua haujlwm zoo, thiab txo qhov tshwm sim ntawm cov dej khib nyiab, tsis tsim cov roj khib nyiab, cov kuab tshuaj organic thiab cov organic Ntxiv rau, los ntawm kev siv rooj plaub 1 kev npaj ntawm 1, 1), 3-trichloroacetone, ntxiv rau hauv phau ntawv 5/6 nplooj ntawv 7 CN 109516908 A 7 dej kua, siv ncaj qha rau hauv kev tsim cov folic acid, ua rau tag nrho cov txiaj ntsig ntawm folic acid nce 5% los ntawm qhov hnyav, kev huv si yog 99.2% los ntawm qhov hnyav saum toj no; Ntxiv mus, vim tias txoj kev ntxuav tsis qhia txog cov kuab tshuaj organic, tsis muaj kev pheej hmoo zoo rau qhov zoo ntawm folic acid. Ntxiv mus, txoj kev ntxuav siv dej ua cov kuab tshuaj crystallization, thiab cov kua dej huv ntawm 1,1, 3-trichloroacetone yog siv ncaj qha rau hauv kev tsim cov folic acid, txo cov tshuaj tiv thaiv sab.

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