Ntawm qhov tod tes, qhov kev tsim kho tau muab txoj hauv kev ua kom huv ntawm 1,1, 3-trichloroacetone, nyob rau hauv txoj kev muaj cov kauj ruam hauv qab no.

Flash:

(1) Crude 1,1, 3-trichloroacetone tov nrog dej;

(2) Recrystallization ntawm cov tshuaj sab saud tom qab sawv; ib yam li

(3) cov khoom siv recrystallized yog lim tawm thiab ntxuav nrog dej;

Qhov twg, nyob rau hauv Kauj Ruam (1), qhov hnyav piv ntawm cov khoom nyoos hais tias 1,1, 3-trichloroacetone rau cov dej yog 1.0.1-2).

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

(0.4-0.6), ntxiv optimized li 1:0.5; Hauv kev tsim khoom, qhov ntau npaum li cas ntawm 1,1, 3-trichloroacetone crude khoom thiab dej yog tswj nyob rau saum toj no.

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

Raws li qhov kev tsim kho tam sim no, hauv kauj ruam (1), 1,1, 3-trichloroacetone crude khoom 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 ntsug rau 10-30 feeb; Zoo dua, hauv Kauj Ruam (1), hais tias 1,1, 3-trichloropropyl

Cov ketone crude yog tov nrog dej ntawm qhov kub ntawm 30-35 ℃ rau 25-30 feeb, thiab tom qab ntawd sawv ntsug rau 10-15 feeb; Nyob rau hauv lub tam sim no invention

, siv 1,1, 3-trichloroacetone crude li raw khoom, nyob rau hauv cov tshuaj tiv thaiv kettle, tov nrog dej, stirred ntawm ib tug tej yam kub thiab txias tom qab sawv.

Delamination. Tom qab delamination, cov roj txheej qis dua raug tshem tawm, feem ntau yog tshem tawm cov tshuaj chlorine siab thiab tawm hauv cov tshuaj sab saud rau kev siv tom qab.

Raws li qhov kev tsim kho, hauv kauj ruam (1), cov khoom siv raw 1,1, 3-trichloroacetone yog tov nrog dej thiab tuaj yeem sib tov.

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

Cov khoom tuaj yeem sib tov sib xyaw nrog dej. Zoo dua, qhov sib tov yog 100-300r / min.

Nyob rau hauv lub invention tam sim no, cov dej yog nyiam dua deionized dej.

Raws li kev tsim khoom, hauv kauj ruam (2), cov txheej txheem recrystallization yuav yog: kub ntawm 0 txog 35 ℃, lub sij hawm ntawm 0.5 -

10 teev, zoo dua, recrystallization yog nqa tawm ntawm tus nqi stirring ntawm 50-300 RPM; Zoo dua, lub reknot

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

Txiv hmab txiv ntoo zoo.

[0034] Tsis tas li 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 yog nplawm ntawm tus nqi ntawm 100-200 RPM thiab dej ntxiv ntawm tus nqi ntawm 300-500 ml / min.

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

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

Qhov kub ntawm qhov khoom yog tov nrog dej.

Raws li kev tsim, hauv Kauj Ruam (3), cov tshuaj tiv thaiv sib tov tom qab Kauj Ruam (2) tuaj yeem lim tawm los ntawm kev kaw lub siab, lossis tuaj yeem ua tau.

Cov khoom siv lead ua yog tau los ntawm nias ncaj qha los ntawm lub sieve phaj nyob rau hauv qab ntawm lub reactor. Hauv kev tsim khoom tam sim no, huab cua thiab / lossis nitrogen zoo dua yog siv

Lub siab pom, nws yog qhov zoo dua los siv nitrogen rau siab pom, thiab lub siab tuaj yeem yog 0.1-0.2MPa, nyiam dua 0.12 -

0.18mp ua.

Raws li qhov kev tsim kho, cov khoom siv lead ua precipitated tom qab siab pom yog ntxuav nrog dej, nyob rau hauv cov dej hais tias yog ntxuav.

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

Tsis muaj kev txwv ceev.

Raws li kev tsim khoom, purity ntawm 1,1, 3-trichloroacetone crude khoom yuav yog 50-65% los ntawm qhov hnyav.

Nplooj 3/6 ntawm kev qhia

5

CN 109516908 A

5

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

Cov tshuaj aqueous ntawm 1,1, 3-trichloroacetone yog siv ncaj qha los npaj folic acid.

Kev ua haujlwm ntawm purification txoj kev tsim, xws li stratified extraction, crystallization filtration thiab lwm yam, tuaj yeem nqa tawm hauv lub kaw lus kaw.

Ib puag ncig-phooj ywg, thiab txo qis kev tsim cov dej pov tseg, tsis muaj cov kuab tshuaj organic pov tseg thiab cov pa roj organic pov tseg; Tsis tas li ntawd, txoj kev purification

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

Txoj kev siv dej ua cov kuab tshuaj crystallization, thiab cov kua dej huv huv 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 los ntawm 5% los ntawm qhov hnyav, thiab purity siab dua 99.2% los ntawm qhov hnyav, uas tuaj yeem tau txais txiaj ntsig zoo.

Ntawm folic acid.

Lub invention yog piav nyob rau hauv kom meej los ntawm txoj kev ntawm embodiments hauv qab no.

[0042] Nyob rau hauv cov nram qab no embodiments thiab proportions, tshwj tsis yog tias muaj lwm yam teev, cov ntaub ntawv uas siv yog muaj nyob rau hauv kev muag khoom, tshwj tsis yog hais tias lwm yam.

Txoj kev siv yog txoj kev paib nyob rau hauv daim teb no.

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

Lub 1,1, 3-trichloroacetone npaj los ntawm purification txoj kev tam sim no invention [0047] yog purified nyob rau hauv ib tug 50-liter reactor nruab nrog ib tug lim sieve phaj nyob rau hauv qab [0048] Ua ntej, lub purity ntawm 1,1 yog 65. % los ntawm qhov hnyav, 3-trichloroacetone 20Kg thiab dej 10Kg nyob rau hauv cov tshuaj tiv thaiv kettle tov nyob rau hauv 24 stirring rau 12 feeb, qhov stirring tus nqi yog 200r / min, nyob rau hauv lub stirring txheej txheem ntxiv dej, dej ntawm tus nqi ntawm 300 ml / min. , thiab tom qab ntawd cov sib tov sawv ntsug rau 10 feeb, sib cais los ntawm qis roj txheej, tshem tawm cov tshuaj chlorine siab; Qhov thib ob, qhov kub ntawm cov txheej txheej saum toj kawg nkaus tau txo qis mus rau 5 thiab nplawm rau 2 teev ntawm qhov sib tov ntawm 100r / min. Tom qab ntawd, cov khoom siv lead ua tau ncaj qha los ntawm lub sieve phaj nyob rau hauv qab ntawm cov tshuaj tiv thaiv kettle los ntawm nitrogen siab pom ntawm ib tug siab ntawm 0.1 MPa, thiab ces sprayed thiab ntxuav nrog 2 kg dej txias. Qhov hnyav ntub dej ntawm 1,1, 3-trichloroacetone yog 9.8 kg, thiab chromatographic ntshiab (GC) yog 96.8 wt % [0051] Kev ua haujlwm koom nrog hauv txoj kev purification no, xws li static stratification, tshem tawm cov tshuaj chlorine siab impurities, crystallization, Kev lim dej thiab ntxuav dej, tuaj yeem nqa tawm hauv lub cev kaw, uas yog ib puag ncig tus phooj ywg, thiab txo qis kev tsim cov dej khib nyiab thiab tsis tsim cov kuab tshuaj pov tseg thiab cov organic pov tseg [0052]. Tsis tas li ntawd, vim tias txoj kev purification yam tsis tau qhia cov kuab tshuaj organic, thiab cov tshuaj chlorine siab kom tshem tawm cov impurities hauv cov txheej txheem purification, tsis muaj kev pheej hmoo ntawm folic acid zoo, tab sis kuj los ntawm kev ua piv txwv ntawm kev npaj ntawm 1, 1, 3 - folic acid hla kev txuas nrog acetone dej yaj ncaj qha siv hauv kev tsim khoom, ua rau folic acid txhim kho tag nrho cov txiaj ntsig 5 %, qhov purity ntawm 99 5 qhov hnyav % Piv txwv 2 [0054] Qhov no embodiment hais tias 1,1, 3-trichloroacetone npaj los ntawm purification txoj kev tam sim no invention [0055] yog purified nyob rau hauv 50-litre reactor nruab nrog lub lim sieve phaj nyob rau hauv qab [0056] Ua ntej,1,1 nrog ib tug purity ntawm 50%, 3-trichloroacetone 20Kg thiab dej 4Kg tov. nyob rau hauv lub reactor, stirring rau 15 feeb ntawm 45, stirring tus nqi ntawm 300r / min, nyob rau hauv lub stirring txheej txheem ntxiv dej, dej ntawm tus nqi ntawm 300 ml / min, thiab ces cov sib tov sawv ntsug rau 15 feeb, sib cais los ntawm cov dej. qis roj txheej, tshem tawm cov tshuaj chlorine siab; Qhov thib ob, qhov kub ntawm cov txheej txheej sab saud tom qab stratification tau qis dua mus rau 20, thiab tus nqi nplawm yog 200r / min rau 0.5 h. Tom qab ntawd, cov khoom siv lead ua tau ncaj qha los ntawm lub sieve phaj hauv qab ntawm lub reactor los ntawm nitrogen siab pom ntawm lub siab ntawm 0. 2MPa. Tom qab ntawd, cov khoom siv lead ua tau txau thiab ntxuav nrog 1Kg ntawm 25 dej txias, thiab ntub dej hnyav ntawm 1,1, 3-trichloroacetone yog 8.2kg los ntawm txoj kev txo cov purification txoj kev koom tes hauv cov static stratification tshem tawm cov chlorine impurities siab, crystallization, pom thiab dej ntxuav dej ua haujlwm tuaj yeem ua tiav hauv Lub cev kaw, qhov chaw ua haujlwm yog tus phooj ywg, thiab txo qis kev tsim cov dej khib nyiab, tsis muaj pov tseg cov kuab tshuaj organic thiab cov organic pov tseg [0060] Tsis tas li ntawd, txij li txoj kev ua. tsis qhia cov kuab tshuaj organic thiab tshem tawm cov tshuaj chlorine siab thaum lub sijhawm ua kom huv, tsis muaj kev pheej hmoo 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, nce tag nrho cov txiaj ntsig ntawm folic acid los ntawm 4.9% los ntawm qhov hnyav thiab ua tiav purity ntawm 99 Qhov no embodiment hais tias 1,1, 3-trichloroacetone npaj los ntawm purification txoj kev ntawm tam sim no invention [0063] yog purified nyob rau hauv ib tug 50. -litre reactor haum nrog lub lim sieve phaj rau hauv qab [0064] Ua ntej, 1,1 nrog purity ntawm 60%, 3-trichloroacetone 20Kg tov nrog dej 40Kg nyob rau hauv cov tshuaj tiv thaiv kettle, stirring rau 30 feeb ntawm 15, tus nqi stirring ntawm 100r / min, hauv cov txheej txheem nplawm kom ntxiv dej, dej ntawm tus nqi ntawm 500 ml / min, thiab tom qab ntawd cov sib tov sawv ntsug rau 30 feeb, sib cais los ntawm cov roj qis, tshem tawm cov tshuaj chlorine siab; Qhov thib ob, qhov kub ntawm cov txheej txheej sab saud tom qab stratification tau qis dua mus rau 10, thiab tus nqi nplawm yog 100r / min rau 10 teev. Tom qab ntawd, cov khoom siv lead ua tau ncaj qha los ntawm lub sieve phaj nyob rau hauv qab ntawm lub reactor los ntawm nitrogen siab pom ntawm lub siab ntawm 0.2MPa, thiab ces sprayed 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 purification no, xws li static stratification, tshem tawm cov tshuaj chlorine siab impurities, crystallization. , lim dej thiab ntxuav dej, tuaj yeem nqa tawm hauv lub cev kaw, uas muaj qhov chaw ua haujlwm zoo, thiab txo qis kev tsim cov dej khib nyiab thiab tsis tsim cov kuab tshuaj pov tseg thiab cov organic pov tseg [0068]. Tsis tas li ntawd, vim hais tias txoj kev purification yam tsis tau qhia cov kuab tshuaj organic, thiab cov tshuaj chlorine siab kom tshem tawm cov impurities hauv cov txheej txheem purification, tsis muaj kev pheej hmoo ntawm folic acid zoo, thiab yuav ua piv txwv 3 kev npaj ntawm 1, 1, 3 - cross- txuas nrog acetone, dej kom yaj, ncaj qha siv nyob rau hauv zus tau tej cov folic acid, ua folic acid los txhim kho tag nrho cov yield 5. 3 nyhav %, lub purity ntawm 99. 2 nyhav % Rau feem 1 [0070] purified 1,1, 3- trichloroacetone raws li tus qauv ntawm embodiment 1, tshwj tsis yog tias nyob rau hauv kauj ruam (1), dej tsis siv, Xwb, organic solvents tau siv. Yog li ntawd, cov 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 los ntawm 2% los ntawm qhov hnyav thiab qhov purity yog 95% los ntawm qhov hnyav. Tsis tas li ntawd, vim yog kev qhia txog cov kuab tshuaj organic hauv txoj kev ua kom huv no, muaj kev pheej hmoo zoo rau qhov zoo ntawm folic acid [0071] hauv kev faib ua feem 2 [0072]. 1,1, 3-trichloroacetone yog purified raws li txoj kev hauv Piv txwv 1. Qhov txawv yog tias nyob rau hauv Kauj Ruam (1), tus nqi ntawm cov dej yog 50Kg, uas ua rau muaj kev loj hlob ntawm kev tsim cov dej khib nyiab thiab txo qis ntawm 1 Cov. 1,1, 3-trichloroacetone crystals yog yaj nyob rau hauv dej thiab ncaj qha siv nyob rau hauv zus tau tej cov folic acid, thiaj li hais tias tag nrho cov yield ntawm folic acid tsuas yog nce los ntawm 5.6% los ntawm qhov hnyav thiab purity yog 99.6% los ntawm qhov hnyav [0073] ] tawm tsam qhov piv ntawm 3 [0074]. 1,1 raug ntxuav los ntawm txoj kev piv txwv 1, 3-trichloroacetone, qhov sib txawv yog tias nyob rau hauv kauj ruam (1), lub siab chlorine heteroplastid tsis raug tshem tawm, qhov tshwm sim ntawm kev npaj ntawm 1,1, 3-trichloroacetone muaj ib tug loj. Tus naj npawb ntawm cov tshuaj chlorinated, qhov zoo ntawm folic acid txaus ntshai [0075] Raws li cov piv txwv saum toj no 1-3 thiab yog qhov tshwm sim ntawm qhov ntsuas ntawm 1-3: txoj kev purification yuav tsum cia sawv ntsug txheej siv lead ua lim kom tshem tawm cov tshuaj chlorine siab impurities ntxuav ua haujlwm. xws li tag nrho tab sis nyob rau hauv lub airtight system, tus phooj ywg ua hauj lwm ib puag ncig, thiab zoo heev txo qhov tshwm sim ntawm cov dej khib nyiab, tsis tsim cov pa khib nyiab, organic solvent thiab organic ntxiv, los ntawm kev siv rooj plaub 1 kev npaj ntawm 1, 1), 3-trichloroacetone. , ntxiv nyob rau hauv phau ntawv 5/6 nplooj 7 CN 109516908 A 7 dej tov, ncaj qha siv nyob rau hauv zus tau tej cov folic acid, ua kom tag nrho cov tawm los ntawm folic acid nce 5% los ntawm qhov hnyav, purity yog 99.2% los ntawm qhov hnyav saum toj no; Ntxiv mus, vim hais tias txoj kev purification tsis qhia cov organic hnyav, tsis muaj kev pheej hmoo rau qhov zoo ntawm folic acid. Ntxiv mus, txoj kev purification siv dej raws li cov kuab tshuaj crystallization, thiab purified aqueous tov ntawm 1,1, 3-trichloroacetone ncaj qha siv nyob rau hauv zus tau tej cov folic acid, txo cov sab kev xav.

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