Kumbali imodzi, chipangizochi chimapereka njira yoyeretsera ya 1,1, 3-trichloroacetone, pomwe njirayo ili ndi magawo otsatirawa.

Kuwala:

(1) Chosaphika cha 1,1, 3-trichloroacetone chosakanizidwa ndi madzi;

(2) Kubwezeretsanso kwa yankho lapamwamba pambuyo poyima; Komanso

(3) makhiristo olimba omwe amapangidwanso amasefedwa ndikutsukidwa ndi madzi;

Pamene, mu Gawo (1), chiŵerengero cha kulemera kwa 1,1, 3-trichloroacetone yosakanizidwa ndi kuchuluka kwa madzi ndi 10.1-2).

Makamaka, mu Gawo (1), chiŵerengero cha kulemera kwa chinthu chosaphikidwa cha 1,1, 3-trichloroacetone ndi kuchuluka kwa madzi chikhoza kukhala 1:

(0.4-0.6), yowonjezeredwa kukhala 1:0.5; Mu chipangizochi, mlingo wa 1,1, 3-trichloroacetone crude product ndi madzi umayendetsedwa pamwambapa.

Mtundu wa kuyera kwambiri kwa 1,1, 3-trichloroacetone ungapezeke.

Malinga ndi zomwe zapangidwa pano, mu gawo (1), chinthu chosaphikidwa cha 1, 1, 3-trichloroacetone ndi madzi zitha kukonzedwa pa kutentha kwa 10-50℃

Sakanizani kwa mphindi 10-30 motsatira zomwe zili mu bukhuli, kenako musiyeni kwa mphindi 10-30; Makamaka, mu Gawo (1), anati 1,1, 3-trichloropropyl

Ketone wosakanizidwa unasakanizidwa ndi madzi pa kutentha kwa 30-35℃ kwa mphindi 25-30, kenako unayima kwa mphindi 10-15; Mu chipangizochi chomwe chapangidwa pano

, pogwiritsa ntchito 1, 1, 3-trichloroacetone crude ngati zinthu zopangira, mu ketulo yoyankhira, yosakanizidwa ndi madzi, yosunthidwa pa kutentha kwina pambuyo poyimirira

Delamination: Pambuyo pa delamination, mafuta otsika amachotsedwa, makamaka pochotsa zinyalala zambiri za chlorine ndikusiya yankho lapamwamba kuti ligwiritsidwe ntchito mtsogolo.

Malinga ndi luso limeneli, mu gawo (1), 1, 3-trichloroacetone yosaphwanyidwa imasakanizidwa ndi madzi ndipo imatha kusunthidwanso.

Mikhalidwe, momwe mulibe malire enieni pa mikhalidwe yosakaniza ndi zida, bola ngati 1,1, 3-trichloroacetone ingakhale yolimba

Chogulitsacho chingasakanizidwe mofanana ndi madzi. Ndibwino kuti chiŵerengero cha kusakaniza chikhale 100-300r/min.

Mu chipangizochi, madzi ndi abwino kwambiri kukhala opanda ayoni.

Malinga ndi zomwe zapangidwazi, mu gawo (2), mikhalidwe yobwezeretsanso mphamvu ya crystallization ikhoza kukhala: kutentha kuyambira 0 mpaka 35℃, nthawi kuyambira 0.5 -

Kwa maola 10, makamaka, recrystallization imachitika pa liwiro losakaniza la 50-300 RPM; makamaka, reknot

Madzi amawonjezedwanso mu njira yopangira makristalo, pomwe madzi amawonjezedwa pamlingo wa 200-600 ml/min; Pansi pa izi, mphamvu yobwezeretsanso makristalo

Zipatso ndi zabwino.

[0034] Kuphatikiza apo, mikhalidwe yobwezeretsanso ndi iyi: kutentha kwa 10-15℃, nthawi ya maola 2-3, ndi mikhalidwe yobwezeretsanso.

Khiristo imasakanizidwa pa liwiro la 100-200 RPM ndipo madzi amawonjezedwa pa liwiro la 300-500 ml/min.

Pansi pa izi, mphamvu ya recrystallization imakhala yabwino.

Mu chipangizochi, kutentha kwa recrystallization komwe kwafotokozedwa mu gawo (2) ndi kotsika kuposa kwa 1,1, 3-trichloroacetone mu gawo (1)

Kutentha komwe mankhwalawa amasakanizidwa ndi madzi.

Malinga ndi luso lamakonoli, mu Gawo (3), chisakanizo cha reaction pambuyo pa Gawo (2) chikhoza kusefedwa ndi kukakamizidwa kotsekedwa, kapena chikhoza kusinthidwa

Makristalo olimba amapezeka pokanikiza mwachindunji kudzera mu mbale ya sieve pansi pa reactor. Mu chipangizochi, mpweya ndi/kapena nayitrogeni zimagwiritsidwa ntchito bwino.

Kusefa kwa kupanikizika, ndi bwino kugwiritsa ntchito nayitrogeni posefa kupanikizika, ndipo kupanikizika kungakhale 0.1-0.2MPa, makamaka 0.12 -

0. 18 mpa.

Malinga ndi luso limeneli, kristalo wothira madzi pambuyo poyeretsedwa amatsukidwa ndi madzi, momwe madziwo amatsukidwa.

Palibe malire enieni, mwachitsanzo, mutha kusankha 1-2kg ya kutsuka ndi madzi ngati kutentha kuli pakati pa 2-25℃, ndikupopera.

Palibe malire enieni a liwiro.

Malinga ndi luso lamakonoli, kuyera kwa chinthu chosaphikidwa cha 1,1, 3-trichloroacetone kungakhale 50-65% polemera.

Masamba 3/6 a malangizo

5

CN 109516908 A

5

Komano, njira yatsopanoyi imaperekanso folic acid yomwe imapangidwa pogwiritsa ntchito njira iliyonse yomwe yafotokozedwa pamwambapa.

Yankho lamadzi la 1,1, 3-trichloroacetone limagwiritsidwa ntchito mwachindunji pokonzekera folic acid.

Kugwira ntchito kwa njira yoyeretsera ya chipangizochi, monga kuchotsa zinthu mosiyanasiyana, kusefa kwa makristalo ndi zina zotero, kumatha kuchitika mu dongosolo lotsekedwa.

Yosamalira chilengedwe, ndipo imachepetsa kwambiri kupanga madzi otayira, palibe zosungunulira zachilengedwe ndi mpweya wotayira zachilengedwe; Kuphatikiza apo, njira yoyeretsera

Palibe zinthu zosungunulira zachilengedwe zomwe zimalowetsedwa, ndipo zinyalala zambiri za chlorine zimachotsedwa panthawi yoyeretsa, kotero palibe chiopsezo cha mtundu wa folic acid.

Njirayi imagwiritsa ntchito madzi ngati chosungunulira makristalo, ndipo yankho lamadzi loyeretsedwa la 1,1, 3-trichloroacetone limagwiritsidwa ntchito mwachindunji popanga folic acid.

Kuchuluka kwa folic acid kumatha kuwonjezeka ndi 5%, ndipo kuyera kwake kuli pamwamba pa 99.2%, zomwe zimapangitsa kuti munthu akhale ndi khalidwe labwino.

Ya folic acid.

Kupangidwaku kwafotokozedwa mwatsatanetsatane pogwiritsa ntchito njira zomwe zili pansipa.

[0042] Mu njira zotsatirazi ndi kuchuluka kwake, pokhapokha ngati zanenedwa mwanjira ina, zipangizo zomwe zagwiritsidwa ntchito zimapezeka kudzera mu kugula kwamalonda, pokhapokha ngati zanenedwa mwanjira ina

Njira yomwe imagwiritsidwa ntchito ndi njira yachikhalidwe m'munda uno.

Chitsanzo cha gasi chromatography chinali GC-2014, chogulidwa ku Shimadzu Company.

1,1, 3-trichloroacetone yokonzedwa pogwiritsa ntchito njira yoyeretsera ya chipangizochi [0047] imayeretsedwa mu reactor ya malita 50 yokhala ndi mbale yosefera pansi [0048] Choyamba, kuyera kwa 1,1 ndi 65% polemera, 3-trichloroacetone 20Kg ndi madzi 10Kg mu ketulo yoyamwa, yosakaniza mu 24 kusakaniza kwa mphindi 12, pomwe kusakaniza kuli 200r/min, mu njira yosakaniza kuti muwonjezere madzi, madziwo pa liwiro la 300 ml/min, kenako kusakanizako kunayima kwa mphindi 10, kolekanitsidwa ndi mafuta otsika, kuchotsa zonyansa zambiri za chlorine; Kachiwiri, kutentha kwa yankho lapamwamba lokhala ndi zigawo kunachepetsedwa kufika pa 5 ndikusakanikirana kwa maola awiri pa liwiro losakaniza la 100r/min. Kenako, kristalo wolimba unapezedwa mwachindunji kudzera mu sieve plate yomwe ili pansi pa ketulo yoyankhira pogwiritsa ntchito nitrogen pressure filtration pa 0.1 MPa, kenako unapopera ndikutsukidwa ndi madzi ozizira a 2 kg. Kulemera konyowa kwa 1,1, 3-trichloroacetone kunali 9.8 kg, ndipo chromatographic pure (GC) inali 96.8 wt % [0051]. Ntchito yomwe ikugwiritsidwa ntchito mu njira yoyeretsera iyi, monga static stratification, kuchotsa zinyalala zambiri za chlorine, crystallization, sefa ndi kutsuka madzi, ikhoza kuchitika mu thupi lotsekedwa, lomwe ndi losamala zachilengedwe, ndipo limachepetsa kwambiri kupanga madzi otayika ndipo silipanga zinyalala za organic solvent ndi organic waste gas [0052]. Kuphatikiza apo, chifukwa njira yoyeretsera popanda kuyambitsa zosungunulira zachilengedwe, komanso chlorine wambiri kuti achotse zinyalala mu njira yoyeretsera, palibe chiopsezo cha mtundu wa folic acid, komanso ndi chitsanzo chokhazikitsa kukonzekera kwa 1, 1, 3 - folic acid yolumikizidwa ndi acetone madzi osungunuka omwe amagwiritsidwa ntchito mwachindunji popanga, imapangitsa folic acid kukweza zokolola zonse 5 kulemera %, chiyero cha 99 5 kulemera % Chitsanzo 2 [0054] Njira iyi imati 1,1, 3-trichloroacetone yokonzedwa ndi njira yoyeretsera ya chipangizochi [0055] imayeretsedwa mu reactor ya malita 50 yokhala ndi mbale yosefera pansi [0056] Choyamba, 1,1 yokhala ndi chiyero cha 50%, 3-trichloroacetone 20Kg ndi madzi 4Kg osakanikirana mu reactor, kusakaniza kwa mphindi 15 pa 45, mlingo wosakaniza wa 300r/min, mu njira yosakaniza kuti muwonjezere madzi, madzi pamlingo wa 300 ml /min, kenako Chosakanizacho chinaima kwa mphindi 15, cholekanitsidwa ndi mafuta otsika, chotsani zonyansa zambiri za chlorine; Kachiwiri, kutentha kwa yankho la pamwamba pambuyo pa kugawa kunachepetsedwa kufika pa 20, ndipo liwiro losakaniza linali 200r/min kwa maola 0.5. Kenako, kristalo wolimba unapezedwa mwachindunji kudzera mu mbale ya sieve pansi pa reactor poyesa kusefa kwa nayitrogeni pa kuthamanga kwa 0.2MPa. Kenako, kristalo wolimba unathiridwa ndi kutsukidwa ndi 1Kg ya madzi ozizira 25, ndipo kulemera konyowa kwa 1,1, 3-trichloroacetone kunali 8.2kg pogwiritsa ntchito njira yochepetsera. Njira yoyeretsera yomwe ikukhudzidwa ndi kugawa kwa static stratification kuchotsa zonyansa zambiri za chlorine, crystallization, sefa ndi ntchito zotsuka madzi zitha kuchitika mu dongosolo lotsekedwa la thupi, malo ogwirira ntchito ndi abwino, ndipo amachepetsa kwambiri kupanga madzi otayira, palibe zosungunulira zachilengedwe ndi mpweya wotayira zachilengedwe [0060]. Kuphatikiza apo, popeza njirayo siyiyambitsa zosungunulira zachilengedwe ndikuchotsa zonyansa zambiri za chlorine panthawi yoyeretsera, palibe chiopsezo cha mtundu wa folic acid, ndipo 1,1, 3-trichloroacetone yokonzedwa ndi Chitsanzo 2 imasungunuka m'madzi ndikugwiritsidwa ntchito mwachindunji popanga folic acid, kuonjezera kuchuluka kwa folic acid ndi 4.9% ndi kulemera ndikupeza chiyero cha 99. Njira iyi imati 1,1, 3-trichloroacetone yokonzedwa ndi njira yoyeretsera ya chipangizochi [0063] imayeretsedwa mu lita 50. Choyatsiracho chili ndi mbale yoyeretsera fyuluta pansi [0064] Choyamba, 1,1 yokhala ndi chiyero cha 60%, 3-trichloroacetone 20Kg yosakaniza ndi madzi 40Kg mu ketulo yoyeretsera, kusakaniza kwa mphindi 30 pa 15, kuchuluka kwa kusakaniza kwa 100r/min, mu ndondomeko yosakaniza kuti muwonjezere madzi, madziwo pa mlingo wa 500 ml/min, kenako chisakanizocho chinaima kwa mphindi 30, cholekanitsidwa ndi gawo lotsika la mafuta, kuchotsa zonyansa zambiri za chlorine; Kachiwiri, kutentha kwa yankho la gawo lapamwamba pambuyo pa kugawa kunachepetsedwa kufika pa 10, ndipo kuchuluka kwa kusakaniza kunali 100r/min kwa maola 10. Kenako, kristalo wolimba unapezedwa mwachindunji kudzera mu mbale yoyeretsera pansi pa choyatsiracho ndi kusefa kwa nayitrogeni pa kuthamanga kwa 0.2MPa, kenako kupopera ndikutsukidwa ndi 1Kg ya madzi ozizira 5. Kulemera konyowa kwa 1,1, 3-trichloroacetone kunali 6.9kg, ndipo chromatographic pure (GC) inali 98.3% polemera [0067]. Ntchito yomwe ikugwiridwa mu njira yoyeretserayi, monga kugawa kwa static, kuchotsa zinyalala zambiri za chlorine, crystallization, kusefa ndi kutsuka madzi, ikhoza kuchitika m'thupi lotsekedwa, lomwe lili ndi malo ogwirira ntchito abwino, ndipo limachepetsa kwambiri kupanga madzi otayika ndipo silipanga zinyalala za organic solvent ndi mpweya wa organic zinyalala [0068]. Kuphatikiza apo, chifukwa njira yoyeretsera popanda kuyambitsa zosungunulira zachilengedwe, komanso chlorine yambiri kuti ichotse zinyalala mu njira yoyeretsera, palibe chiopsezo cha mtundu wa folic acid, ndipo mwachitsanzo, idzakhala yokonzekera 3 ya 1, 1, 3 - yolumikizidwa ndi acetone, madzi osungunuka, omwe amagwiritsidwa ntchito mwachindunji popanga folic acid, amapangitsa folic acid kukweza zokolola zonse 5.3 kulemera %, chiyero cha 99.2 kulemera % Pa chiŵerengero 1 [0070] choyeretsera 1,1, 3-trichloroacetone malinga ndi njira yogwiritsira ntchito 1, kupatula kuti mu gawo (1), madzi sagwiritsidwa ntchito, M'malo mwake, zosungunulira zachilengedwe zinagwiritsidwa ntchito. Zotsatira zake, 1,1, 3-trichloroacetone yokonzedwayo inasungunuka m'madzi ndipo inagwiritsidwa ntchito mwachindunji popanga folic acid. Kuchuluka kwa folic acid konse kunawonjezeka ndi 2% polemera ndipo chiyero chinali 95% polemera. Kuphatikiza apo, chifukwa cha kuyambitsidwa kwa zinthu zosungunulira zachilengedwe mu njira yoyeretsera iyi, pali chiopsezo cha khalidwe la folic acid [0071] poyerekeza ndi 2 [0072]. 1,1, 3-trichloroacetone imayeretsedwa malinga ndi njira yomwe ili mu Chitsanzo 1. Kusiyana kwake ndikuti mu Gawo (1), kuchuluka kwa madzi ndi 50Kg, zomwe zimapangitsa kuti pakhale kuwonjezeka kwakukulu kwa kupanga madzi otayira komanso kuchepa kwa 1. Kuchuluka kwa makhiristo a 1,1, 3-trichloroacetone kunasungunuka m'madzi ndikugwiritsidwa ntchito mwachindunji popanga folic acid, kotero kuti kuchuluka konse kwa folic acid kunangowonjezeka ndi 5.6% polemera ndipo chiyero chinali 99.6% polemera [0073] motsutsana ndi chiŵerengero cha 3 [0074]. 1,1 idayeretsedwa pogwiritsa ntchito njira ya Chitsanzo 1, 3-trichloroacetone, kusiyana kwake ndikuti mu gawo (1), heteroplastid ya chlorine yambiri siichotsedwa, zotsatira za kukonzekera kwa 1,1, 3-trichloroacetone zili ndi mankhwala ambiri a chlorine, mtundu wa chiopsezo cha folic acid [0075] Malinga ndi chitsanzo chapamwambachi 1-3 ndipo ndi zotsatira za sikelo ya 1-3: njira yoyeretsera imaphatikizapo kulola kuti kristalo iume yosalala kuti ichotse zinyalala zambiri za chlorine ntchito zotsuka monga zonse koma mu dongosolo lopanda mpweya, malo ogwirira ntchito abwino, komanso kuchepetsa kwambiri kuchuluka kwa madzi otayika, sikupanga mpweya wotayira, zosungunulira zachilengedwe ndi zachilengedwe. Kuphatikiza apo, pokhazikitsa chitsanzo 1 kukonzekera kwa 1, 1), 3-trichloroacetone, onjezani m'buku 5/6 tsamba 7 CN 109516908 Yankho la madzi 7, lomwe limagwiritsidwa ntchito mwachindunji popanga folic acid, limapangitsa kuti phindu lonse la folic acid liwonjezeke ndi 5% polemera, chiyero ndi 99.2% polemera pamwambapa; Komanso, chifukwa njira yoyeretsera siyambitsa zosungunulira zachilengedwe, palibe chiopsezo cha mtundu wa folic acid. Komanso, njira yoyeretsera imagwiritsa ntchito madzi ngati chosungunulira cha crystallization, ndipo yankho lamadzi loyeretsedwa la 1,1, 3-trichloroacetone limagwiritsidwa ntchito mwachindunji popanga folic acid, kuchepetsa zotsatira zoyipa.

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