Kumbali imodzi, kupangidwaku kumapereka njira yoyeretsera ya 1,1, 3-trichloroacetone, momwe njirayo ili ndi njira zotsatirazi.

Kung'anima:

(1) 1,1, 3-trichloroacetone wosakanizidwa ndi madzi;

(2) Recrystallization chapamwamba njira atayima; Komanso

(3) makhiristo olimba opangidwanso amasefedwa ndikutsukidwa ndi madzi;

Momwe, mu Gawo (1), chiŵerengero cha kulemera kwa 1,1, 3-trichloroacetone yomwe yanenedwa ku kuchuluka kwa madzi ndi 1.0.1-2).

Makamaka, mu Gawo (1), kulemera kwa 1,1, 3-trichloroacetone crude product ku kuchuluka kwa madzi kungakhale 1:

(0.4-0.6), kukonzedwanso ngati 1: 0.5; Popanga, mlingo wa 1,1, 3-trichloroacetone crude product ndi madzi umayendetsedwa pamwambapa.

Mitundu yambiri yoyera 1,1, 3-trichloroacetone imatha kupezeka.

Malinga ndi zomwe zapezedwa pano, mu sitepe (1), 1,1, 3-trichloroacetone crude product ndi madzi zitha kukonzedwa pa kutentha kwa 10-50 ℃

Sakanizani kwa mphindi 10-30 pansi pa zikhalidwe, ndiyeno muyime kwa mphindi 10-30; Makamaka, mu Gawo (1), anati 1,1, 3-trichloropropyl

Ketone yaiwisi imasakanizidwa ndi madzi pa kutentha kwa 30-35 ℃ kwa mphindi 25-30, kenako inayima kwa mphindi 10-15; M'zinthu zamakono

, pogwiritsa ntchito 1,1, 3-trichloroacetone crude monga zopangira, mu ketulo anachita, wothira madzi, wosonkhezeredwa ndi kutentha kwina atayima.

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

Malingana ndi kupangidwa, mu sitepe (1), 1,1, 3-trichloroacetone yosakanizidwa ndi madzi ndipo imathanso kugwedezeka.

Mikhalidwe, yomwe palibe malire enieni pazochitika zolimbikitsa ndi zida, bola ngati 1,1, 3-trichloroacetone ikhoza kukhala yovuta.

Mankhwalawa akhoza kusakanikirana mofanana ndi madzi. Makamaka, mlingo wosakanikirana ndi 100-300r / min.

Masiku ano, madziwo ndi madzi opangidwa ndi deionized.

Malinga ndi kupangidwa, mu sitepe (2), zinthu recrystallization akhoza kukhala: kutentha kuchokera 0 mpaka 35 ℃, nthawi kuchokera 0.5 -

Maola 10, makamaka, recrystallization ikuchitika pa mlingo wolimbikitsa wa 50-300 RPM; Makamaka, reknot

Madzi amawonjezeredwa mu ndondomeko ya crystallization, momwe madzi amawonjezeredwa pa mlingo wa 200-600 ml / min; Pazimenezi, recrystallization dzuwa

Chipatso ndi chabwino.

[0034] Kupitilira apo, mawonekedwe a recrystallization ndi: kutentha kwa 10-15 ℃, nthawi ya maola 2-3, ndi mikhalidwe yokonzanso.

Crystal imagwedezeka pa mlingo wa 100-200 RPM ndipo madzi amawonjezeredwa pa mlingo wa 300-500 ml / min.

Pazifukwa izi, recrystallization zotsatira ndi bwino.

Pakupangidwa kwamakono, kutentha kwa recrystallization komwe kufotokozedwa mu sitepe (2) ndikotsika kuposa kwa 1,1, 3-trichloroacetone mu sitepe (1)

Kutentha komwe mankhwalawa amasakanikirana ndi madzi.

Malinga ndi kupangidwa, mu Gawo (3), zomwe zimasakanikirana pambuyo pa Gawo (2) zitha kusefedwa ndi kutsekeka kotseka, kapena kutha

Makhiristo olimba amapezedwa mwa kukanikiza mwachindunji mu mbale ya sieve pansi pa riyakitala. Pazopanga zamakono, mpweya ndi/kapena nayitrogeni zimagwiritsidwa ntchito bwino

Pressure kusefera, ndi bwino kugwiritsa ntchito nayitrogeni kwa kuthamanga kusefera, ndipo kuthamanga kungakhale 0.1-0.2MPa, makamaka 0,12 -

0.18 mpa.

Malinga ndi kupangidwako, kristalo wokhazikika pambuyo pa kusefera kwamphamvu imatsukidwa ndi madzi, momwe madziwo amatsukidwa.

Palibe malire enieni, mwachitsanzo, mutha kusankha 1-2kg yotsuka madzi opopera pansi pa kutentha kwa 2-25 ℃, ndi kupopera mbewu mankhwalawa.

Palibe malire enieni othamanga.

Malinga ndi kupangidwako, chiyero cha 1,1, 3-trichloroacetone chosakanizidwa chikhoza kukhala 50-65 % kulemera kwake.

Masamba 3/6 a malangizo

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CN 109516908 A

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Kupangidwa kwamakono, kumbali ina, kumaperekanso folic acid yomwe imakonzedwa ndi njira iliyonse yomwe tafotokozayi

Njira yamadzimadzi ya 1,1, 3-trichloroacetone imagwiritsidwa ntchito mwachindunji kukonza folic acid.

Kugwiritsa ntchito njira yoyeretsera zomwe zidapangidwa, monga stratified m'zigawo, kusefera kwa crystallization ndi zina zotero, zitha kuchitika munjira yotsekedwa.

Environment-wochezeka, ndi kuchepetsa kwambiri m'badwo wa madzi zinyalala, palibe zinyalala organic solvents ndi organic zinyalala mpweya; Komanso, kuyeretsa njira

Palibe zosungunulira za organic zomwe zimayambitsidwa, ndipo zonyansa zambiri za chlorine zimachotsedwa panthawi yoyeretsa, kotero palibe chiwopsezo chamtundu wa folic acid.

Njirayi imagwiritsa ntchito madzi ngati chosungunulira cha crystallization, ndipo njira yoyeretsera yamadzimadzi ya 1,1, 3-trichloroacetone imagwiritsidwa ntchito mwachindunji kupanga folic acid.

Zokolola zonse za kupatsidwa folic acid zitha kuonjezeredwa ndi 5 % polemera, ndipo chiyero chimaposa 99.2% polemera, chomwe chingapezeke chapamwamba kwambiri.

Kupatsidwa folic acid.

Zomwe zidapangidwazo zikufotokozedwa mwatsatanetsatane pogwiritsa ntchito ma embodiments pansipa.

[0042] M'mawonekedwe ndi magawo otsatirawa, pokhapokha atanenedwa mwanjira ina, zida zomwe zimagwiritsidwa ntchito zimapezeka pogula malonda, pokhapokha zitanenedwa mwanjira ina.

Njira yomwe imagwiritsidwa ntchito ndi yodziwika bwino pamundawu.

Mtundu wa chromatography wa gasi unali GC-2014, wogulidwa ku Shimadzu Company.

The 1,1, 3-trichloroacetone yokonzedwa ndi njira yoyeretsera yomwe yapangidwa kale [0047] imayeretsedwa mu riyakitala ya 50-lita yokhala ndi mbale ya sefa pansi [0048] Choyamba, chiyero cha 1,1 ndi 65 % ndi kulemera , 3-trichloroacetone 20Kg ndi madzi 10Kg mu anachita ketulo wothira 24 oyambitsa kwa mphindi 12, pamene yogwira mtima mlingo ndi 200r/mphindi, mu yoyambitsa ndondomeko kuwonjezera madzi, madzi pa mlingo wa 300 ml/mphindi. , ndiyeno osakaniza anaima kwa mphindi 10, olekanitsidwa ndi mafuta m'munsi wosanjikiza, kuchotsa mkulu chlorine zosafunika; Kachiwiri, kutentha kwa wosanjikiza chapamwamba njira adatchithisira kwa 5 ndi analimbikitsa kwa 2 hours pa oyambitsa mlingo wa 100r/min. Kenako, olimba krustalo analandira mwachindunji kudzera sieve mbale pansi zimene ketulo ndi nayitrogeni kuthamanga kusefera pa mavuto a 0,1 MPa, ndiyeno sprayed ndi kutsukidwa ndi 2 makilogalamu madzi ozizira. Kulemera konyowa kwa 1,1, 3-trichloroacetone kunali 9.8 kg, ndipo chromatographic pure (GC) inali 96.8 wt % [0051] Opaleshoni yomwe imakhudzidwa ndi njira yoyeretsera iyi, monga static stratification, kuchotsa zonyansa zambiri za chlorine, crystallization, kusefera ndi kutsuka madzi, akhoza kuchitidwa mu dongosolo chatsekedwa thupi, amene ndi wochezeka zachilengedwe, ndipo amachepetsa kwambiri m'badwo wa madzi zinyalala ndipo samatulutsa zinyalala zosungunulira organic ndi organic zinyalala gasi [0052]. Kuphatikiza apo, chifukwa njira yoyeretsera popanda kuyambitsa zosungunulira za organic, ndi klorini yayikulu kuchotsa zonyansa pakuyeretsa, palibe chiwopsezo chamtundu wa folic acid, komanso kugwiritsa ntchito chitsanzo cha kukonzekera kwa 1, 1, 3 - kupatsidwa folic acid mtanda olumikizidwa ndi acetone madzi kusungunuka mwachindunji ntchito kupanga, kumapangitsa kupatsidwa folic acid kusintha wonse zokolola 5 kulemera %, chiyero cha 99 5 kulemera % Chitsanzo 2 [0054] Maonekedwe ake amanena kuti 1,1, 3-trichloroacetone yokonzedwa ndi njira yoyeretsera ya kupangidwa kwamakono [0055] imayeretsedwa mu 50-lita riyakitala okonzeka ndi fyuluta mbale sieve pansi [0056] Choyamba, 1,1 ndi chiyero cha 50% , 3-trichloroacetone 20Kg ndi madzi 4Kg wosakaniza. mu riyakitala, oyambitsa kwa mphindi 15 pa 45, oyambitsa mlingo wa 300r/mphindi, mu oyambitsa ndondomeko kuwonjezera madzi, madzi pa mlingo wa 300 ml/mphindi, ndiyeno osakaniza anaima kwa mphindi 15, wosiyana ndi mafuta osanjikiza otsika, chotsani zonyansa zambiri za chlorine; Kachiwiri, kutentha kwa yankho lapamwamba pambuyo pa stratification kunatsitsidwa mpaka 20, ndipo kuthamanga kunali 200r / min kwa 0,5 h. Ndiye, olimba krustalo analandira mwachindunji kupyolera sieve mbale pansi pa riyakitala ndi asafe kuthamanga kusefera pa mavuto a 0. 2MPa. Kenako, kristalo wolimba adapopera ndi kutsukidwa ndi 1Kg ya madzi ozizira 25, ndipo kulemera konyowa kwa 1,1, 3-trichloroacetone kunali 8.2kg ndi njira yochepetsera Njira yoyeretsera yomwe imakhudzidwa ndi kuchotseratu zonyansa zambiri za chlorine, crystallization, kusefera ndi kuchapa madzi ntchito angathe kuchitidwa mu A chatsekedwa dongosolo thupi, malo ogwira ntchito ndi ochezeka, ndi kuchepetsa kwambiri m'badwo wa madzi zinyalala, palibe zinyalala zosungunulira organic ndi organic zinyalala gasi [0060] Komanso, popeza njira amachita osayambitsa zosungunulira za organic ndikuchotsa zonyansa zambiri za chlorine panthawi yoyeretsa, palibe chiopsezo chamtundu wa folic acid, ndipo 1,1, 3-trichloroacetone yokonzedwa ndi Chitsanzo 2 imasungunuka m'madzi ndipo imagwiritsidwa ntchito mwachindunji popanga kupatsidwa folic acid, kuonjezera zokolola zonse za kupatsidwa folic acid ndi 4.9% pa kulemera kwake ndi kukwaniritsa chiyero cha 99 Maonekedwe awa akunena kuti 1,1, 3-trichloroacetone yokonzedwa ndi njira yoyeretsera ya kupangidwa kwamakono [0063] imayeretsedwa mu 50 -lita riyakitala wodzazidwa ndi fyuluta mbale sieve pansi [0064] Choyamba, 1,1 ndi chiyero cha 60% , 3-trichloroacetone 20Kg wothira madzi 40Kg mu ketulo anachita, oyambitsa kwa mphindi 30 pa 15, ndi kusonkhezera mlingo. wa 100r/mphindi, poyambitsa ndondomeko kuwonjezera madzi, madzi pa mlingo wa 500 ml/mphindi, ndiyeno osakaniza anaima kwa mphindi 30, wosiyana ndi mafuta wosanjikiza m'munsi, kuchotsa mkulu chlorine zosafunika; Kachiwiri, kutentha kwa yankho lapamwamba pambuyo pa stratification kunatsitsidwa mpaka 10, ndipo kuthamanga kunali 100r/min kwa maola 10. Ndiye, olimba krustalo analandira mwachindunji kupyolera sieve mbale pansi pa riyakitala ndi nayitrogeni kuthamanga kusefera pa mavuto a 0.2MPa, ndiyeno sprayed ndi kutsukidwa ndi 1Kg 5 madzi ozizira. Kulemera konyowa kwa 1,1, 3-trichloroacetone kunali 6.9kg, ndipo chromatographic pure (GC) inali 98.3% ndi kulemera kwake [0067] Opaleshoni yomwe imakhudzidwa ndi njira yoyeretsera iyi, monga static stratification, kuchotsa zonyansa za chlorine, crystallization. , kusefera ndi kutsuka madzi, kungathe kuchitidwa mu dongosolo lotsekedwa la thupi, lomwe liri ndi malo ogwirira ntchito ochezeka, ndipo amachepetsa kwambiri mbadwo wa madzi otayira ndipo samatulutsa zinyalala zosungunulira organic ndi organic zinyalala gasi [0068]. Komanso, chifukwa kuyeretsedwa njira popanda kuyambitsa zosungunulira organic, ndi chlorine mkulu kuchotsa zonyansa mu ndondomeko kuyeretsedwa, palibe chiopsezo khalidwe pa khalidwe la kupatsidwa folic acid, ndipo adzakhala Mwachitsanzo 3 kukonzekera 1, 1, 3 - mtanda olumikizidwa ndi acetone, madzi kupasuka, mwachindunji ntchito kupanga kupatsidwa folic acid, kupanga kupatsidwa folic acid kusintha wonse zokolola 5. 3 kulemera%, chiyero cha 99. 2 kulemera % Pakuti gawo 1 [0070] oyeretsedwa 1,1, 3- trichloroacetone molingana ndi njira yowonetsera 1, kupatula kuti mu sitepe (1), madzi sagwiritsidwa ntchito, M'malo mwake, zosungunulira za organic zidagwiritsidwa ntchito. Zotsatira zake, 1,1, 3-trichloroacetone yokonzedwayo idasungunuka m'madzi ndipo imagwiritsidwa ntchito mwachindunji popanga folic acid. Zokolola zonse za kupatsidwa folic acid zinangowonjezeka ndi 2% kulemera kwake ndipo chiyero chinali 95% polemera. Kuonjezera apo, chifukwa cha kuyambitsidwa kwa zosungunulira za organic mu njira yoyeretsera iyi, pali chiopsezo cha khalidwe la folic acid [0071] mu gawo la 2 [0072]. 1,1, 3-trichloroacetone imayeretsedwa molingana ndi njira yomwe ili mu Chitsanzo 1. Kusiyanitsa ndiko kuti mu Gawo (1), kuchuluka kwa madzi ndi 50Kg, zomwe zimapangitsa kuwonjezeka kwakukulu kwa mbadwo wa madzi onyansa ndi kuchepa kwa 1 The zokolola za 1,1, 3-trichloroacetone makhiristo anasungunuka m'madzi ndipo mwachindunji ntchito kupanga kupatsidwa folic acid, kotero kuti okwana zokolola za kupatsidwa folic acid anangowonjezeka ndi 5.6% ndi kulemera ndi chiyero anali 99.6% kulemera [0073] ] motsutsana ndi chiŵerengero cha 3 [0074]. 1,1 idayeretsedwa ndi njira ya Chitsanzo 1, 3-trichloroacetone, kusiyana ndi kuti mu sitepe (1), mkulu wa chlorine heteroplastid samachotsedwa, chifukwa cha kukonzekera kwa 1,1, 3-trichloroacetone ili ndi lalikulu. chiwerengero cha mankhwala klorini, khalidwe la kupatsidwa folic acid chiopsezo [0075] Malinga ndi chitsanzo pamwamba 1-3 ndi chifukwa cha sikelo 1-3: njira kuyeretsedwa kumaphatikizapo tiyeni tiyime wosanjikiza galasi fyuluta kuchotsa mkulu chlorine zonyansa kutsuka ntchito. monga zonse koma mu dongosolo airtight, wochezeka ntchito malo, ndipo kwambiri kuchepetsa kuchuluka kwa madzi zinyalala, samatulutsa zinyalala zosungunulira, organic zosungunulira ndi organic Komanso, ndi kukhazikitsa mlandu 1 kukonzekera 1, 1), 3-trichloroacetone. , kuwonjezera m'buku 5/6 tsamba 7 CN 109516908 A 7 madzi njira, mwachindunji ntchito kupanga kupatsidwa folic acid, kupanga okwana zokolola za kupatsidwa folic acid kuchuluka 5 % ndi kulemera, chiyero ndi 99,2 % ndi kulemera pamwamba; Komanso, chifukwa njira yoyeretsera sikuyambitsa zosungunulira za organic, palibe chiopsezo chamtundu wa folic acid. Komanso, njira yoyeretsera imagwiritsa ntchito madzi monga crystallization zosungunulira, ndi oyeretsedwa amadzimadzi njira ya 1,1, 3-trichloroacetone mwachindunji ntchito kupanga kupatsidwa folic acid, kuchepetsa mbali zochita.

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MIT-Malingaliro a kampani IVY Industry Co., Ltd

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