Ngakolunye uhlangothi, ukusungulwa kunikeza indlela yokuhlanza ye-1,1, 3-trichloroacetone, lapho indlela iqukethe izinyathelo ezilandelayo.

I-Flash:

(1) I-1,1, 3-trichloroacetone exutshwe namanzi;

(2) Ukwenziwa kabusha kwekhambi eliphezulu ngemva kokuma; Kanye ne

(3) amakristalu aqinile akhiqizwe kabusha ayahlungwa futhi agezwe ngamanzi;

Lapho, Esinyathelweni (1), isilinganiso sesisindo salokhu okungahluziwe okushiwo 1,1, 3-trichloroacetone enanini lamanzi ngu-10.1-2).

Ngokukhethekile, Esinyathelweni (1), isilinganiso sesisindo somkhiqizo ongahluziwe ongu-1,1, 3-trichloroacetone enanini lamanzi singaba ngu-1:

(0.4-0.6), ithuthukiswe futhi njengo-1:0.5; Ekusungulweni, umthamo womkhiqizo ongcolile we-1,1, 3-trichloroacetone namanzi ulawulwa kulokhu okungenhla.

Uhla lokuhlanzeka okuphezulu 1,1, 3-trichloroacetone lungatholakala.

Ngokusho kokusungulwa kwamanje, esinyathelweni (1), umkhiqizo ongahluziwe we-1,1, 3-trichloroacetone namanzi kungalungiswa ezingeni lokushisa lika-10-50 ℃

Hlanganisa imizuzu engu-10-30 ngaphansi kwezimo, bese uvumela ukuthi ume imizuzu engu-10-30; Ngokungcono, kuSinyathelo (1), uthe 1,1, 3-trichloropropyl

I-ketone eluhlaza ixutshwe namanzi ekushiseni kwe-30-35 ℃ imizuzu engu-25-30, bese ima imizuzu engu-10-15; Ekusungulweni kwamanje

, kusetshenziswa i-1,1, 3-trichloroacetone eluhlaza njengempahla eluhlaza, kugedlela lokusabela, elixutshwe namanzi, elinyakaziswa ezingeni lokushisa elithile ngemva kokuma.

I-Delamination. Ngemuva kwe-delamination, ungqimba lwamafutha aphansi luyasuswa, ikakhulukazi ngokususa ukungcola okuphezulu kwe-chlorine nokushiya isisombululo esiphezulu ukuze sisetshenziswe kamuva.

Ngokokusungulwa, esinyathelweni (1), i-1,1, 3-trichloroacetone engahluziwe ixutshwe namanzi futhi inganyakaziswa.

Izimo, lapho kungekho mkhawulo othize ezimweni ezinyakazayo kanye nemishini, inqobo nje uma i-1,1, 3-trichloroacetone ingaba mahhadla

Umkhiqizo ungaxutshwa ngokulinganayo namanzi. Okungcono, izinga lokuxuba liyi-100-300r/min.

Ekusungulweni kwamanje, amanzi angcono kakhulu ahlanjululwe ngamanzi.

Ngokusho kokusungulwa, esinyathelweni (2), izimo zokuvuselela kabusha zingase zibe: izinga lokushisa kusuka ku-0 kuye ku-35 ℃, isikhathi sisuka ku-0.5 -

Amahora angu-10, okungcono, i-recrystallization yenziwa ngesilinganiso esishukumisayo se-50-300 RPM; Okungcono, i-reknot

Amanzi aphinde afakwe ohlelweni lwe-crystallization, lapho amanzi engezwa khona ngesilinganiso se-200-600 ml / min; Ngaphansi kwalezi zimo, recrystallization ukusebenza kahle

Izithelo zinhle.

[0034] Ngokuqhubekayo, izimo zokuvuselela kabusha yilezi: izinga lokushisa lika-10-15 ℃, isikhathi samahora angu-2-3, nezimo zokuvuselela kabusha.

I-crystal ishukunyiswa ngesilinganiso se-100-200 RPM futhi amanzi engezwa ngesilinganiso se-300-500 ml / min.

Ngaphansi kwalezi zimo, umphumela we-recrystallization ungcono.

Ekusungulweni kwamanje, izinga lokushisa lokwenziwa kabusha kwekristalu elichazwe esinyathelweni (2) liphansi kunalelo lika-1,1, 3-trichloroacetone esinyathelweni (1)

Izinga lokushisa lapho umkhiqizo uxutshwa khona namanzi.

Ngokusho kokusungulwa, ku-Isinyathelo (3), ingxube yokusabela ngemva kwesinyathelo (2) ingahlungwa ngokucindezelwa okuvaliwe, noma ingaba

Amakristalu aqinile atholakala ngokucindezela ngokuqondile ipuleti lesisefo elingaphansi kwe-reactor. Ekusungulweni kwamanje, kungcono ukusebenzisa umoya kanye/noma i-nitrogen

Ukuhlunga kwengcindezi, kungcono ukusebenzisa i-nitrogen yokuhlunga ingcindezi, futhi ingcindezi ingaba ngu-0.1-0.2MPa, okungcono kakhulu ngu-0.12 -

0.18 mpa.

Ngokusho kokusungulwa, i-crystal encibilikisiwe ngemuva kokuhlunga ingcindezi igezwa ngamanzi, lapho amanzi ashiwo egezwa khona.

Awukho umkhawulo othize, isibonelo, ungakhetha u-1-2kg wokugeza isifutho samanzi ngaphansi kwesimo sokushisa kwe-2-25 ℃, bese ufutha.

Awukho umkhawulo wejubane othize.

Ngokusho kokusungulwa, ukuhlanzeka komkhiqizo ongahluziwe we-1,1, 3-trichloroacetone kungaba ngu-50-65 % ngesisindo.

Amakhasi 3/6 omyalelo

5

CN 109516908 A

5

Ukusungulwa kwamanje, ngakolunye uhlangothi, kuhlinzeka nge-folic acid elungiswa nganoma iyiphi yezindlela ezichazwe ngenhla

Isixazululo esinamanzi se-1,1, 3-trichloroacetone sisetshenziswa ngokuqondile ukulungisa i-folic acid.

Ukusebenza kwendlela yokuhlanza yokusungulwa, njengokukhishwa kwe-stratified, ukuhlunga kwe-crystallization nokunye, kungenziwa ohlelweni oluvaliwe.

Imvelo enobungane, futhi inciphisa kakhulu ukukhiqizwa kwamanzi angcolile, azikho izincibilikisi zemvelo ezilahlwayo kanye negesi yemfucuza ephilayo; Ngaphezu kwalokho, indlela yokuhlanza

Awekho ama-organic solvents angeniswayo, futhi ukungcola okuphezulu kwe-chlorine kuyasuswa ngesikhathi sokuhlanzwa, ngakho-ke ayikho ingozi yekhwalithi yekhwalithi ye-folic acid.

Indlela isebenzisa amanzi njenge-crystallization solvent, futhi isixazululo samanzi esihlanzekile se-1,1, 3-trichloroacetone sisetshenziselwa ngokuqondile ukukhiqizwa kwe-folic acid.

Isivuno esiphelele se-folic acid singanyuswa ngo-5% ngesisindo, futhi ubumsulwa bungaphezu kwama-99.2 % ngesisindo, esingathola izinga eliphezulu.

Iqukethe i-folic acid.

Ukusungulwa kuchazwa ngokuningiliziwe ngokusebenzisa i-embodiments ngezansi.

[0042] Kulezi zifanekiso nezilinganiso ezilandelayo, ngaphandle uma kucaciswe ngenye indlela, izinto ezisetshenziswayo zitholakala ngokuthengwa kwezentengiso, ngaphandle uma kucaciswe ngenye indlela.

Indlela esetshenziswayo iyindlela ejwayelekile kulo mkhakha.

Imodeli ye-gas chromatography bekuyi-GC-2014, ethengwe ku-Shimadzu Company.

I-1,1, 3-trichloroacetone elungiselelwe indlela yokuhlanza yokusungulwa kwamanje [0047] ihlanzwa ku-reactor engamalitha angu-50 efakwe ipuleti lesihluzo lesihlungi ngezansi [0048] Okokuqala, ubumsulwa be-1,1 bungama-65 % ngesisindo , 3-trichloroacetone 20Kg kanye namanzi 10Kg kugedlela lokusabela elixutshwe ku-24 livuselela imizuzu engu-12, lapho izinga elishukumisayo liyi-200r/min, enqubweni eshukumisayo yokwengeza amanzi, amanzi ngesilinganiso se-300 ml / min. , bese ingxube imile imizuzu engu-10, ihlukaniswe nesendlalelo samafutha aphansi, isuse ukungcola okuphezulu kwe-chlorine; Okwesibili, izinga lokushisa lesisombululo esiphezulu se-layer lehliselwa ku-5 futhi livuselelwe amahora angu-2 ngesilinganiso esishukumisayo se-100r / min. Khona-ke, i-crystal eqinile yatholwa ngokuqondile ngepuleti yesisefo ngaphansi kweketela lokusabela ngokuhlunga kwe-nitrogen pressure ngokucindezela kwe-0.1 MPa, bese ifafazwa futhi igezwe ngamanzi abandayo angu-2 kg. Isisindo esimanzi se-1,1, 3-trichloroacetone sasingu-9.8 kg, kanti i-chromatographic pure (GC) yayingu-96.8 wt % [0051] Ukuhlinzwa okuhilelekile kule ndlela yokuhlanza, njengokuhlelwa kwe-static, ukususwa kokungcola okuphezulu kwe-chlorine, i-crystallization, ukuhlunga kanye nokugeza amanzi, kungenziwa ohlelweni lomzimba oluvaliwe, oluhambisana nemvelo, futhi kunciphisa kakhulu ukukhiqizwa kwamanzi angcolile futhi akukhiqizi imfucumfucu ye-solvent ne-organic waste gas [0052]. Ngaphezu kwalokho, ngenxa yokuthi indlela yokuhlanza ngaphandle kokwethula i-solvent ephilayo, kanye ne-chlorine ephezulu yokususa ukungcola enqubweni yokuhlanza, ayikho ingozi yekhwalithi yekhwalithi ye-folic acid, kodwa futhi nangesibonelo sokuqaliswa kokulungiswa kwe-1, 1, 3 - i-folic acid exhunywe ngokuphambana namanzi e-acetone encibilikisiwe ngokuqondile ekukhiqizeni, yenza i-folic acid ithuthukise isivuno esiphelele 5 isisindo %, ukuhlanzeka kwe-99 5 isisindo % Isibonelo 2 [0054] Lokhu kufanekisa kusho ukuthi i-1,1, 3-trichloroacetone elungiselelwe indlela yokuhlanza yento esunguliwe manje [0055] ihlanzwa ku-reactor engamalitha angama-50 efakwe ipuleti lesisefo esisefe phansi [0056] Okokuqala,1,1 ngobumsulwa obungu-50% , 3-trichloroacetone 20Kg namanzi 4Kg okuxutshwe ku-reactor, ivuselela imizuzu engu-15 ku-45, izinga elishukumisayo lika-300r / min, enkambisweni yokugqugquzela ukwengeza amanzi, amanzi ngesilinganiso se-300 ml / min, bese ingxube imile imizuzu engu-15, ihlukaniswe ungqimba lwamafutha aphansi, susa ukungcola okuphezulu kwe-chlorine; Okwesibili, izinga lokushisa lesisombululo sesendlalelo esiphezulu emva kokuhlukaniswa kwehliswa ku-20, futhi izinga lokugqugquzela laliyi-200r / min ye-0.5 h. Khona-ke, ikristalu eqinile yatholwa ngokuqondile ngepuleti yesisefo ngaphansi kwe-reactor ngokuhlunga kwe-nitrogen pressure ngokucindezela kwe-0. 2MPa. Khona-ke, i-crystal eqinile yafafazwa futhi yagezwa nge-1Kg yamanzi abandayo angu-25, futhi isisindo esimanzi se-1,1, 3-trichloroacetone sasingu-8.2kg ngendlela yokunciphisa Indlela yokuhlanza ehilelekile ekususweni kwe-static stratification kokungcola okuphezulu kwe-chlorine, crystallization, filtration kanye nokugeza amanzi imisebenzi kungenziwa A evaliwe uhlelo umzimba, indawo yokusebenza enobungane, futhi kunciphisa kakhulu ukukhiqizwa kwamanzi angcolile, akukho imfucuza organic solvent kanye organic imfucuza gas [0060] Ngaphezu kwalokho, kusukela indlela enza angethuli izincibilikisi eziphilayo futhi asuse ukungcola okuphezulu kwe-chlorine phakathi nenqubo yokuhlanza, ayikho ingozi yekhwalithi yekhwalithi ye-folic acid, futhi i-1,1, 3-trichloroacetone elungiselelwe yiSibonelo sesi-2 iyancibilika emanzini futhi isetshenziswe ngokuqondile ekukhiqizeni i-folic acid, okwandisa isivuno esiphelele se-folic acid ngo-4.9% ngesisindo nokufeza ukuhlanzeka kwe-99 Lokhu kufanekisa kusho ukuthi i-1,1, 3-trichloroacetone elungiselelwe indlela yokuhlanza yokusungulwa kwamanje [0063] ihlanzwa ku-50 -litre reactor efakwe ipuleti lesisefo esisefo ngezansi [0064] Okokuqala,1,1 ngokuhlanzeka okungu-60%, 3-trichloroacetone 20Kg exutshwe namanzi 40Kg kugedlela lokusabela, inyakaza imizuzu engama-30 ku-15, izinga lokunyakazisa ye-100r / min, enkambisweni yokugqugquzela ukwengeza amanzi, amanzi ngesilinganiso se-500 ml / min, bese ingxube imele imizuzu engu-30, ihlukaniswe nongqimba lwamafutha aphansi, isuse ukungcola okuphezulu kwe-chlorine; Okwesibili, izinga lokushisa lesisombululo sesendlalelo esiphezulu ngemuva kokufakwa kwe-stratification kwehliswa ku-10, futhi izinga lokugqugquzela laliyi-100r / min amahora angu-10. Khona-ke, i-crystal eqinile yatholwa ngokuqondile ngepuleti yesisefo ngaphansi kwe-reactor ngokuhlunga kwe-nitrogen pressure ngokucindezela kwe-0.2MPa, bese ifuthwa futhi igezwe nge-1Kg yamanzi abandayo angu-5. Isisindo esimanzi se-1,1, 3-trichloroacetone sasingu-6.9kg, kanti i-chromatographic pure (GC) yayingu-98.3% ngesisindo [0067] Ukusebenza okuhilelekile kule ndlela yokuhlanza, njengokuhlelwa kwe-static, ukususwa kokungcola okuphezulu kwe-chlorine, i-crystallization , ukuhlunga nokugeza kwamanzi, kungenziwa ohlelweni lomzimba oluvaliwe, olunendawo yokusebenza enobungane, futhi kunciphisa kakhulu ukukhiqizwa kwamanzi angcolile futhi akukhiqizi imfucumfucu ye-solvent ne-organic waste gas [0068]. Ngaphezu kwalokho, ngoba indlela yokuhlanza ngaphandle kokwethula i-solvent ephilayo, kanye ne-chlorine ephezulu yokususa ukungcola enqubweni yokuhlanza, ayikho ingozi yekhwalithi yekhwalithi ye-folic acid, futhi kuyoba isibonelo 3 ukulungiswa kwe-1, 1, 3 - cross- exhunywe ne-acetone, amanzi okumele ancibilike, asetshenziswe ngokuqondile ekukhiqizeni i-folic acid, enza i-folic acid ithuthukise isivuno sonke 5. 3 isisindo %, ukuhlanzeka kwe-99. 2 isisindo % Ngokwengxenye 1 [0070] ehlanjululwe 1,1, 3- i-trichloroacetone ngokwendlela yokufanisa 1, ngaphandle kokuthi esinyathelweni (1), amanzi awasetshenziswa, Kunalokho, kwasetshenziswa izinyibilikisi eziphilayo. Ngenxa yalokho, i-1,1, 3-trichloroacetone elungiselelwe yachithwa emanzini futhi yasetshenziswa ngokuqondile ekukhiqizeni i-folic acid. Isamba sesivuno se-folic acid sande kuphela ngo-2 % ngesisindo kanti ubumsulwa bube ngu-95 % ngesisindo. Ukwengeza, ngenxa yokwethulwa kwezinyibilikisi zemvelo kule ndlela yokuhlanza, kunengozi yekhwalithi yekhwalithi ye-folic acid [0071] ngokulingana 2 [0072]. I-1,1, 3-trichloroacetone ihlanjululwa ngokwendlela eseSibonelweni 1. Umehluko wukuthi Esinyathelweni (1), inani lamanzi liyi-50Kg, okuholela ekwenyukeni okukhulu kokukhiqizwa kwamanzi angcolile kanye nokuncipha kwe-1 The isivuno se-1,1, i-3-trichloroacetone crystals yachithwa emanzini futhi yasetshenziswa ngokuqondile ekukhiqizeni i-folic acid, ukuze isivuno esiphelele se-folic acid sande kuphela ngo-5.6% ngesisindo futhi ubumsulwa bungu-99.6% ngesisindo [0073 ] ngokumelene nesilinganiso esingu-3 [0074]. I-1,1 yahlanjululwa ngendlela yeSibonelo 1, i-3-trichloroacetone, umehluko wukuthi esinyathelweni (1), i-heteroplastid ephezulu ye-chlorine ayisusiwe, umphumela wokulungiswa kwe-1,1, 3-trichloroacetone iqukethe enkulu inombolo ye-chlorinated compounds, ikhwalithi yengozi ye-folic acid [0075] Ngokusho kwesibonelo esingenhla 1-3 futhi ingumphumela wesilinganiso se-1-3: indlela yokuhlanza ihilela ukumisa isihlungi sekristalu esinezingqimba ukuze sisuse imisebenzi yokugeza ukungcola okuphezulu kwe-chlorine njengakho konke kodwa ohlelweni olungenawo umoya, indawo yokusebenza enobungane, futhi kunciphise kakhulu ukwenzeka kwamanzi angcolile, akukhiqizi igesi engcolile, i-organic solvent kanye ne-organic Ngaphezu kwalokho, ngokusebenzisa icala 1 ukulungiswa kwe-1, 1), 3-trichloroacetone. , engeza encwadini ye-5/6 ikhasi 7 CN 109516908 Isixazululo samanzi esingu-7, esisetshenziswe ngokuqondile ekukhiqizeni i-folic acid, yenza isivuno esiphelele se-folic acid senyuke ngo-5 % ngesisindo, ukuhlanzeka kungu-99.2 % ngesisindo ngenhla; Ngaphezu kwalokho, ngenxa yokuthi indlela yokuhlanza ayifaki i-solvent ephilayo, ayikho ingozi yekhwalithi yekhwalithi ye-folic acid. Ngaphezu kwalokho, indlela yokuhlanza isebenzisa amanzi njenge-crystallization solvent, futhi isixazululo samanzi esihlanzekile se-1,1, 3-trichloroacetone sisetshenziswa ngokuqondile ekukhiqizeni i-folic acid, ukunciphisa ukusabela okuhlangene.

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