Ngakolunye uhlangothi, lo mbono unikeza indlela yokuhlanza engu-1,1, 3-trichloroacetone, lapho le ndlela ihlanganisa izinyathelo ezilandelayo.

I-Flash:

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

(2) Ukuphinda kusetshenziswe isixazululo esingaphezulu ngemva kokuma; Kanye

(3) amakristalu aqinile aphinde asetshenziswa ayahlungwa bese egezwa ngamanzi;

Lapho, ku-Isinyathelo (1), isilinganiso sesisindo se-crude 1, 1, 3-trichloroacetone eshiwoyo enanini lamanzi singu-10.1-2).

Kungcono, ku-Isinyathelo (1), isilinganiso sesisindo somkhiqizo ongcolile ongu-1,1, 3-trichloroacetone nenani lamanzi singaba ngu-1:

(0.4-0.6), okuthuthukisiwe ngokwengeziwe njenge-1:0.5; Kulo mbono, umthamo womkhiqizo ongahluziwe we-1,1, 3-trichloroacetone kanye namanzi ulawulwa kulokhu okungenhla.

Ububanzi bokuhlanzeka okuphezulu kwe-1,1, 3-trichloroacetone bungatholakala.

Ngokusho kwalokhu okusunguliwe, esinyathelweni (1), umkhiqizo ongcolile we-1, 1, 3-trichloroacetone kanye namanzi kungalungiswa ekushiseni okungu-10-50℃

Hlanganisa imizuzu eyi-10-30 ngaphansi kwezimo, bese uyiyeka ime imizuzu eyi-10-30; Kungcono, ku-Isinyathelo (1), kusho i-1,1, 3-trichloropropyl

I-ketone eluhlaza yaxutshwa namanzi ekushiseni okungu-30-35℃ imizuzu engu-25-30, yabe isima imizuzu eyi-10-15; Kulokhu kusungulwa kwamanje

, kusetshenziswa i-1,1, 3-trichloroacetone crude njengezinto ezingavuthiwe, eketheni lokusabela, lixutshwe namanzi, livuselelwe ekushiseni okuthile ngemva kokuma

Ukususwa kwe-Delamination. Ngemva kokususwa kwe-delamination, ungqimba lwamafutha olungezansi luyasuswa, ikakhulukazi ngokususa ukungcola okuphezulu kwe-chlorine bese kushiya isixazululo esiphezulu ukuze sisetshenziswe kamuva.

Ngokusho kwalokhu kusungulwa, esinyathelweni (1), i-crude 1, 1, 3-trichloroacetone ixutshwa namanzi futhi ingavuselelwa.

Izimo, lapho kungekho mkhawulo oqondile ezimweni zokuxuba kanye nemishini, inqobo nje uma i-1,1, 3-trichloroacetone ingaba nzima

Umkhiqizo ungaxutshwa ngokulinganayo namanzi. Kungcono ukuthi izinga lokuxuba libe ngu-100-300r/min.

Kulokhu okusunguliwe, kungcono ukuthi amanzi abe ngamanzi angenawo ama-ion.

Ngokusho kwalokhu kusungulwa, esinyathelweni (2), izimo zokuphinda kusetshenziswe kabusha zingaba: izinga lokushisa kusuka ku-0 kuya ku-35℃, isikhathi kusuka ku-0.5 -

Amahora ayi-10, okungcono kakhulu, ukuphinda kusetshenziswe kabusha kwenziwa ngesivinini sokuxubha esingu-50-300 RPM; Okungcono kakhulu, ukuphinda kusetshenziswe kabusha

Amanzi aphinde engezwe enkambisweni yokwenza ikristalu, lapho amanzi engezwa khona ngesilinganiso esingu-200-600 ml/min; Ngaphansi kwalezi zimo, ukusebenza kahle kokwenza ikristalu kabusha

Izithelo zinhle.

[0034] Ngaphezu kwalokho, izimo zokwenziwa kabusha kwekristalu yilezi: izinga lokushisa elingu-10-15℃, isikhathi samahora angu-2-3, kanye nezimo zokwenziwa kabusha kwekristalu.

Ikristalu ivuselelwa ngesivinini esingu-100-200 RPM bese amanzi engezwa ngesivinini esingu-300-500 ml/min.

Ngaphansi kwalezi zimo, umphumela wokuphinda usebenzise i-crystallization ungcono.

Kulokhu okusunguliwe, izinga lokushisa lokuphinda kusetshenziswe kabusha elichazwe esinyathelweni (2) liphansi kunele-1,1, 3-trichloroacetone esinyathelweni (1)

Izinga lokushisa lapho umkhiqizo uxutshwa khona namanzi.

Ngokusho kwalokhu kusungulwa, kuSinyathelo (3), ingxube yokusabela ngemva kweSinyathelo (2) ingahlungwa ngokucindezela okuvaliwe, noma ingahlungwa

Amakristalu aqinile atholakala ngokucindezela ngqo ngepuleti lesihlungo phansi kwe-reactor. Kulokhu kusungulwa, kungcono ukusebenzisa umoya kanye/noma i-nitrogen

Ukuhlunga ingcindezi, kungcono ukusebenzisa i-nitrogen ekuhlungeni ingcindezi, futhi ingcindezi ingaba ngu-0.1-0.2MPa, okungcono kube ngu-0.12 -

0. 18 mpa.

Ngokusho kwalokhu kusungulwa, ikristalu elihlanziwe ngemuva kokuhlunga ingcindezi ligezwa ngamanzi, lapho amanzi ashiwoyo egezwa khona.

Akukho mkhawulo othize, isibonelo, ungakhetha i-1-2kg yokuwasha ngamanzi ngaphansi kwesimo sokushisa esingu-2-25℃, bese ufutha.

Akukho mkhawulo wejubane othize.

Ngokusho kwalokhu kusungulwa, ubumsulwa bomkhiqizo ongahluziwe we-1,1, 3-trichloroacetone bungaba ngu-50-65% ngesisindo.

Amakhasi 3/6 emiyalelo

5

I-CN 109516908 A

5

Ngakolunye uhlangothi, lesi sisungulo siphinde sinikeze i-folic acid elungiselelwe nganoma iyiphi yalezi zindlela ezichazwe ngenhla.

Isixazululo samanzi se-1,1, 3-trichloroacetone sisetshenziswa ngqo ukulungisa i-folic acid.

Ukusebenza kwendlela yokuhlanza yale nqubo, njengokukhipha okuhlanganisiwe, ukuhlunga kwe-crystallization nokunye, kungenziwa ohlelweni oluvaliwe.

Iyavikela imvelo, futhi inciphisa kakhulu ukukhiqizwa kwamanzi amdaka, akukho zincibilikisi zemfucuza eziphilayo kanye negesi yemfucuza yemvelo; Ngaphezu kwalokho, indlela yokuhlanza

Azikho izinyibilikisi eziphilayo ezifakwayo, futhi ukungcola okuphezulu kwe-chlorine kuyasuswa ngesikhathi senqubo yokuhlanzwa, ngakho-ke akukho bungozi bekhwalithi kwikhwalithi ye-folic acid.

Le ndlela isebenzisa amanzi njenge-crystallization solvent, kanti isixazululo samanzi esihlanziwe se-1,1, 3-trichloroacetone sisetshenziswa ngqo ekukhiqizweni kwe-folic acid.

Isivuno esiphelele se-folic acid singandiswa ngo-5% ngesisindo, kanti ubumsulwa bungaphezu kuka-99.2% ngesisindo, okungaba sezingeni eliphezulu.

I-folic acid.

Lokhu kusungulwa kuchazwe ngokuningiliziwe ngezindlela ezingezansi.

[0042] Ezindleleni ezilandelayo kanye nezilinganiso, ngaphandle uma kuchazwe ngenye indlela, izinto ezisetshenzisiwe ziyatholakala ngokuthenga kwezentengiselwano, ngaphandle uma kuchazwe ngenye indlela

Indlela esetshenziswayo iyindlela evamile kule nsimu.

Imodeli ye-gas chromatography yayiyi-GC-2014, eyathengwa eShimadzu Company.

I-1,1, 3-trichloroacetone elungiselelwe ngendlela yokuhlanza yale ntsha [0047] ihlanzwa ku-reactor engamalitha angu-50 efakwe ipuleti lesihlungi phansi [0048] Okokuqala, ubumsulwa be-1,1 bungu-65% ngesisindo, i-3-trichloroacetone engu-20Kg kanye namanzi angu-10Kg eketheni yokusabela exutshwe ku-24 uvuselela imizuzu eyi-12, lapho izinga lokuvuselela lingu-200r/min, enkambisweni yokuvuselela ukwengeza amanzi, amanzi ngesilinganiso esingu-300 ml/min, bese ingxube ime imizuzu eyi-10, ihlukaniswe nongqimba lwamafutha oluphansi, isuse ukungcola okuphezulu kwe-chlorine; Okwesibili, izinga lokushisa lesisombululo esingaphezulu esinezingqimba lehliswa libe ngu-5 futhi lavuselelwa amahora ama-2 ngesilinganiso sokuvuselela esingu-100r/min. Ngemuva kwalokho, ikristalu eqinile yatholakala ngqo ngepuleti lesihlungo phansi kwekettle yokusabela ngokuhluzwa kwengcindezi ye-nitrogen ngokucindezela okungu-0.1 MPa, bese ifafazwa futhi ihlanzwe ngamanzi abandayo angu-2 kg. Isisindo esimanzi esingu-1,1, 3-trichloroacetone sasingu-9.8 kg, kanti i-chromatographic pure (GC) yayingu-96.8 wt % [0051] Umsebenzi ohilelekile kule ndlela yokuhlanza, njengokuhlukanisa okungaguquki, ukususa ukungcola okuphezulu kwe-chlorine, ukwakheka kwekristalu, ukuhlunga kanye nokugeza ngamanzi, kungenziwa ohlelweni lomzimba oluvaliwe, olunobungani nemvelo, futhi lunciphisa kakhulu ukukhiqizwa kwamanzi amdaka futhi alukhiqizi imfucuza ye-organic solvent kanye negesi yemfucuza ye-organic [0052]. Ngaphezu kwalokho, ngenxa yokuthi indlela yokuhlanza ngaphandle kokufaka i-organic solvent, kanye ne-chlorine ephezulu yokususa ukungcola enkambisweni yokuhlanza, akukho bungozi bekhwalithi kwikhwalithi ye-folic acid, kodwa futhi ngesibonelo sokusetshenziswa kokulungiswa kwe-1, 1, 3 - folic acid exhunywe ngamanzi e-acetone ancibilikisiwe asetshenziswa ngqo ekukhiqizeni, kwenza i-folic acid ithuthukise isivuno esiphelele 5 isisindo %, ubumsulwa be-99 5 isisindo % Isibonelo 2 [0054] Lolu hlobo lokwenziwa luthi i-1,1, 3-trichloroacetone elungiselelwe ngendlela yokuhlanza yale ntsha [0055] ihlanzwa ku-reactor engamalitha angu-50 efakwe ipuleti lesihlungi phansi [0056] Okokuqala, 1,1 ngobumsulwa obungu-50% , 3-trichloroacetone 20Kg namanzi angu-4Kg axutshwe ku-reactor, evuselela imizuzu eyi-15 ku-45, izinga lokuvuselela elingu-300r/min, enkambisweni yokuvuselela ukwengeza amanzi, amanzi ngesilinganiso esingu-300 ml/min, bese ingxube yahlala imizuzu eyi-15, ihlukaniswe nengqimba kawoyela engezansi, isuse ukungcola okuphezulu kwe-chlorine; Okwesibili, izinga lokushisa lesisombululo sengqimba ephezulu ngemva kokuhlukaniswa kwe-stratification lehliswa laya ku-20, kanti izinga lokuxuba lalingu-200r/min amahora angu-0.5. Ngemuva kwalokho, ikristalu eqinile yatholakala ngqo ngepuleti lesihlungo phansi kwe-reactor ngokuhlunga ingcindezi ye-nitrogen ngengcindezi engu-0.2MPa. Ngemuva kwalokho, ikristalu eqinile yafuthwa futhi yagezwa nge-1Kg yamanzi abandayo angu-25, kanti isisindo esimanzi esingu-1,1, 3-trichloroacetone sasingu-8.2kg ngendlela yokunciphisa. Indlela yokuhlanza ehilelekile ekususweni kwe-static stratification kokungcola okuphezulu kwe-chlorine, i-crystallization, i-filtration kanye nemisebenzi yokugeza ngamanzi ingenziwa ohlelweni lomzimba oluvaliwe, indawo yokusebenza inobungane, futhi inciphisa kakhulu ukukhiqizwa kwamanzi amdaka, akukho nkunkuma ye-organic solvent kanye negesi ye-organic waste [0060] Ngaphezu kwalokho, njengoba le ndlela ingengezi izinyibilikisi eziphilayo futhi isusa ukungcola okuphezulu kwe-chlorine ngesikhathi senqubo yokuhlanza, akukho bungozi bekhwalithi yekhwalithi ye-folic acid, kanti i-1,1, 3-trichloroacetone elungiselelwe yiSibonelo 2 iyancibilika emanzini futhi isetshenziswe ngqo ekukhiqizweni kwe-folic acid, okwandisa isivuno esiphelele se-folic acid ngo-4.9% ngesisindo futhi kufezwe ubumsulwa obungu-99. Le ndlela yokuhlanza ithi i-1,1, 3-trichloroacetone elungiselelwe ngendlela yokuhlanza yale nkampani [0063] ihlanzwa kumalitha angu-50. i-reactor ifakwe ipuleti lesihlungi esicwengekile phansi [0064] Okokuqala, i-1,1 enobumsulwa obungu-60%, i-3-trichloroacetone engu-20Kg exutshwe namanzi angu-40Kg eketheni lokusabela, ivuselela imizuzu engama-30 ku-15, izinga lokuvuselela elingu-100r/min, enkambisweni yokuvuselela ukuze kufakwe amanzi, amanzi ngesilinganiso esingu-500 ml/min, bese ingxube ime imizuzu engama-30, ihlukaniswe nengqimba yamafutha engezansi, isuse ukungcola okuphezulu kwe-chlorine; Okwesibili, izinga lokushisa lesixazululo sengqimba ephezulu ngemva kokuhlukaniswa kwe-stratification lehliswa laya ku-10, kanti izinga lokuvuselela lalingu-100r/min amahora ayi-10. Ngemuva kwalokho, ikristalu eqinile yatholakala ngqo ngepuleti lesihlungi phansi kwe-reactor ngokuhluzwa kwengcindezi ye-nitrogen ngokucindezela okungu-0.2MPa, bese ifafazwa futhi ihlanzwe nge-1Kg yamanzi abandayo ama-5. Isisindo esimanzi se-1,1, 3-trichloroacetone sasingu-6.9kg, kanti i-chromatographic pure (GC) yayingu-98.3% ngesisindo [0067] Umsebenzi ohilelekile kule ndlela yokuhlanza, njengokwakheka kwe-static stratification, ukususwa kokungcola okuphezulu kwe-chlorine, ukwakheka kwekristalu, ukuhlunga kanye nokugeza ngamanzi, kungenziwa ohlelweni lomzimba oluvaliwe, olunendawo yokusebenza enobungane, futhi lunciphisa kakhulu ukukhiqizwa kwamanzi amdaka futhi alukhiqizi imfucuza ye-organic solvent kanye negesi yemfucuza ye-organic [0068]. Ngaphezu kwalokho, ngenxa yokuthi indlela yokuhlanza ngaphandle kokufaka i-organic solvent, kanye ne-chlorine ephezulu yokususa ukungcola enkambisweni yokuhlanza, akukho bungozi bekhwalithi kwikhwalithi ye-folic acid, futhi kuzoba isibonelo ukulungiswa okungu-3 kwe-1, 1, 3 - okuxhunywe nge-cross-linked ne-acetone, amanzi okuncibilikisa, asetshenziswa ngqo ekukhiqizeni i-folic acid, kwenza i-folic acid ithuthukise isivuno esiphelele esingu-5.3 isisindo %, ubumsulwa obungu-99.2 isisindo % Ngokwesilinganiso esingu-1 [0070] i-1,1, 3-trichloroacetone ehlanziwe ngokwendlela yokusebenza 1, ngaphandle kokuthi esinyathelweni (1), amanzi awasetshenziswa, Esikhundleni salokho, kwasetshenziswa i-organic solvents. Ngenxa yalokho, i-1,1, 3-trichloroacetone elungisiwe yancibilikiswa emanzini futhi yasetshenziswa ngqo ekukhiqizeni i-folic acid. Isivuno esiphelele se-folic acid sanda ngo-2% kuphela ngesisindo kanti ubumsulwa babungu-95% ngesisindo. Ngaphezu kwalokho, ngenxa yokwethulwa kwezinyibilikisi eziphilayo kule ndlela yokuhlanza, kunengozi yekhwalithi yekhwalithi ye-folic acid [0071] ngesilinganiso sesi-2 [0072]. I-1,1, 3-trichloroacetone ihlanzwa ngokwendlela eseSibonelweni 1. Umehluko uwukuthi eSinyathelweni (1), inani lamanzi lingu-50Kg, okuholela ekwandeni okukhulu ekukhiqizweni kwamanzi amdaka kanye nokwehla kwe-1. Isivuno samakristalu angu-1,1, 3-trichloroacetone sancibilika emanzini futhi sasetshenziswa ngqo ekukhiqizweni kwe-folic acid, ngakho-ke isivuno esiphelele se-folic acid sanda ngo-5.6% ngesisindo kanye nobumsulwa obungu-99.6% ngesisindo [0073] uma kuqhathaniswa nesilinganiso esingu-3 [0074]. I-1,1 yahlanzwa ngendlela yeSibonelo 1, i-3-trichloroacetone, umehluko uwukuthi esinyathelweni (1), i-heteroplastid ephezulu ye-chlorine ayisuswa, umphumela wokulungiswa kwe-1,1, i-3-trichloroacetone uqukethe inani elikhulu lamakhemikhali ane-chlorine, ikhwalithi yengozi ye-folic acid [0075] Ngokusho kwesibonelo esingenhla 1-3 futhi umphumela wesilinganiso sika-1-3: indlela yokuhlanza ihilela isihlungi sekristalu esinogqinsi esihlanganisiwe ukususa ukungcola okuphezulu kwe-chlorine imisebenzi yokuwasha njengayo yonke ngaphandle kohlelo lomoya, indawo yokusebenza enobungane, futhi inciphise kakhulu ukwanda kwamanzi amdaka, ayikhiqizi igesi engcolile, i-solvent ephilayo kanye ne-organic Ngaphezu kwalokho, ngokusebenzisa icala 1 ukulungiswa kwe-1, 1), i-3-trichloroacetone, engeza encwadini 5/6 ikhasi 7 CN 109516908 Isixazululo samanzi esingu-7, esisetshenziswa ngqo ekukhiqizweni kwe-folic acid, senza isivuno esiphelele se-folic acid sande ngo-5% ngesisindo, ubumsulwa bungu-99.2% ngesisindo ngenhla; Ngaphezu kwalokho, ngoba indlela yokuhlanza ayilethi i-organic solvent, ayikho ingozi yekhwalithi kwikhwalithi ye-folic acid. Ngaphezu kwalokho, indlela yokuhlanza isebenzisa amanzi njenge-crystallization solvent, kanti isixazululo samanzi esihlanziwe se-1,1, 3-trichloroacetone sisetshenziswa ngqo ekukhiqizweni kwe-folic acid, okunciphisa ukusabela okungekuhle.

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