Kwelinye icala, le mveliso ibonelela ngendlela yokucoca i-1,1, 3-trichloroacetone, apho le ndlela ibandakanya la manyathelo alandelayo.

Ifleshi:

(1) I-1,1, i-3-trichloroacetone ekrwada exutywe namanzi;

(2) Ukuphinda kusetyenziswe isisombululo esingaphezulu emva kokuma; Kanye

(3) iikristale eziqinileyo eziphinde zahluzwa ziyahluzwa zize zihlanjwe ngamanzi;

Apho, kwiNyathelo (1), umlinganiselo wobunzima be-crude 1,1, 3-trichloroacetone ekhankanyiweyo kubungakanani bamanzi yi-10.1-2).

Kungcono, kwiNyathelo (1), umlinganiselo wobunzima bemveliso eluhlaza eyi-1,1, 3-trichloroacetone kubungakanani bamanzi unokuba yi-1:

(0.4-0.6), iphuculwe ngakumbi njenge-1:0.5; Kolu vumbululo, umthamo we-1,1, 3-trichloroacetone crude product kunye namanzi ulawulwa koku kungasentla.

Uluhlu lococeko oluphezulu lwe-1,1, 3-trichloroacetone lunokufunyanwa.

Ngokwesi sixhobo sitsha, kwinyathelo (1), imveliso eluhlaza ye-1,1, 3-trichloroacetone kunye namanzi zinokulungiswa kubushushu be-10-50℃

Xuba imizuzu eli-10-30 phantsi kweemeko ezithile, uze uyiyeke ime imizuzu eli-10-30; Kungcono, kwiNyathelo (1), kuthiwe i-1,1, i-3-trichloropropyl

I-ketone eluhlaza ixutywe namanzi kubushushu obuyi-30-35℃ imizuzu engama-25-30, yaze yema imizuzu eli-10-15; Kule nto intsha yangoku.

, kusetyenziswa i-1,1, 3-trichloroacetone crude njengezinto eziluhlaza, kwiketile yokusabela, ixutywe namanzi, ixutywe kubushushu obuthile emva kokuma

Ukususwa kwe-oyile. Emva kokususwa kwe-oyile, umaleko weoyile osezantsi uyasuswa, ngokuyintloko ngokususa ukungcola okuphezulu kwe-chlorine kwaye kushiyeke isisombululo esiphezulu ukuze sisetyenziswe kamva.

Ngokwesi sivumbululo, kwinyathelo (1), i-crude 1, 1, 3-trichloroacetone ixutywe namanzi kwaye ingaxutywa

Iimeko, apho kungekho mda uthile kwiimeko zokuxukuxa nezixhobo, lo gama nje i-1,1, 3-trichloroacetone inokuba rhabaxa

Imveliso ingaxutywa ngokulinganayo namanzi. Kungcono ukuba izinga lokuxuba libe yi-100-300r/min.

Kule mveliso intsha, kungcono ukuba amanzi abe ngamanzi angena-ion.

Ngokwesi sixhobo, kwinqanaba (2), iimeko zokuphinda kusetyenziswe i-crystallization zingaba: ubushushu ukusuka kwi-0 ukuya kwi-35℃, ixesha ukusuka kwi-0.5 -

Iiyure ezili-10, kungcono, ukuphinda kusetyenziswe i-crystallization kwenziwa ngesantya sokuxukuxa se-50-300 RPM; Kungcono, ukuphinda kusetyenziswe i-reknot

Amanzi akwafakwa kwinkqubo yokwenza ikristale, apho amanzi ongezwa ngesantya se-200-600 ml/min; Phantsi kwezi meko, ukusebenza kakuhle kwe-recrystallization

Isiqhamo silungile.

[0034] Ngaphezulu, iimeko zokuphinda kusetyenziswe kwakhona zezi: ubushushu obuyi-10-15℃, ixesha leeyure ezi-2-3, kunye neemeko zokuphinda kusetyenziswe kwakhona.

Ikristale ixutywa ngesantya se-100-200 RPM kwaye amanzi ongezwa ngesantya se-300-500 ml/min.

Phantsi kwezi meko, isiphumo sokuphinda sisetyenziswe singcono.

Kule nto intsha, ubushushu bokuphinda kusetyenziswe obuchazwe kwinyathelo (2) buphantsi kune-1,1, 3-trichloroacetone kwinyathelo (1)

Ubushushu apho imveliso ixutywa khona namanzi.

Ngokwesi sivumbululo, kwiNyathelo (3), umxube wempendulo emva kweNyathelo (2) unokuhluzwa ngoxinzelelo oluvaliweyo, okanye ungenziwa

Iikristale eziqinileyo zifumaneka ngokucinezela ngqo kwipleyiti yesihluzo ezantsi kwe-reactor. Kule mveliso intsha, kungcono ukusebenzisa umoya kunye/okanye i-nitrogen.

Ukucoca uxinzelelo, kungcono ukusebenzisa i-nitrogen ekuhluzeni uxinzelelo, kwaye uxinzelelo lungaba yi-0.1-0.2MPa, kungcono i-0.12 -

0. 18 mpa.

Ngokwesi sixhobo, ikristale ehlanjwe emva kokuhluzwa koxinzelelo ihlanjwa ngamanzi, apho amanzi akhankanyiweyo ahlanjwa khona.

Akukho mda uthile, umzekelo, ungakhetha i-1-2kg yokuhlamba ngamanzi phantsi kobushushu obuyi-2-25℃, kwaye utshize.

Akukho mda wesantya uthile.

Ngokwesi sixhobo, ubunyulu bemveliso eluhlaza ye-1,1, 3-trichloroacetone bunokuba yi-50-65% ngobunzima.

Amaphepha 3/6 emiyalelo

5

I-CN 109516908 A

5

Kwelinye icala, olu vumbululo lukwabonelela nge-folic acid elungiselelwe nayiphi na indlela echazwe apha ngasentla.

Isisombululo samanzi se-1,1, 3-trichloroacetone sisetyenziswa ngokuthe ngqo ekulungiseleleni i-folic acid.

Ukusebenza kwendlela yokucoca le mveliso, efana nokukhupha izinto ezidityanisiweyo, ukuhluza ikristale njalo njalo, kungenziwa kwinkqubo evaliweyo.

Iyakhathalela okusingqongileyo, kwaye inciphisa kakhulu ukuveliswa kwamanzi amdaka, akukho zinyibilikisi zendalo kunye negesi yenkunkuma yendalo; Ukongeza, indlela yokucoca

Akukho zinyibilikisi ze-organic ezifakwayo, kwaye ukungcola okuphezulu kwe-chlorine kuyasuswa ngexesha lenkqubo yokucoca, ngoko ke akukho mngcipheko kumgangatho we-folic acid.

Le ndlela isebenzisa amanzi njengesinyibilikisi sekristale, kwaye isisombululo samanzi esicociweyo se-1,1, 3-trichloroacetone sisetyenziswa ngokuthe ngqo kwimveliso ye-folic acid.

Isivuno sipheleleyo se-folic acid singanyuswa nge-5% ngobunzima, kwaye ubumsulwa bungaphezulu kwe-99.2% ngobunzima, nto leyo enokufumana umgangatho ophezulu.

Ye-folic acid.

Olu vumbululo luchazwe ngokweenkcukacha ngeendlela ezingezantsi.

[0042] Kwimifuziselo elandelayo kunye nomlinganiselo, ngaphandle kokuba kuchazwe ngenye indlela, izixhobo ezisetyenzisiweyo ziyafumaneka ngokuthenga ngorhwebo, ngaphandle kokuba kuchazwe ngenye indlela

Indlela esetyenzisiweyo yindlela eqhelekileyo kweli candelo.

Imodeli ye-gas chromatography yayiyi-GC-2014, yathengwa kwiShimadzu Company.

I-1,1, 3-trichloroacetone elungiselelwe ngendlela yokucoca yale mveliso [0047] icocwa kwi-reactor ye-50-litre exhotyiswe ngepleyiti yesihluzo ezantsi [0048] Okokuqala, ubunyulu be-1,1 buyi-65% ngobunzima, i-3-trichloroacetone eyi-20Kg kunye namanzi ayi-10Kg kwi-kettle yokusabela exutywe kwi-24 ukuxuba imizuzu eli-12, apho izinga lokuxuba liyi-200r/min, kwinkqubo yokuxuba ukongeza amanzi, amanzi ngesantya se-300 ml/min, uze emva koko umxube ume imizuzu eli-10, wahlulwe kumaleko weoyile osezantsi, ususe ukungcola okuphezulu kwe-chlorine; Okwesibini, ubushushu besisombululo esingaphezulu esinamaleko behliswa ukuya kwi-5 kwaye buxutywe iiyure ezi-2 ngesantya sokuxuba se-100r/min. Emva koko, ikristale eqinileyo ifunyenwe ngqo ngepleyiti yesihluzo ezantsi kweketile yokusabela ngokuhluza uxinzelelo lwe-nitrogen kuxinzelelo lwe-0.1 MPa, emva koko yatshizwa yaza yahlanjwa ngamanzi abandayo angama-2 kg. Ubunzima obumanzi be-1,1, 3-trichloroacetone yayiyi-9.8 kg, kwaye i-chromatographic pure (GC) yayiyi-96.8 wt % [0051] Umsebenzi obandakanyekayo kule ndlela yokucoca, njengokuhluzwa okungashukumiyo, ukususa ukungcola okuphezulu kwe-chlorine, i-crystallization, i-filtration kunye nokuhlamba ngamanzi, unokwenziwa kwinkqubo yomzimba evaliweyo, enobuhlobo nokusingqongileyo, kwaye inciphisa kakhulu ukuveliswa kwamanzi amdaka kwaye ayivelisi inkunkuma ye-organic solvent kunye negesi yenkunkuma yendalo [0052]. Ukongeza, kuba indlela yokucoca ngaphandle kokungenisa isinyibilikisi sendalo, kunye ne-chlorine ephezulu yokususa ukungcola kwinkqubo yokucoca, akukho mngcipheko kumgangatho we-folic acid, kodwa nangomzekelo wokusetyenziswa kokulungiswa kwe-1, 1, 3 - folic acid edityaniswe namanzi e-acetone anyibilikisiweyo asetyenziswa ngqo kwimveliso, yenza i-folic acid iphucule isivuno iyonke sibe yi-5 ubunzima %, ubunyulu be-99 5 ubunzima % Umzekelo 2 [0054] Olu hlobo lubonisa ukuba i-1,1, 3-trichloroacetone elungiselelwe yindlela yokucoca yale vumbululo [0055] ihlanjululwa kwi-reactor ye-50-litre exhotyiswe ngepleyiti yesihluzo ezantsi [0056] Okokuqala, i-1,1 enobunyulu be-50%, i-3-trichloroacetone 20Kg kunye namanzi e-4Kg axutywe kwi-reactor, exutywa imizuzu eli-15 kwi-45, izinga lokuxuba le-300r/min, kwinkqubo yokuxuba ukongeza amanzi, amanzi ngesantya se-300 ml/min, kwaye emva koko Umxube wema imizuzu eli-15, wahlulwe kumaleko weoyile osezantsi, susa ukungcola okuphezulu kwe-chlorine; Okwesibini, ubushushu besisombululo somaleko ongaphezulu emva kokuhluzwa kwe-stratification behliswa ukuya kuma-20, kwaye izinga lokuxuba libe yi-200r/min kangangeeyure eziyi-0.5. Emva koko, i-crystal eqinileyo yafunyanwa ngqo ngepleyiti yesihluzo ezantsi kwe-reactor ngokuhluza uxinzelelo lwe-nitrogen kuxinzelelo lwe-0.2MPa. Emva koko, ikristale eqinileyo yatshizwa yaza yahlanjwa nge-1Kg yamanzi abandayo angama-25, kwaye ubunzima obumanzi be-1,1, 3-trichloroacetone babuyi-8.2kg ngendlela yokunciphisa. Indlela yokucoca ebandakanyeka ekususweni kwe-static stratification yokungcola okuphezulu kwe-chlorine, i-crystallization, i-filtration kunye nemisebenzi yokuhlamba amanzi ingenziwa kwinkqubo yomzimba evaliweyo, imeko yokusebenza inobuhlobo, kwaye inciphisa kakhulu ukuveliswa kwamanzi amdaka, akukho nkunkuma ye-organic solvent kunye negesi yenkunkuma yendalo [0060] Ukongeza, ekubeni le ndlela ingangenisi izinyibilikisi ze-organic kwaye isusa ukungcola okuphezulu kwe-chlorine ngexesha lenkqubo yokucoca, akukho mngcipheko kumgangatho we-folic acid, kwaye i-1,1, 3-trichloroacetone elungiselelwe nguMzekelo 2 iyanyibilika emanzini kwaye isetyenziswa ngokuthe ngqo kwimveliso ye-folic acid, inyusa isivuno sipheleleyo se-folic acid nge-4.9% ngobunzima kwaye ifezekisa ubumsulwa be-99. Le ndlela ithi i-1,1, 3-trichloroacetone elungiselelwe yindlela yokucoca yale vumbululo [0063] ihlanjululwa kwi-50-litre. i-reactor ifakwe ipleyiti yesihluzo esisezantsi [0064] Okokuqala, i-1,1 enobumsulwa be-60%, i-3-trichloroacetone 20Kg ixutywe namanzi i-40Kg kwi-kettle yokusabela, ivuselela imizuzu engama-30 kwi-15, izinga lokuvuselela le-100r/min, kwinkqubo yokuvuselela ukongeza amanzi, amanzi ngesantya se-500 ml/min, uze emva koko umxube ume imizuzu engama-30, wahlulwe kumaleko weoyile osezantsi, ususe ukungcola okuphezulu kwe-chlorine; Okwesibini, ubushushu besisombululo somaleko ongaphezulu emva kokuhluzwa kwe-stratification behlisiwe ukuya kwi-10, kwaye izinga lokuvuselela libe yi-100r/min iiyure ezili-10. Emva koko, i-crystal eqinileyo ifunyenwe ngqo ngepleyiti yesihluzo ezantsi kwe-reactor ngokuhluza uxinzelelo lwe-nitrogen kuxinzelelo lwe-0.2MPa, emva koko yatshizwa yaza yahlanjwa nge-1Kg yamanzi abandayo ama-5. Ubunzima obumanzi be-1,1, 3-trichloroacetone yayiyi-6.9kg, kwaye i-chromatographic pure (GC) yayiyi-98.3% ngobunzima [0067]. Umsebenzi obandakanyekayo kule ndlela yokucoca, njengokwakheka kwe-static, ukususa ukungcola okuphezulu kwe-chlorine, i-crystallization, i-filtration kunye nokuhlamba ngamanzi, unokwenziwa kwinkqubo yomzimba evaliweyo, enendawo yokusebenza enobuhlobo, kwaye inciphisa kakhulu ukuveliswa kwamanzi amdaka kwaye ayivelisi inkunkuma ye-organic solvent kunye ne-organic waste gas [0068]. Ukongeza, kuba indlela yokucoca ngaphandle kokungenisa isinyibilikisi sendalo, kunye ne-chlorine ephezulu yokususa ukungcola kwinkqubo yokucoca, akukho mngcipheko kumgangatho we-folic acid, kwaye umzekelo iya kuba yi-3 yokulungiselela i-1, 1, 3 - edityaniswe ne-acetone, amanzi okunyibilikisa, esetyenziswa ngokuthe ngqo ekuveliseni i-folic acid, yenza i-folic acid ukuphucula isivuno iyonke yi-5.3 ubunzima %, ubumsulwa be-99.2 ubunzima % Kwi-1 proportions [0070] i-1,1, 3-trichloroacetone ecociweyo ngokwendlela yokwenziwa 1, ngaphandle kokuba kwinyathelo (1), amanzi akasetyenziswa, Endaweni yoko, kwasetyenziswa izinyibilikisi zendalo. Ngenxa yoko, i-1,1, 3-trichloroacetone elungisiweyo yanyibilika emanzini yaza yasetyenziswa ngokuthe ngqo ekuveliseni i-folic acid. Isivuno sipheleleyo se-folic acid sandiswe kuphela yi-2% ngobunzima kwaye ubumsulwa be-95% ngobunzima. Ukongeza, ngenxa yokungeniswa kwezinyibilikisi ze-organic kule ndlela yokucoca, kukho umngcipheko womgangatho womgangatho we-folic acid [0071] ngokwesilinganiselo sesi-2 [0072]. I-1,1, 3-trichloroacetone iyahlanjululwa ngokwendlela ekuMzekelo 1. Umahluko kukuba kwiNyathelo (1), ubungakanani bamanzi yi-50Kg, nto leyo ebangela ukwanda okukhulu kokuveliswa kwamanzi amdaka kunye nokwehla kwe-1. Isivuno se-1,1, 3-trichloroacetone crystals sanyibilika emanzini kwaye sasetyenziswa ngokuthe ngqo kwimveliso ye-folic acid, ngoko ke isivuno sipheleleyo se-folic acid sandiswe kuphela yi-5.6% ngobunzima kwaye ubumsulwa babuyi-99.6% ngobunzima [0073] ngokuchasene nomlinganiselo we-3 [0074]. I-1,1 ihlanjululwe ngendlela yoMzekelo 1, i-3-trichloroacetone, umahluko kukuba kwinyathelo (1), i-heteroplastid ephezulu ye-chlorine ayisuswa, isiphumo sokulungiswa kwe-1,1, i-3-trichloroacetone iqulethe inani elikhulu leekhompawundi ze-chlorine, umgangatho wengozi ye-folic acid [0075] Ngokomzekelo ongentla 1-3 kwaye sisiphumo sesikali se-1-3: indlela yokucoca ibandakanya isihluzo sekristale esinomgangatho omaleko ukususa ukungcola okuphezulu kwe-chlorine imisebenzi yokuhlamba efana nayo yonke into ngaphandle kwenkqubo yomoya, indawo yokusebenza enobuhlobo, kwaye inciphise kakhulu ukwanda kwamanzi amdaka, ayivelisi igesi emdaka, isinyibilikisi se-organic kunye ne-organic Ukongeza, ngokusebenzisa imeko 1 ukulungiswa kwe-1, 1), 3-trichloroacetone, yongeza kwincwadi 5/6 iphepha 7 CN 109516908 Isisombululo samanzi se-7, esisetyenziswa ngokuthe ngqo kwimveliso ye-folic acid, senza isivuno sipheleleyo se-folic acid sande nge-5% ngobunzima, ubumsulwa yi-99.2% ngobunzima ngasentla; Ngaphezu koko, kuba indlela yokucoca ayingenisi isinyibilikisi sendalo, akukho mngcipheko kumgangatho we-folic acid. Ngaphezu koko, indlela yokucoca isebenzisa amanzi njengesinyibilikisi sekristale, kwaye isisombululo samanzi esicociweyo se-1,1, 3-trichloroacetone sisetyenziswa ngokuthe ngqo kwimveliso ye-folic acid, nto leyo enciphisa iziphumo ebezingalindelekanga.

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