Ngakolunye uhlangothi, ukuveliswa kunika indlela yokuhlanjululwa kwe-1,1, 3-trichloroacetone, apho indlela iquka la manyathelo alandelayo.
Ifleshi:
(1) Ekrwada 1,1, 3-trichloroacetone exutywe namanzi;
(2) Ukuhlaziywa kwakhona kwesisombululo esiphezulu emva kokuma; Njengo
(3) iikristale eziqinileyo ezenziwe ngokutsha ziyahluzwa zize zihlanjwe ngamanzi;
Apho, kwiNyathelo (1), umlinganiselo wobunzima bobukrwada obuxeliweyo 1,1, 3-trichloroacetone kubungakanani bamanzi ngu-1
0.1-2).
Ngokukhethekileyo, kwiNyathelo (1), umlinganiselo wobunzima bemveliso ekrwada ye-1,1, 3-trichloroacetone kubungakanani bamanzi unokuba ngu-1:
(0.4-0.6), iphuculwe ngakumbi njenge-1: 0.5; Ekuvelisweni, umthamo we-1,1, 3-trichloroacetone imveliso ekrwada kunye namanzi ilawulwa apha ngasentla.
Uluhlu lokucoceka okuphezulu kwe-1,1, i-3-trichloroacetone inokufumaneka.
Ngokutsho koyilo lwangoku, kwinyathelo (1), i-1,1, 3-trichloroacetone imveliso ekrwada kunye namanzi inokulungiswa kubushushu obuyi-10-50℃
Hlanganisa imizuzu eyi-10-30 phantsi kweemeko, uze uvumele ukuma imizuzu eyi-10-30; Ngokukhethekileyo, kwiNyathelo (1), uthe 1,1, 3-trichloropropyl
I-ketone ekrwada ixutywe namanzi kwiqondo lobushushu le-30-35℃ imizuzu engama-25-30, emva koko yema imizuzu eyi-10-15; Kwimveliso yangoku
, usebenzisa i-1,1, i-3-trichloroacetone ekrwada njengento ekrwada, kwiketile yokusabela, ixutywe namanzi, ivuselelwe kubushushu obuthile emva kokuma.
I-Delamination. Emva kwe-delamination, i-oyile ephantsi iyasuswa, ngokukodwa ngokususa ukungcola okuphezulu kweklorini kunye nokushiya isisombululo esiphezulu sokusetyenziswa kamva.
Ngokwendlela yokuyila, kwinyathelo (1), i-1,1, 3-trichloroacetone ekrwada ixutywe namanzi kwaye inokushukunyiswa.
Iimeko, apho kungekho mda ukhethekileyo kwiimeko ezishukumisayo kunye nezixhobo, ukuba nje i-1,1, 3-trichloroacetone ingaba rhabaxa.
Imveliso inokuxutywa ngokulinganayo ngamanzi. Ngokukhethekileyo, izinga lokuxuba liyi-100-300r / min.
Kwimveliso yangoku, amanzi akhethwa ukuba angabikho.
Ngokutsho kokuqanjwa, kwinyathelo (2), iimeko zokuphinda zenziwe kwakhona: ubushushu ukusuka kwi-0 ukuya kwi-35 ℃, ixesha ukusuka kwi-0.5 -
Iiyure ze-10, ngokukhethekileyo, i-recrystallization iqhutyelwa kwinqanaba elishukumisayo le-50-300 RPM; Ngokukhethekileyo, i-reknot
Amanzi aphinda afakwe kwinkqubo ye-crystallization, apho amanzi afakwe kwizinga le-200-600 ml / min; Phantsi kwezi meko, recrystallization ukusebenza kakuhle
Isiqhamo silungile.
[0034] Ngaphezulu ngokufanelekileyo, iimeko zokuhlaziya: iqondo lokushisa le-10-15 ℃, ixesha leeyure ze-2-3, kunye neemeko zokuvuselela
I-crystal ishukunyiswa kwinqanaba le-100-200 RPM kwaye amanzi ayongezwa kwinqanaba le-300-500 ml / min.
Ngaphantsi kwezi meko, i-recrystallization effect ingcono.
Kwimveliso yangoku, iqondo lobushushu le-recrystallization elichazwe kwisinyathelo (2) lingaphantsi kune-1,1, i-3-trichloroacetone kwinqanaba (1)
Iqondo lokushisa apho imveliso ixutywe namanzi.
Ngokutsho kokuqanjwa, kwiNyathelo (3), umxube wokuphendula emva kweNyathelo (2) unokuhluzwa ngoxinzelelo oluvaliweyo, okanye unokuba
Iikristale eziqinileyo zifumaneka ngokucinezela ngokuthe ngqo kwipleyiti ye-sieve ezantsi kwe-reactor. Kuyilo lwangoku, umoya kunye/okanye initrogen ikhethwa ukuba isetyenziswe
Ukuhluzwa koxinzelelo, kungcono ukusebenzisa i-nitrogen yoxinzelelo loxinzelelo, kwaye uxinzelelo lunokuba ngu-0.1-0.2MPa, ngokukhetha i-0.12 -
0. 18 mpa.
Ngokokuqulunqwa, ikristale enamanzi emva koxinzelelo lokucoca ihlanjwa ngamanzi, apho amanzi axeliweyo ahlanjwa khona.
Akukho mda othile, umzekelo, ungakhetha i-1-2kg yokuhlamba amanzi phantsi kwemeko yobushushu be-2-25 ℃, kunye nokutshiza.
Akukho mda ukhethekileyo wesantya.
Ngokutsho kokuqanjwa, ukucoceka kwe-1,1, i-3-trichloroacetone yemveliso ekrwada ingaba yi-50-65 % ubunzima.
Amaphepha 3/6 omyalelo
5
CN 109516908 A
5
Ukuveliswa kwangoku, ngakolunye uhlangothi, kunika i-folic acid elungiselelwe nayiphi na indlela echazwe ngasentla
Isisombululo samanzi se-1,1, i-3-trichloroacetone isetyenziselwa ngokuthe ngqo ukulungisa i-folic acid.
Ukusebenza kwendlela yokuhlanjululwa kwemveliso, njenge-stratified extraction, i-crystallization filtration kunye nokunye, kunokwenziwa kwindlela evaliweyo.
Imeko-bume, kwaye inciphisa kakhulu ukuveliswa kwamanzi amdaka, akukho nkunkuma ye-solvents ye-organic kunye ne-organic waste gas; Ukongeza, indlela yokucoca
Akukho zinyibilikisi eziphilayo zingeniswa, kwaye ukungcola okuphezulu kweklorini kuyasuswa ngexesha lenkqubo yokucoca, ngoko akukho mngcipheko wekhwalithi kumgangatho we-folic acid.
Indlela isebenzisa amanzi njenge-crystallization solvent, kunye nesisombululo se-aqueous ecocekileyo ye-1,1, i-3-trichloroacetone isetyenziselwa ngokuthe ngqo ukuveliswa kwe-folic acid.
Isivuno esipheleleyo se-folic acid sinokunyuswa nge-5% ngobunzima, kwaye ubunyulu bungaphezulu kwe-99.2% ngobunzima, obunokufumana umgangatho ophezulu.
Kwi-folic acid.
Ukuqanjwa kuchazwe ngokweenkcukacha ngokusebenzisa i-embodiments engezantsi.
[0042] Kolu phawu lulandelayo kunye nomlinganiselo, ngaphandle kokuba kuchazwe ngenye indlela, izinto ezisetyenziswayo zifumaneka ngokuthengwa kwezorhwebo, ngaphandle kokuba kuchazwe ngenye indlela.
Indlela esetyenziswayo yindlela eqhelekileyo kulo mmandla.
Imodeli yechromatography yegesi yayiyi-GC-2014, ethengwe kwiNkampani yeShimadzu.
I-1,1, i-3-trichloroacetone elungiselelwe yindlela yokuhlanjululwa kwezinto ezikhoyo ngoku [0047] ihlanjululwe kwi-reactor ye-50-litre exhotywe ngepleyiti yesihluzo ezantsi [0048] Okokuqala, ukucoceka kwe-1,1 yi-65 I-% ngobunzima, i-3-trichloroacetone 20Kg kunye namanzi 10Kg kwi-kettle yokusabela exutywe kwi-24 evuselela imizuzu eyi-12, apho izinga lokuvuselela liyi-200r / min, kwinkqubo yokuvuselela ukongeza amanzi, amanzi kwinqanaba le-300 ml / min. , kwaye ke umxube wema imizuzu eyi-10, uhlukaniswe kwi-oyile ephantsi, ususe ukungcola okuphezulu kwe-chlorine; Okwesibini, iqondo lokushisa lesisombululo esiphezulu se-layer liye lancitshiswa ukuya kwi-5 kwaye lixutywe ngeeyure ze-2 kwisantya esichukumisayo se-100r / min. Emva koko, i-crystal eqinile yafunyanwa ngokuthe ngqo kwi-plate ye-sieve ezantsi kwe-kettle yokusabela ngokucoca ngoxinzelelo lwe-nitrogen kuxinzelelo lwe-0.1 MPa, kwaye emva koko itshizwe kwaye ihlanjwe nge-2 kg yamanzi abandayo. Ubunzima obumanzi be-1,1, i-3-trichloroacetone yayingu-9.8 kg, kwaye i-chromatographic pure (GC) yayingu-96.8 wt% [0051] Umsebenzi obandakanyekayo kule ndlela yokucoca, njenge-static stratification, ukususwa kokungcola okuphezulu kwe-chlorine, i-crystallization, ukuhluzwa kunye nokuhlamba kwamanzi, kunokuqhutyelwa kwinkqubo yomzimba evaliweyo, ehambelana nokusingqongileyo, kwaye inciphisa kakhulu isizukulwana samanzi angcolileyo kwaye ayivelisi inkunkuma ye-solvent kunye ne-organic waste gas [0052]. Ukongeza, ngenxa yokuba indlela yokucoca ngaphandle kokuzisa i-solvent ye-organic, kunye ne-chlorine ephezulu yokususa ukungcola kwinkqubo yokucoca, akukho mngcipheko womgangatho kumgangatho we-folic acid, kodwa nangomzekelo wokuphunyezwa kokulungiswa kwe-1, 1, 3 - folic acid cross-ezinxulunyaniswa ne-acetone amanzi inyibilika ngqo esetyenziswa kwimveliso, yenza folic acid ukuphucula isivuno jikelele 5 ubunzima %, ukusulungeka 99 5 ubunzima % Umzekelo 2 [0054] Le embodiment ithi 1,1, 3-trichloroacetone elungiselelwe ngu. indlela yokuhlanjululwa kwemveliso yangoku [0055] ihlanjululwe kwi-reactor ye-50-litre exhotyiswe ngepleyiti yesihluzo ezantsi [0056] Okokuqala, 1,1 ngococeko lwe-50% , 3-trichloroacetone 20Kg kunye namanzi 4Kg exutywe kwi-reactor, ivuselela imizuzu eyi-15 kwi-45, isantya esishukumisayo se-300r / min, kwinkqubo yokuvuselela ukongeza amanzi, amanzi ngesantya se-300 ml / min, kwaye emva koko umxube wema imizuzu eyi-15, wahlukana ne i-oyile ephantsi, ukususa ukungcola okuphezulu kwe-chlorine; Okwesibini, ubushushu besisombululo soluhlu oluphezulu emva kokuba i-stratification iyancipha ukuya kwi-20, kwaye izinga lokuvuselela laliyi-200r / min kwi-0.5 h. Emva koko, i-crystal eqinile yafunyanwa ngokuthe ngqo kwi-sieve plate ezantsi kwe-reactor ngokucoca ngoxinzelelo lwe-nitrogen kuxinzelelo lwe-0. 2MPa. Emva koko, i-crystal eqinile yafafazwa kwaye ihlanjwe nge-1Kg yamanzi abandayo angama-25, kunye nobunzima obumanzi be-1,1, i-3-trichloroacetone yayiyi-8.2kg ngendlela yokunciphisa Indlela yokucoca ebandakanyekayo ekususweni kwe-static stratification yokungcola okuphezulu kwe-chlorine, crystallization, filtration kunye nemisebenzi yokuhlamba amanzi inokuqhutywa kwinkqubo yomzimba evaliweyo, indawo yokusebenza inobubele, kwaye inciphisa kakhulu ukuveliswa kwamanzi amdaka, akukho nkunkuma ye-solvent kunye nerhasi yenkunkuma [0060] Ukongeza, ekubeni le ndlela yenza angazisi izinyibilikisi zezinto eziphilayo kwaye asuse ukungcola okuphezulu kweklorine ngexesha lenkqubo yokucoca, akukho mngcipheko womgangatho kumgangatho we-folic acid, kunye ne-1,1, i-3-trichloroacetone elungiselelwe nguMzekelo 2 ichithwa emanzini kwaye isetyenziswe ngokuthe ngqo kwimveliso i-folic acid, ukwandisa isivuno esipheleleyo se-folic acid nge-4.9% ngobunzima kunye nokufezekisa ukucoceka kwe-99 Le embodiment ithi i-1,1, i-3-trichloroacetone elungiselelwe yindlela yokuhlanjululwa kwemveliso yangoku [0063] ihlanjululwe kwi-50 -ilitha i-reactor ifakwe ipleyiti yesihluzo ezantsi [0064] Okokuqala,1,1 ngococeko lwe-60%, i-3-trichloroacetone 20Kg ixutywe namanzi 40Kg kwi-kettle yokusabela, ivuselela imizuzu engama-30 kwi-15, izinga lokuvuselela. of 100r/min, kwinkqubo yokuxhokonxa ukongeza amanzi, amanzi ngesantya 500 ml / min, kwaye ke umxube wema imizuzu engama-30, ahlulwe umaleko oyile esezantsi, ukususa ukungcola chlorine eliphezulu; Okwesibini, ubushushu besisombululo soluhlu oluphezulu emva kokuba i-stratification iyancipha ukuya kwi-10, kwaye izinga lokuvuselela laliyi-100r / min kwiiyure ze-10. Emva koko, i-crystal eqinile yafunyanwa ngokuthe ngqo kwi-sieve plate ezantsi kwe-reactor ngokucoca ngoxinzelelo lwe-nitrogen kuxinzelelo lwe-0.2MPa, kwaye emva koko ifafazwe kwaye ihlanjwe nge-1Kg ye-5 yamanzi abandayo. Ubunzima obumanzi be-1,1, i-3-trichloroacetone yayingu-6.9kg, kwaye i-chromatographic pure (GC) yayingu-98.3% ngobunzima [0067] Umsebenzi obandakanyekayo kule ndlela yokucoca, njenge-static stratification, ukususwa kokungcola okuphezulu kwe-chlorine, i-crystallization. , ukuhluzwa kunye nokuhlamba kwamanzi, kunokuqhutyelwa kwinkqubo yomzimba evaliweyo, enendawo yokusebenza enobungane, kwaye inciphisa kakhulu ukuveliswa kwamanzi amdaka kwaye ayivelisi inkunkuma ye-solvent kunye ne-organic waste gas [0068]. Ukongeza, ngenxa yokuba indlela yokucoca ngaphandle kokuzisa i-solvent ye-organic, kunye ne-chlorine ephezulu yokususa ukungcola kwinkqubo yokucoca, akukho mngcipheko wekhwalithi kumgangatho we-folic acid, kwaye iya kuba ngumzekelo we-3 ukulungiswa kwe-1, 1, 3 - cross- edityaniswe ne-acetone, amanzi okuchithwa, asetyenziswe ngokuthe ngqo kwimveliso ye-folic acid, yenza i-folic acid iphucule isivuno esipheleleyo 5. 3 ubunzima %, ukucoceka kwe-99. 2 ubunzima % Ngomlinganiselo we-1 [0070] uhlanjululwe 1,1, 3- i-trichloroacetone ngokwendlela ye-embodiment 1, ngaphandle kokuba kwinqanaba (1), amanzi awasetyenziswanga, Endaweni yoko, kusetyenziswe izinyibilikisi eziphilayo. Ngenxa yoko, i-1,1, i-3-trichloroacetone elungiselelwe yachithwa emanzini kwaye isetyenziswe ngokuthe ngqo kwimveliso ye-folic acid. Isivuno esipheleleyo se-folic acid sanyuswa kuphela nge-2 % ngobunzima kwaye ukucoceka kwaba ngama-95 % ubunzima. Ukongezelela, ngenxa yokuqaliswa kwee-solvents eziphilayo kule ndlela yokucoca, kukho umngcipheko womgangatho kumgangatho we-folic acid [0071] ngokwe-2 [0072]. I-1,1, i-3-trichloroacetone ihlanjululwa ngokwendlela ekuMzekeliso 1. Umahluko kukuba kwiNyathelo (1), umthamo wamanzi ngu-50Kg, okubangelwa ukwanda okukhulu kokuveliswa kwamanzi amdaka kunye nokuncipha kwe-1 The isivuno se-1,1, i-3-trichloroacetone crystals yachithwa emanzini kwaye isetyenziswe ngokuthe ngqo kwimveliso ye-folic acid, ukwenzela ukuba isivuno esipheleleyo se-folic acid sande kuphela nge-5.6% ngobunzima kwaye ubunyulu be-99.6% ngesisindo [0073] ] ngokuchasene nomlinganiselo we-3 [0074]. I-1,1 yahlanjululwa ngendlela yoMzekelo 1, 3-trichloroacetone, umahluko kukuba kwinqanaba (1), i-chlorine ephezulu ye-heteroplastid ayisuswanga, umphumo wokulungiswa kwe-1,1, 3-trichloroacetone iqulethe enkulu inani leekhompawundi chlorinated, umgangatho folic acid ingozi [0075] Ngokutsho lo mzekelo ungasentla 1-3 kwaye sisiphumo isikali 1-3: indlela yokucoca ibandakanya let stand layered crystal filter ukususa imisebenzi yokuhlamba ukungcola chlorine ephezulu. njengazo zonke kodwa kwinkqubo yomoya, indawo yokusebenza enobuhlobo, kwaye yanciphisa kakhulu iziganeko zamanzi amdaka, ayivelisi inkunkuma yegesi, i-solvent ye-organic kunye ne-organic Ukongeza, ngokuphumeza ityala 1 ukulungiswa kwe-1, 1), 3-trichloroacetone. , yongeza kwincwadi ye-5/6 iphepha le-7 CN 109516908 Isisombululo samanzi se-7, esisetyenziswe ngokuthe ngqo kwimveliso ye-folic acid, yenza isivuno esipheleleyo se-folic acid sande nge-5% ngobunzima, ubunyulu bu-99.2% ngesisindo esingaphezulu; Ngaphezu koko, ngenxa yokuba indlela yokucoca ayifaki i-solvent ye-organic, akukho mngcipheko wekhwalithi kumgangatho we-folic acid. Ngaphezu koko, indlela yokucoca isebenzisa amanzi njenge-crystallization solvent, kunye nesisombululo se-aqueous ecocekileyo ye-1,1, i-3-trichloroacetone isetyenziswe ngokuthe ngqo kwimveliso ye-folic acid, ukunciphisa ukusabela kwecala.
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