Kune rimwe divi, kugadzirwa kunopa nzira yekuchenesa ye1,1, 3-trichloroacetone, umo iyo nzira inosanganisira anotevera matanho.
Flash:
(1) Crude 1,1, 3-trichloroacetone yakasanganiswa nemvura;
(2) Recrystallization yemhinduro yepamusoro mushure mekumira;Naizvozvowo
(3) makristasi akasimba anosefa uye anogezwa nemvura;
Imo, muChikamu (1), huremu hwehuremu hwataurwa 1,1, 3-trichloroacetone kuhuwandu hwemvura i1.
0.1-2).
Zvichida, muChikamu (1), huremu hwechiyero che1,1, 3-trichloroacetone crude product kusvika kuhuwandu hwemvura hunogona kuva 1:
(0.4-0.6), yakagadziridzwa zvakare se1: 0.5;Mukugadzirwa, kuyerwa kwe1,1, 3-trichloroacetone crude chigadzirwa uye mvura inodzorwa mune zviri pamusoro.
Rudzi rwekuchena kwepamusoro 1,1, 3-trichloroacetone inogona kuwanikwa.
Zvinoenderana nekugadzirwa kwazvino, mudanho (1), iyo 1,1, 3-trichloroacetone crude chigadzirwa uye mvura inogona kugadzirwa patembiricha ye10-50 ℃
Sakanidza 10-30 maminitsi pasi pemamiriro ezvinhu, uye worega kumira kwemaminitsi 10-30;Zvichida, muChikamu (1), akati 1,1, 3-trichloropropyl
Iyo ketone isina kuchena yakasanganiswa nemvura pakupisa kwe30-35 ℃ kwemaminitsi 25-30, ndokuzomira kwemaminitsi 10-15;Muchigadzirwa chazvino
, uchishandisa 1,1, 3-trichloroacetone crude seyakabikwa, mu kettle yekupindura, yakasanganiswa nemvura, yakamutswa pane imwe tembiricha mushure mekumira.
Delamination.Mushure me delamination, iyo yakaderera mafuta layer inobviswa, kunyanya nekubvisa yakakwira chlorine tsvina uye kusiya mhinduro yepamusoro kuti ishandiswe gare gare.
Zvinoenderana nekugadzirwa, mudanho (1), iyo isina kuchena 1,1, 3-trichloroacetone inosanganiswa nemvura uye inogona zvakare kumutswa.
Mamiriro ezvinhu, umo pasina kuganhurirwa kwakananga pamamiriro ekusimudzira uye zvishandiso, chero bedzi iyo 1,1, 3-trichloroacetone inogona kuve yakaoma.
Chigadzirwa chacho chinogona kusanganiswa nemvura.Kunyanya, chiyero chekusanganiswa chiri 100-300r / min.
Muchigadzirwa chemazuva ano, mvura inonyanya kushandiswa mvura.
Zvinoenderana neyakagadzirwa, mudanho (2), iyo recrystallization mamiriro anogona kunge ari: tembiricha kubva 0 kusvika 35 ℃, nguva kubva 0.5 -
Maawa gumi, zviri nani, iyo recrystallization inoitwa pamwero unokurudzira we50-300 RPM;Zvakanaka, reknot
Mvura inowedzerwawo mumutambo wekristalllization, umo mvura inowedzerwa pamwero we200-600 ml / min;Pasi pemamiriro ezvinhu aya, recrystallization kunyatsoshanda
Muchero wakanaka.
[0034] Kuwedzera zvakanyanya, mamiriro ekristalllization ndeaya: tembiricha ye10-15 ℃, nguva yemaawa 2-3, uye mamiriro ekudzokorora.
Iyo crystal inokurudzirwa pamwero we 100-200 RPM uye mvura inowedzerwa pamwero we 300-500 ml / min.
Pasi pemamiriro ezvinhu aya, recrystallization effect iri nani.
Muchigadzirwa chazvino, tembiricha yerecrystallization inotsanangurwa mudanho (2) yakaderera pane iyo ye1,1, 3-trichloroacetone mudanho (1)
Kupisa uko chigadzirwa chacho chinosanganiswa nemvura.
Zvinoenderana nekugadzirwa, muNhanho (3), musanganiswa wekuita mushure meNhanho (2) inogona kusefa kunze nekuvharirwa kumanikidzwa, kana inogona
Makristasi akasimba anowanikwa nekudzvanya zvakananga kuburikidza nesefa ndiro pazasi pe reactor.Muchigadzirwa chazvino, mweya uye / kana nitrogen zviri nani kushandiswa
Pressure filtration, zviri nani kushandisa nitrogen yekumanikidza kusefa, uye kumanikidza kunogona kuva 0.1-0.2MPa, zviri nani 0.12 -
0. 18 mpa.
Zvinoenderana neyakagadzirwa, iyo yakadzikira kristaro mushure mekumanikidzwa kusefa inoshambidzwa nemvura, umo mvura yakataurwa inogezwa.
Iko hakuna chaiyo muganho, semuenzaniso, unogona kusarudza 1-2kg yemvura yekupfapfaidza yekugeza pasi pemamiriro ekupisa kwe2-25 ℃, uye pfapfaidza.
Hapana chakananga chinogumira.
Zvinoenderana nekugadzirwa, kuchena kwe1,1, 3-trichloroacetone crude chigadzirwa chinogona kunge chiri 50-65 % nehuremu.
Mapeji 3/6 emirayiridzo
5
CN 109516908 A
5
Ikozvino kugadzirwa, kune rumwe rutivi, inopawo folic acid iyo inogadzirwa neimwe yenzira dzakatsanangurwa pamusoro apa
Mushonga wemvura we1,1, 3-trichloroacetone unoshandiswa zvakananga kugadzira folic acid.
Iko kushanda kweiyo nzira yekuchenesa yekugadzirwa, senge stratified extraction, crystallization filtration uye zvichingodaro, inogona kuitwa mune yakavharwa system.
Zvakatipoteredza-ane hushamwari, uye kuderedza zvakanyanya kugadzirwa kwemvura yakaraswa, pasina tsvina organic solvents uye organic tsvina gasi;Mukuwedzera, nzira yekuchenesa
Hapana organic solvents inounzwa, uye iyo yakakwira chlorine tsvina inobviswa panguva yekucheneswa, saka hapana njodzi yemhando kumhando yefolic acid.
Iyo nzira inoshandisa mvura se crystallization solvent, uye yakanatswa aqueous solution ye1,1, 3-trichloroacetone inoshandiswa zvakananga kugadzira folic acid.
Iyo yakazara goho refolic acid inogona kuwedzerwa ne5% nehuremu, uye kuchena kuri pamusoro pe99.2% nehuremu, iyo inogona kuwana yepamusoro mhando.
Ne folic acid.
Iyo yakagadzirwa inotsanangurwa zvakadzama kuburikidza ne embodiments pazasi.
[0042] Mune anotevera embodiments uye zviyero, kunze kwekunge zvatsanangurwa neimwe nzira, zvinhu zvinoshandiswa zvinowanikwa kuburikidza nekutenga kwekutengesa, kunze kwekunge zvataurwa neimwe nzira.
Mutoo unoshandiswa ndiwo wakajairika mundima iyi.
Iyo gasi chromatography modhi yaive GC-2014, yakatengwa kubva kuShimadzu Company.
Iyo 1,1, 3-trichloroacetone yakagadzirwa nenzira yekuchenesa yekugadzirwa kwazvino [0047] inonatswa mu50-litre reactor yakashongedzerwa sefa sieve ndiro pazasi [0048] Kutanga, kuchena kwe1,1 ndeye 65. % ne uremu , 3-trichloroacetone 20Kg uye mvura 10Kg mune inopindurwa kettle yakavhenganiswa mu 24 ichikurudzira kwemaminitsi gumi nemaviri, apo chiyero chekukurudzira chiri 200r / min, mukukurudzira kuwedzera mvura, mvura pachiyero che 300 ml / min. , uye ipapo musanganiswa wakamira kwemaminitsi gumi, wakaparadzaniswa nemafuta ezasi, kubvisa tsvina yakakwirira yeklorini;Chechipiri, kutonhora kwemushonga wepamusoro wepamusoro kwakaderedzwa kusvika ku5 uye kukurudzirwa kwemaawa maviri pamwero we 100r / min.Zvadaro, kristaro yakasimba yakawanikwa zvakananga kuburikidza neplate ye sieve pazasi kweketero yekuita ne nitrogen pressure filtration pakumanikidzwa kwe 0.1 MPa, ndokuzopfapfaidza uye yakashambidzwa ne 2 kg mvura inotonhora.Huremu hwakanyorova hwe1,1, 3-trichloroacetone hwaive 9.8 kg, uye chromatographic pure (GC) yaive 96.8 wt% [0051] Kuvhiya kunobatanidzwa mune iyi nzira yekuchenesa, senge static stratification, kubviswa kwepamusoro chlorine tsvina, crystallization, kusefa uye kugezwa kwemvura, kunogona kuitwa mune yakavharwa system system, iyo ine ushamwari kwezvakatipoteredza, uye inoderedza zvakanyanya kugadzirwa kwemvura yakaraswa uye haiburitse tsvina organic solvent uye organic tsvina gasi [0052].Uye zvakare, nekuti iyo nzira yekuchenesa pasina kuunza organic solvent, uye yakakwira chlorine kubvisa tsvina mukucheneswa, hapana njodzi yemhando pamhando yefolic acid, asiwo nekuita muenzaniso wekugadzirira kwe1, 1, 3 - folic acid cross-linked with acetone water yakanyungudutswa yakananga kushandiswa mukugadzirwa, inoita folic acid kuvandudza goho rose 5 uremu %, kuchena kwe 99 5 uremu % Muenzaniso 2 [0054] Ichi embodiment inotaura kuti 1,1, 3-trichloroacetone yakagadzirwa ne nzira yekuchenesa yechigadzirwa chazvino [0055] inonatswa mu50-litre reactor yakashongedzerwa sefa sieve ndiro pazasi [0056] Kutanga,1,1 nekuchena kwe50%, 3-trichloroacetone 20Kg uye mvura 4Kg yakasanganiswa. mu reactor, ichikurudzira kwemaminitsi gumi nemashanu pa45, chiyero chekukurudzira che 300r / min, mukukurudzira kuwedzera mvura, mvura pachiyero che 300 ml / min, uye ipapo musanganiswa wakamira kwemaminitsi gumi nemashanu, wakaparadzaniswa kubva kune yakaderera mafuta layer, bvisa yakakwira chlorine impurities;Chechipiri, kutonhora kwepamusoro-soro yekugadzirisa mushure mekugadzirisa kwakaderedzwa kusvika ku20, uye chiyero chekukurudzira chaiva 200r / min ye 0.5 h.Zvadaro, kristaro yakasimba yakawanikwa zvakananga kuburikidza neplate ye sieve iri pasi pe reactor ne nitrogen pressure filtration pakumanikidzwa kwe 0. 2MPa.Zvadaro, kristaro yakasimba yakapfapfaidzwa uye yakashambidzwa ne1Kg ye25 mvura inotonhora, uye huremu hwakanyorova hwe1,1, 3-trichloroacetone yaiva 8.2kg nenzira yekuderedza Nzira yekuchenesa inobatanidzwa mukubvisa static stratification yekusvibiswa kwepamusoro kweklorini, crystallization, filtration uye mvura yekugeza mabasa inogona kuitwa muA yakavharwa system system, nzvimbo yekushanda ine hushamwari, uye inoderedza zvakanyanya kugadzirwa kwemvura yakasviba, hapana tsvina organic solvent uye organic tsvina gasi [0060] Mukuwedzera, sezvo nzira yacho ichiita. kwete kuunza organic solvents uye inobvisa yakakwira chlorine tsvina panguva yekucheneswa, hapana njodzi yemhando yemhando yefolic acid, uye iyo 1,1, 3-trichloroacetone yakagadzirwa neMuenzaniso 2 inonyungudika mumvura uye inoshandiswa zvakananga mukugadzirwa kwe folic acid, ichiwedzera goho rose refolic acid ne4.9% nekurema uye kuwana kuchena kwe99 Embodiment iyi inotaura kuti 1,1, 3-trichloroacetone yakagadzirwa nenzira yekuchenesa t.iye aripo kugadzirwa [0063] inonatswa mu50-litre reactor yakasungirirwa sefa sieve ndiro pazasi [0064] Kutanga,1,1 nekuchena kwe60% , 3-trichloroacetone 20Kg yakasanganiswa nemvura 40Kg mu kettle yekupindura. , ichikurudzira maminitsi makumi matatu pa15, iyo inokonzera 100r / min, mukukurudzira kuwedzera mvura, mvura pachiyero che 500 ml / min, uye ipapo musanganiswa wakamira kwemaminitsi makumi matatu, wakaparadzaniswa nemafuta ezasi. , bvisa tsvina yakakwirira yeklorini;Chechipiri, tembiricha yepamusoro-soro sarudzo mushure mekugadzirisa kwakaderedzwa kusvika ku10, uye chiyero chekukurudzira chaiva 100r / min kwemaawa gumi.Zvadaro, kristaro yakasimba yakawanikwa zvakananga kuburikidza neplate ye sieve pazasi pe reactor ne nitrogen pressure filtration pakumanikidzwa kwe 0.2MPa, ndokuzopfapfaidza nekushambidzwa ne1Kg ye5 mvura inotonhora.Huremu hwakanyorova hwe1,1, 3-trichloroacetone hwaive 6.9kg, uye chromatographic pure (GC) yaive 98.3% nehuremu [0067] Kuvhiya kunobatanidzwa mune iyi nzira yekuchenesa, senge static stratification, kubviswa kwepamusoro chlorine tsvina, crystallization. , kusefa uye kushambidzwa kwemvura, kunogona kuitwa mune yakavharwa system system, iyo ine ushamwari yekushanda nharaunda, uye inoderedza zvakanyanya chizvarwa chemarara emvura uye haiburitse tsvina organic solvent uye organic tsvina gasi [0068].Mukuwedzera, nokuti nzira yekuchenesa pasina kuunza organic solvent, uye high chlorine kubvisa tsvina mukucheneswa, hapana ngozi yehutano pamhando ye folic acid, uye ichava semuenzaniso 3 kugadzirira kwe1, 1, 3 - cross- yakabatana neacetone, mvura yekunyunguduka, inoshandiswa zvakananga mukugadzirwa kwefolic acid, inoita folic acid kuvandudza goho rose 5. 3 uremu %, kuchena kwe99. 2 uremu % Nokuda kwechikamu 1 [0070] yakanatswa 1,1, 3- trichloroacetone maererano nenzira ye embodiment 1, kunze kwekuti munhanho (1), mvura haishandiswi, Pane kudaro, organic solvents yakashandiswa.Somugumisiro, iyo yakagadzirirwa 1,1, 3-trichloroacetone yakanyungudutswa mumvura uye yakashandiswa zvakananga mukugadzirwa kwefolic acid.Goho rose refolic acid rakangowedzerwa ne2% nekurema uye kuchena kwaive 95% nekurema.Mukuwedzera, nekuda kwekuiswa kwezvinonyungudutsa zvehupenyu mune iyi nzira yekuchenesa, kune ngozi yehutano kuhutano hwefolic acid [0071] muchikamu 2 [0072].1,1, 3-trichloroacetone inonatswa maererano nenzira iri muMuenzaniso 1. Musiyano ndewekuti muChikamu (1), huwandu hwemvura ndeye 50Kg, zvichiita kuti kuwedzera kukuru mukugadzirwa kwemvura yakasviba uye kuderera kwe1 The goho re1,1, 3-trichloroacetone makristasi akanyungudutswa mumvura uye akashandiswa zvakananga mukugadzirwa kwefolic acid, kuitira kuti goho rose refolic acid rakangowedzerwa ne5.6% nekurema uye kuchena kwaive 99.6% nekurema [0073 ] zvichienderana nereshiyo ye3 [0074].1,1 yakacheneswa nenzira yeMuenzaniso 1, 3-trichloroacetone, mutsauko ndewekuti padanho (1), iyo yakakwira chlorine heteroplastid haina kubviswa, mhedzisiro yekugadzirira kwe1,1, 3-trichloroacetone ine yakakura. nhamba yemakemikari eklorini, kunaka kwefolic acid ngozi [0075] Maererano nemuenzaniso wepamusoro 1-3 uye ndiwo mugumisiro wechiyero che 1-3: nzira yekuchenesa inosanganisira rega kumira yakavharidzirwa crystal filter kubvisa yakakwirira chlorine tsvina yekugeza mabasa. zvakadai sezvose asi mumhepo inodzivirira mhepo, nzvimbo yekushanda inoshamwaridzana, uye yakaderedza zvakanyanya kuitika kwemvura yakasvibiswa, haibudisi gasi remarara, organic solvent uye organic Uyezve, nekushandisa nyaya 1 kugadzirira kwe1, 1), 3-trichloroacetone. , kuwedzera mubhuku 5/6 peji 7 CN 109516908 A 7 mhinduro yemvura, inoshandiswa zvakananga mukugadzirwa kwefolic acid, inoita kuti chibereko chefolic acid chiwedzere 5 % nekurema, kuchena ndeye 99.2 % nekurema pamusoro;Uyezve, nekuti nzira yekuchenesa haiunze organic solvent, hapana njodzi yemhando yemhando yefolic acid.Uyezve, nzira yekuchenesa inoshandisa mvura secrystallization solvent, uye yakacheneswa aqueous solution ye1,1, 3-trichloroacetone inoshandiswa zvakananga mukugadzirwa kwefolic acid, kuderedza maitiro eparutivi.
Athena CEO
Whatsapp/wechat:+86 13805212761
MIT-Iyo kambani IVY Industry CO., LTD
ADD:Jiangsu Province, China
Nguva yekutumira: Aug-12-2021