Kune rumwe rutivi, chigadzirwa ichi chinopa nzira yekuchenesa ye1,1, 3-trichloroacetone, apo nzira iyi ine matanho anotevera.

Mwenje:

(1) 1, 1, 3-trichloroacetone isina kuchena yakasanganiswa nemvura;

(2) Kudzokorodza mushonga wepamusoro mushure mekumira; Pamwe chete

(3) makristaro akaoma akagadziriswazve anosefetwa osukwa nemvura;

MuDanho (1), chiyero chehuremu hwe crude 1, 1, 3-trichloroacetone nehuwandu hwemvura i10.1-2).

Zviri nani kuti, muDanho (1), chiyero chehuremu hwechigadzirwa chisina kucheneswa che1,1, 3-trichloroacetone nehuwandu hwemvura chinogona kuva 1:

(0.4-0.6), yakagadziridzwa zvakare se1:0.5; Mukugadzirwa uku, chiyero che1,1, 3-trichloroacetone crude product nemvura chinodzorwa mune zvataurwa pamusoro apa.

Mhando yekuchena kwakanyanya kwe1,1, 3-trichloroacetone inogona kuwanikwa.

Zvichienderana nepfungwa iyi, muchikamu (1), chigadzirwa chisina kuchena che1,1, 3-trichloroacetone nemvura zvinogona kugadzirwa patembiricha ye10-50℃.

Sanganisa kwemaminitsi gumi kusvika makumi matatu zvichienderana nemamiriro ezvinhu, wobva warega zvimire kwemaminitsi gumi kusvika makumi matatu; Zviri nani, muDanho (1), 1, 3-trichloropropyl yakati

Ketone isina kucheneswa yakasanganiswa nemvura patembiricha ye30-35℃ kwemaminitsi 25-30, yozomira kwemaminitsi 10-15; Mukugadzirwa kwazvino

, uchishandisa 1, 1, 3-trichloroacetone crude sezvinhu zvisina kubikwa, muketero ye reaction, yakasanganiswa nemvura, yakakungwa patembiricha yakati mushure mekumira

Delamination. Mushure mekubvisa chlorine, mafuta ari pasi anobviswa, kunyanya nekubvisa tsvina yakawanda yechlorine uye kusiya mhinduro yepamusoro kuti izoshandiswa gare gare.

Zvichienderana nepfungwa iyi, muchikamu (1), 1, 3-trichloroacetone isina kucheneswa inosanganiswa nemvura uye inogonawo kusanganiswa.

Mamiriro ezvinhu, umo pasina muganho chaiwo pamamiriro ekukurunga nemidziyo, chero bedzi 1,1, 3-trichloroacetone ichigona kuomarara

Chigadzirwa ichi chinogona kusanganiswa nemvura zvakaenzana. Zviri nani kuti chiyero chekusanganisa chive 100-300r/min.

Muchigadzirwa ichi, mvura inonyanya kushandiswa semvura isina ion.

Zvichienderana nepfungwa iyi, muchikamu (2), mamiriro ekushandiswazve kwecrystallization anogona kuva: tembiricha kubva pa0 kusvika 35℃, nguva kubva pa0.5 -

Maawa gumi, zviri nani, kudzokororwa kwecrystallization kunoitwa ne stirling rate ye 50-300 RPM; Zviri nani, reknot

Mvura inowedzerwawo panguva yekuumbwa kwekristaro, apo mvura inowedzerwa nechiyero che200-600 ml/min; Pasi pemamiriro ezvinhu aya, kushanda zvakanaka kwekugadzirwa kwekristaro

Muchero wakanaka.

[0034] Uyezve, mamiriro ekugadzirisazve: tembiricha ye10-15℃, nguva yemaawa maviri kusvika matatu, uye mamiriro ekugadzirisazve ...

Kiristaro inokurunganiswa nechiyero che100-200 RPM uye mvura inowedzerwa nechiyero che300-500 ml/min.

Mumamiriro ezvinhu aya, mhedzisiro ye recrystallization iri nani.

Muchigadzirwa ichi, tembiricha ye recrystallization inotsanangurwa muchikamu (2) yakaderera pane ye1,1, 3-trichloroacetone muchikamu (1)

Tembiricha iyo chigadzirwa chinosanganiswa nemvura.

Zvichienderana nepfungwa iyi, muDanho (3), musanganiswa wemhinduro mushure meDanho (2) unogona kuseferwa nekumanikidzwa kwakavharwa, kana kuti unogona

Makristasi akaoma anowanikwa nekudzvanya zvakananga nepasefa iri pasi pe reactor. Mukugadzirwa kwazvino, mhepo uye/kana nitrogen zviri nani kushandisa

Kusefa kwedzvinyiriro, zviri nani kushandisa nitrogen pakusefa kwedzvinyiriro, uye kumanikidzwa kunogona kuva 0.1-0.2MPa, zviri nani kuva 0.12 -

0. 18 mpa.

Zvinoenderana nepfungwa iyi, kristalo inobuda mushure mekusefa kwesimba inogezwa nemvura, umo mvura iyoyo inogezwa.

Hapana muganho chaiwo, semuenzaniso, unogona kusarudza 1-2kg yekugeza nemvura kana tembiricha iri pakati pe2-25℃, wobva wapfapfaidza.

Hapana muganho chaiwo wekumhanya.

Zvichienderana nepfungwa iyi, kuchena kwechigadzirwa chisina kuchena che1,1, 3-trichloroacetone kunogona kuva 50-65% nehuremu.

Mapeji 3/6 emirairo

5

CN 109516908 A

5

Chigadzirwa ichi, kune rumwe rutivi, chinopawo folic acid iyo inogadzirwa neimwe yenzira dzakatsanangurwa pamusoro apa.

Mhinduro yemvura ye1,1, 3-trichloroacetone inoshandiswa zvakananga kugadzira folic acid.

Kushanda kwenzira yekuchenesa yakagadzirwa, yakadai sekubvisa zvinhu zvakakamurwa, kupfapfaidza makristaro nezvimwewo, kunogona kuitwa muhurongwa hwakavharwa.

Inochengetedza nharaunda, uye inoderedza zvikuru kugadzirwa kwemvura yakasviba, hapana marara eorganic solvents uye organic waste gasi; Pamusoro pezvo, nzira yekuchenesa

Hapana zvinonyungudutsa zve organic zvinounzwa, uye tsvina yakawanda ye chlorine inobviswa panguva yekuchenesa, saka hapana njodzi yemhando yepamusoro kumhando ye folic acid.

Nzira iyi inoshandisa mvura se crystallization solvent, uye mvura yakacheneswa ye 1,1, 3-trichloroacetone inoshandiswa zvakananga kugadzira folic acid.

Mugoho wese we folic acid unogona kuwedzerwa ne5% nehuremu, uye kuchena kuri pamusoro pe99.2% nehuremu, izvo zvinogona kuita kuti ive yemhando yepamusoro.

Ye folic acid.

Kugadzirwa uku kunotsanangurwa zvakadzama kuburikidza nemuenzaniso uri pazasi.

[0042] Munzira dzinotevera uye zviyero, kunze kwekunge zvataurwa neimwe nzira, zvinhu zvinoshandiswa zvinowanikwa kuburikidza nekutenga kwekutengesa, kunze kwekunge zvataurwa neimwe nzira

Nzira inoshandiswa ndiyo nzira yakajairika munyaya iyi.

Modhi yegesi chromatography yaive GC-2014, yakatengwa kubva kuShimadzu Company.

Iyo 1,1, 3-trichloroacetone yakagadzirwa nenzira yekuchenesa yechinhu ichi chitsva [0047] inocheneswa mureactor ye50-litre ine plate yekusefa pasi [0048] Kutanga, kuchena kwe1,1 kuri 65% nehuremu, 3-trichloroacetone 20Kg uye mvura 10Kg mukettle yereaction yakasanganiswa mu24 ichikurunga kwemaminitsi gumi nemaviri, uko kukurunga kuri 200r/min, mukuita kwekukurunga kuwedzera mvura, mvura iri pachiyero che300 ml/min, uye ipapo musanganiswa wakamira kwemaminitsi gumi, wakaparadzaniswa nechikamu chezasi chemafuta, kubvisa tsvina yakawanda yechlorine; Chechipiri, tembiricha yemhinduro yepamusoro yakaderedzwa kusvika 5 ndokukurunga kwemaawa maviri pachiyero chekukurunga che100r/min. Zvadaro, kristaro yakasimba yakawanikwa zvakananga kuburikidza neplate yesipo iri pasi pekettle yereaction nekusefa nitrogen pressure pa pressure ye 0.1 MPa, uye yozopfapfaidzwa nekusukwa nemvura inotonhora ye 2 kg. Huremu hwakanyorova hwe 1,1, 3-trichloroacetone hwaive 9.8 kg, uye chromatographic pure (GC) yaive 96.8 wt % [0051]. Kushanda kwakabatanidzwa munzira iyi yekuchenesa, senge static stratification, kubviswa kwe chlorine yakawandisa, crystallization, filtration uye washing water, kunogona kuitwa mu closed body system, iyo ine hushamwari kune nharaunda, uye inoderedza zvikuru kugadzirwa kwemvura yakasviba uye haiburitse marara organic solvent uye organic waste gas [0052]. Pamusoro pezvo, nekuti nzira yekuchenesa isina kuisa organic solvent, uye chlorine yakawanda yekubvisa tsvina mukuchenesa, hapana njodzi yemhando yepamusoro pamhando yefolic acid, asiwo nemuenzaniso wekugadzira we1, 1, 3 - folic acid yakabatana neacetone mvura yakanyungudutswa zvakananga inoshandiswa mukugadzira, inoita kuti folic acid iwedzere goho rose 5 huremu %, kuchena kwe99 5 huremu % Muenzaniso 2 [0054] Iyi nzira inotaura kuti 1,1, 3-trichloroacetone yakagadzirwa nenzira yekuchenesa yechigadzirwa ichi [0055] inocheneswa mureactor ye50-litre ine firita rekusefa pasi [0056] Chekutanga, 1,1 ine kuchena kwe50%, 3-trichloroacetone 20Kg nemvura 4Kg yakasanganiswa mureactor, ichikurunga kwemaminitsi gumi nemashanu pa45, kukurunga kwe300r/min, mukukurudzira kuwedzera mvura, mvura pachiyero che300 ml/min, uye ipapo Musanganiswa wacho wakamira kwemaminitsi gumi nemashanu, wakaparadzaniswa nechikamu chepasi chemafuta, kubvisa tsvina yakawanda yechlorine; Chechipiri, tembiricha yemushonga wechikamu chepamusoro mushure mekupatsanurwa yakaderedzwa kusvika pa20, uye mwero wekusanganisa waive 200r/min kwemaawa 0.5. Zvadaro, kristalo yakasimba yakawanikwa zvakananga kuburikidza neplate yesieve iri pasi pe reactor nekusefa nitrogen pressure papressure ye0.2MPa. Zvadaro, kristaro yakasimba yakapfapfaidzwa ndokusukwa ne1Kg yemvura inotonhora makumi maviri nemashanu, uye huremu hwakanyorova hwe1,1, 3-trichloroacetone hwaive 8.2kg nenzira yekuderedza. Nzira yekuchenesa inobatanidzwa mukubvisa tsvina yakawanda yechlorine, crystallization, filtration uye washing operations inogona kuitwa muA closed body system, nzvimbo yekushanda ine hushamwari, uye inoderedza zvikuru kugadzirwa kwemvura yakasviba, hapana marara organic solvent uye organic waste gas [0060]. Pamusoro pezvo, sezvo nzira iyi isingaunze organic solvents uye inobvisa tsvina yakawanda yechlorine panguva yekuchenesa, hapana njodzi yemhando ye folic acid, uye 1,1, 3-trichloroacetone yakagadzirwa neMuenzaniso 2 inonyungudutswa mumvura uye inoshandiswa zvakananga mukugadzira folic acid, ichiwedzera goho rese re folic acid ne4.9% nehuremu uye ichiwana kuchena kwe99. Iyi nzira inotaura kuti 1,1, 3-trichloroacetone yakagadzirwa nenzira yekuchenesa yechigadzirwa ichi [0063] inocheneswa mu50-litre. reactor yakaiswa ndiro yekusefa pasi [0064] Chekutanga, 1,1 ine kuchena kwe60%, 3-trichloroacetone 20Kg yakasanganiswa nemvura 40Kg mukettle yereaction, ichikurunga kwemaminitsi makumi matatu pa15, mwero wekukurunga we100r/min, mukuita kwekukurunga kuti uwedzere mvura, mvura pamwero we500 ml/min, uye musanganiswa wacho wakamira kwemaminitsi makumi matatu, wakaparadzaniswa nechikamu chemafuta chezasi, kubvisa tsvina yakawanda yechlorine; Chechipiri, tembiricha yemhinduro yepamusoro mushure mekupatsanurwa yakaderedzwa kusvika pa10, uye mwero wekukurunga waive 100r/min kwemaawa gumi. Zvadaro, kristaro yakasimba yakawanikwa zvakananga kuburikidza neplate yesieve iri pasi pereactor nekusefa nitrogen pressure papressure ye0.2MPa, uye yozopfapfaidzwa nekusukwa ne1Kg yemvura inotonhora 5. Huremu hwakanyorova hwe1,1, 3-trichloroacetone hwaive 6.9kg, uye chromatographic pure (GC) yaive 98.3% nehuremu [0067]. Kushanda kwakabatanidzwa munzira iyi yekuchenesa, senge static stratification, kubvisa tsvina yakawanda yechlorine, crystallization, filtration uye washing water, kunogona kuitwa mu closed body system, ine ushamwari hwekushanda, uye inoderedza zvikuru kugadzirwa kwemvura yakasviba uye haiburitse marara e organic solvent uye organic waste gas [0068]. Pamusoro pezvo, nekuti nzira yekuchenesa isina kuisa organic solvent, uye chlorine yakawanda yekubvisa tsvina mukuchenesa, hapana njodzi yemhando yepamusoro pamhando yefolic acid, uye semuenzaniso ichave 3 kugadzirira kwe1, 1, 3 - yakasanganiswa neacetone, mvura yekunyungudutsa, inoshandiswa zvakananga mukugadzira folic acid, inoita kuti folic acid ivandudze goho rese 5.3 huremu %, kuchena kwe99.2 huremu % Pachikamu 1 [0070] chakacheneswa 1,1, 3-trichloroacetone zvichienderana nenzira yekutevedzera 1, kunze kwekuti muchikamu (1), mvura haishandiswe, Pane kudaro, organic solvents yakashandiswa. Nekuda kweizvozvo, 1,1, 3-trichloroacetone yakagadzirirwa yakanyungudutswa mumvura uye yakashandiswa zvakananga mukugadzira folic acid. Goho rese refolic acid rakangowedzerwa ne2% nehuremu uye kuchena kwaive 95% nehuremu. Pamusoro pezvo, nekuda kwekuiswa kwezvinonyungudutsa zve organic munzira iyi yekuchenesa, pane njodzi yemhando yepamusoro kumhando ye folic acid [0071] muchikamu 2 [0072]. 1,1, 3-trichloroacetone inocheneswa zvichienderana nenzira iri muMuenzaniso 1. Musiyano ndewekuti muDanho (1), huwandu hwemvura i50Kg, zvichikonzera kuwedzera kukuru mukuumbwa kwemvura yakasviba uye kudzikira kwe1. Goho re 1,1, 3-trichloroacetone crystals rakanyungudutswa mumvura uye rakashandiswa zvakananga mukugadzirwa kwe folic acid, zvekuti goho rese re folic acid rakangowedzerwa ne5.6% nehuremu uye kuchena kwaive 99.6% nehuremu [0073] zvichienzaniswa nechiyero che3 [0074]. 1,1 yakacheneswa nenzira yeMuenzaniso 1, 3-trichloroacetone, musiyano ndewekuti mudanho (1), heteroplastid yechlorine yakakwira haibviswi, mhedzisiro yekugadzirwa kwe1,1, 3-trichloroacetone ine huwandu hwakawanda hwemakemikari ane chlorine, mhando yengozi yefolic acid [0075] Sekureva kwemuenzaniso uri pamusoro apa 1-3 uye mhedzisiro yechiyero che1-3: nzira yekuchenesa inosanganisira let stand layered crystal filter kubvisa tsvina yakawanda yechlorine mashandisirwo ekusuka akadai seese kunze kwemuchina wemhepo, nzvimbo yekushanda ine hushamwari, uye yakaderedza zvakanyanya kuwanda kwemvura yakasviba, haiburitse gasi rakasviba, organic solvent uye organic. Pamusoro pezvo, nekushandisa kesi 1 kugadzirira kwe1, 1), 3-trichloroacetone, wedzera mubhuku 5/6 peji 7 CN 109516908 A 7 water solution, inoshandiswa zvakananga mukugadzirwa kwefolic acid, inoita kuti goho rese refolic acid riwedzere ne5% nehuremu, kuchena kuri 99.2% nehuremu. pamusoro apa; Uyezve, nekuti nzira yekuchenesa haiunzi organic solvent, hapana njodzi yemhando yepamusoro kumhando yefolic acid. Uyezve, nzira yekuchenesa inoshandisa mvura se crystallization solvent, uye 1,1, 3-trichloroacetone yakacheneswa inoshandiswa zvakananga mukugadzira folic acid, zvichideredza mhedzisiro yemamwe mativi.

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