CONG NGHE MOI - SAN PHAM MOI THI^T Bj PHAN ONG DONG CHAY - NHONG LfU DlilVI VA MOT S6 CfNG DUNG TRONG SAN XUAT HOA CHAT TINH KHI^T, Di/oc PHAM S udt nhieu thd ky qua, cdc thidt bj phan Ong me dd dtigc sd dyng rdng rdi nhieu ITnh vgc san xudt hda chat cdng nghidp Tuy nhien, nhieu qua trinh san xuat hda chat hoat ddng rat tdt thiet bj phan Ong me thi mdt sd Ioal phan Ong nhat djnh lai boat ddng kem hieu qua hon nhung thidt bj dd Trong nhOng trodng hpp ndy, cac nha san xudt hda chat tinh khiet dd chuyen sang sO dyng cdng nhieu hOn cac thiet bj phan Ong ddng chay lien tuc Thidt bj phan Ong ddng ehay lien tyc ed kfch thode nhd hon 10.000 lan so vdi thiet bj phan dng me eung san lopng Ndu phan Ong vd CP ehd hda hpc deu thfch hpp eho ea hai dang thiet bj phan Ong, thidt bj phJin Ong me dung lopng 10.000 lit cd the dope thay the bang thiet bj phan Ong ddng chay vdi dung lopng Ift Cung vdl khd ndng truyen nhiet va truyen vdt chat cao, ty Id cao glCfa dien tfch bd mdt vd the tfch la ddc didm quan trpng cda nhdng thiet bj phan Ong ddng ehay Mdt dde diem khde cda cdc thiet bj phan ufng ddng chay ld thdi gian lou ngan va khdng ddi, ddy Id dieu rd't ed Ipi dieu che nhdhg san phdm de phdn huy phai chju tac ddng Idu ddi nhung dieu kidn can thidt di thge hien phan Ong mong mudn Hon nda, ban chat Hen tyc cda qud trinh ddng chay eung Id mot Ou didm quan trpng, vi nhd dd ma can tdng san lOpng cda me phan Ong ehdng ta chl can van hdnh thidt bj phan Ong thdi gian ddi hdn Dac diem ndy cung gidp giam chi phf ve ddi han, vi viec ndng edp bang each ehd tao nhung thidt bj phan Ong mh edng Idn se khdng cdn can thldt Thidt bi phan Cfng ddng chay lien tuc da the hidn nhieu ou diem dtigc dp dung cdc tinh hudng thfch hpp Vf du, nhdhg Ou didm ndy bao gdm kha ndng tal lap tdt hon qua trinh ph^n Ong, giam ehi phf phdt tridn, tdng dp an todn, vd tao kha ndng tiep can cac CIVHC - SO / phdn ttjf hda chat md bang cdch khae khdng the dope tidp can tren quy md ldn Kha ndng tai lap tot h d n cac dieu kien phan Ong Mdt nhOng ou diem then ehdt eda thidt bj phan Ong ddng chay Hen tuc Id cac didu kien phan Ong ti!/ng Idn van hdnh ed thd dope tdi lap tdt hon so vdi van hanh tCmg me d eac thiet bj phan Ong me tnjyen thdng Vdi thiet bj phan Ong ddng chay, chung ta ed the de dang dat dope mOc nhiet dp da xde djnh vd dong nhat Dieu ndy dde biet quan trpng ddi vdl eac phan Ong ed mifc tda nhiet Idn cac thldt bj phan Ong ddng chay, nhd kfeh thodc nhd ndn nhiet phan {fng dd phan tdn hdn so vdi d thiet bj phan Ong md kieh thode Idn Mot van de ehung can xCf ly van hdnh eac phan tifng tda nhiet cao la s g phdn bd nhiet dp khdng ddng deu Idm sinh edi gpi la nhOng "didm ndng" Tinh trang dd thodng dan den ede hau qua nhO g l i m san lopng, tdng lopng tap ehdt qua trinh CONG NGHE MOI - SAN PHAm mori k RETINOL K Neutrogena ndng cap hodc hieu suat dao dpng nhieu qua tOng me Chung ta hay lay vf du la qua trinh san xud't tetraxyanoetylen oxlt tO tetraxyanoetylen Khi sO' dung hydro peroxit ldm chat oxy hda, nhiet tda khd ed the dtigc kiem sodt d quy md 25g, ndi den nhuhg me Idn hon O quy md 25 g, hieu suat dat dtigc thodng la 65% Khi quy md phan Ong tdng len den 200 g, hieu suat ndy giam xud'ng cdn 0-23% Thdi gian phan Ong toi Ou la 10 phut va ngoai nhOng rdi ro cOa van de tda nhiet thi san pham edn bl phdn hdy tiep xuc vdl node, tao hydro xyanua San phdm ndy la Ong vien rd rdng cho viec ehuydn ddi sang qua trinh ddng chay Viec ehuyen doi da td don gian mdt each bat ngd Chung ta se khdng can dung mdi hode ed dde va khdng can thge hien tdi ou hda Hd thd'ng ddng ehay tao qua trinh lien tuc vdl hal giai doan, vide Idm ngudi trgc tidp bdng node giup gio eho thdi gian phan Ong khdng ddi Trong qua trinh ddng ehay, thdi gian phan Ong td'i ou Id phut, theo quy md, vdl ndng sudt dat 100 g/gld Neu khdng tien hanh tdi ou hda, hieu suat thu hoi dat 47% san pham thu dope d dang khdng mdu, cae ket qua toong to nho tidn hdnh mdt sd cdng doan phan dng GiSm chi p h i nang cap Mot han ehd khae cda qud trinh phan Ong me Id thdi gian edn dd ndng cap phan Cfng to quy md phdng thf nghiem ldn thiet bj phan dng Idn se Idu hdn Tuy eung cd mdt sd didu kidn thf nghidm thfch hpp c i ndng cap len quy md ldn, nhong dd chl la nhung trodng hop hiem hoi Thodng chOng ta se phai thay ddi nhiet dp, dp sudt, thdi gian phan Cfng, qud trinh ed va thdm chf phai thay ddi cd cdc tac nhdn phan Cfng Qua trinh san xudt mdt me 500g retlnol tinh khidt cao Id vf du dien hinh eho vdn dd nay, vi retlnol tinh khidt khdng phai Id phdn td' de thao tae,- nd khdng 6n dinh d nhiSt dp phan Ong vd nhay cam vdl ca khdng khf lan anh sang che dp phan Cfng me, khd ndng tdi lap dieu kien cda qua trinh khd kem, hidu sudt thu hoi thdp (thodng ehi dat 40%) vd can 16 gid de hodn thdnh NhOng ed le khd khdn Idn nhat san xudt retlnol tinh khiet cao la khdng thd Idm sach san pham thd Ddy Id vdn de thge s g Idn ddi vdi vide phat tridn tiep qua trinh phan Ong mk day, qua trinh ddng chay lien tyc dd dope dp dung thdnh cdng, Yeu to then ehdt eho cdng ndy id vide trdnh dope ket tOa lam tac dng phan Cmg De dat dope vide dd, he thdng dung mdl dd dope thay ddi tO metanol va node nho dd dope sCf dung ehd dp phan Ong me Hal ddng tac nhdn rieng re dooc nap vdo thiet bj phan dng ddng chay, mdt ddng vdi I M retinyl axetat THF vd ddng thO hai vdi KOH 2M dung dich node, ea hai d nhidt dp phan Cfng 60''C Node lam ngudi trgc tidp di tO mdt thidt bj phan Cfng ddng chay vd dl vdo thidt bj phan Ong ddng chay ke tldp, dam bao thdi gian phan Cfng vd edc dieu kien khde khdng thay ddi toan bd qud trinh Qua trinh nay da dtigc tdi ou hda ea ve mdt thOa KOH lan tde dp ddng ehay Nd ed thd san xudt retlnol vdi dd tinh khidt 99,9% vd san lopng 35g/gid Dd tinh khidt cao ndy gdy nhdng vdn di ridng cda nd so ket tinh to phat qua trinh boat ddng lidn tuc CIVHC - SO 3/2014 CONG NGHE MOI - SAN PHAIVI MOfl Do tinh Ithiet cao Nhung vdn de ve dd tinh khidt cd thd dope giai quyet bang edeh sO dyng qud trinh ddng ehay lien tyc Vf dy, ngdy nhu cau ddi vdi cac chdt long ion dang ngdy edng Idn, vdi nhOng Ong dyng tO dung mdl eho den cac chat dien ly Tuy nhien, viec san xuat chOng d dang tinh khiet du cao van la thach thOe ldn thge td san xudt, dde biet Id d quy md ldn, vi cd nhieu khd khdn vlee loai bd tap chatvd dung mdi Trong qua trinh phdt trien nhieu dang chdt long ion ed dp tinh khidt cao d quy md kg mot vdn de thgc td Id hien topng nga mau vdng xudt hidn chd't Idng md khdng the dope loai bd ndu nhiet dp phan Cfng tdng len tren 20''C Trdnh dope hien tOpng ehe dp phan Cfng me Id thach thOc ldn, vi phdn Ong alkyl hda tda nhiet manh vd vide dat dp tinh khidt tren 96% Id rdt khd khdn Thaeh thOc da dooc vopt qua bang each chuyen sang chd dp phan Ong ddng chay lidn tyc Nhd dd ed thd dat san lopng 1,5 kg/ gid, vdi dp tinh khidt tren 98% Trong dd, viee sCf dung binh thdy tinh Id ydu td quan trpng di tranh gi vd viec loai bd nhiet bang binh phan Ong thdy tinh vdi kenh rdng mm Id du di ngdn hinh thdnh tap chat cd mdu Cde phan dng tda nhiet nhanh nho phan dng da cd the dtigc kiem soat ddng ehay nhd kha ndng loai bd nhiet d o sau nd dope tao ra, giam xu hodng tao san phdm phu Nang cao d o an toan Cd te mdt nhung uo diem Idn nhat eda vlee sti dung thidt bi phan Ong ddng chay lidn tyc so vdi thiet bi phan Ong me Id nd cd the cai thien dp an todn Idm viec vdi cac chd't nguy hiem Trong eac thiet bj phan Ong me, nhung lopng Idn eac tac nhdn nguy hiem cd the tao nhung rdi ro Idn ca ddi vdi ngOdi van hdnh cung nho mdi trodng xung quanh Nhong d thiet bj ddng ehay, lopng cac chdt nguy hiem cd mdt thidt bj phan Cfng vdo bdt cti luc ndo eung nhd hon nhieu va tao ft CNHC - SO / rOi ro hon DAST (N,N - Diethylaminosulfurtrifluoride) Id tac nhdn flo hda thdng thodng, dope sO dung san xudt nhieu chat trung gian dope pham quan trpng ed chOa ede nguyen td flo Tuy nhien, DAST khd thao tde che dp phan dng me vi nhiet phdn hOy cOa nd thap Tuy phai tinh chd bang cdch chOng ed't, cae tap chat tao thdnh qua trinh chOhg eat se Idm giam tiep dp ben nhiet cda nd Ddy la mdt rdi ro tdng them vi nd phan Cfng de ddng vdi node, tao axit hydrofloric ddc Cau tra ldi ndm d viee san xuat DAST thidt bi phan Ong ddng ehay, sau dd doa nd vao thidt bj phan Ong ddng ehay Hen tuc thO hal, d dd chOng ta thgc hidn qua trinh flo hda Khi dd, vlee thiet kd edn than la cdn thiet vi sulfur tetrafluoride dope sijf dung de san xudt DAST sdi d - 40=0 NgOdl ta da phat trien mdt phOPng phap sO' dyng nd nho khf ddng ehay De lam vlee dd, phan Cfng san xuat DAST dagc thgc hien ma khdng sd dung dung mdl Khi sCf dung thiet bj phan Ong ddng chay lien tue di san xuat DAST, chdng ta ed the dat nang sudt 10 kg/ ngdy Dd dn dinh cda san phdm thd khdng thay ddi, nhong the tfch nhd va tidt dien nhd da Idm tang dang ke dd an toan Phoong phdp ndy cd the dope ap dung de thgc hidn cae qua trinh flo hda lien tyc tren quy md Idn vdi ehi phf thap hon, sCf cdc thiet bj phan Cmg ddng ehay ridng rS, tO dd cd thd phdt tridn quy trinh an todn vd hidu qua de san xuat hpp chat ndy hpp ehdt ma thodng khdng thd dope tiep can theo each khae dung DAST thd Md rong pham vi ap dung cac quy trinh phan Ong Trong mdt sd trodng hpp ede thidt bi phan Cfng ddng chay tao dieu kien dieu che nhOng hpp chdt mdi ma trodc dd khdng thd dope "thge hien bang thiet bj phan Ong me Ngodl ra, neu qua trinh san xuat cd s d dyng eae hda ehd't nguy hiem hode don gian la qua trinh dd khdng thd hoat ddng d quy md ldn hpn, vlee sddyng nhOng lOpng nhd hda chat thidt bj phan Cfng van hanh d dieu kien ddng ehay lien tuc eung td Id cd Ipi hon so vdi d thiet bi phan ufng me Mdt vf du cho trodng hpp ndy Id o-oxylylendiamin hydroclorua Ddy la san pham can dugc san xuat d quy md kg, nhOng ehung ta khong cd quy trinh tdng hpp an toan nao di cd thd san xuat nd d nhung lopng ldn thldt bj phan Cfng me Tuy nhien, hpp chat ndy ed the dope san xudt d quy md micro eac me phan Cfng, bdng edeh chung ta se thidt lap cac thdng sd phan Crng va dd tan, ddng thdi kiem tra dp an todn eda qua trinh Viec dd rat quan trpng, vi mdt cac tac nhdn phan dng dope sCf dung qud trinh la natri azit vOa de chay no vOa ed dde tfnh eao Khi qua trinh ndy dugc chuyen sang thiet bj phan Cfng ddng chay, hai bodc phan Cfng se dope tdeh ridng Qua trinh tao thdnh dlazld vd qua trinh khd dlamin dope thgc hien Quy trinh san xuat nho vay trdnh dope nhu cau tdeh ridng chat trung gian diazid khdng ben Hon hpp phan Ong thd se di vdo thldt bj phan Cfng ddng ehay thCf hai eung vdi tac nhan khCf trlphenylphosphin toluen Phdn Cfng dau tien - qua trinh tao thdnh diazit - cd the dagc thac hidn an todn d 90°C node, thdi gian lou thiet bj phan Ong ddng chay Id 10 p h d i Qua trinh khd dien phut d thldt bj phan Ong ddng chay thO hal Hieu suat thu hdi tdng the dat 60% Nhd dd, chdng ta ed thd san xudt hpp chd't dlamin ndy vdl san lopng Ikg/ngdy San xua't cac san p h a m kem ben Ddi tfnh khdng on dinh cda ban thdn san phdm khie'n cho khdng the thgc hien eae phan Ong me d quy md Idn Nhdng gi ed thd dope tdng hpp phdng thf nghidm hodc thdm chf d quy md pilot thi ddi dOn gian Id khdng the dope thgc hidn d quy md dd Idn dd dap Ong eac nhu cau thOdng mai Thgc hien nhieu me phan dng nhd hon se cho phep ddp Ong nhu cau dd, nhung viec thgdng khdng ed hieu qua ve mat chi phi, thdi gian hodc cdng sudt Cde thldt bj phan Ong ddng chay Hen tuc cd the tao dieu kien san xudt nhung san pham nho vay d nhOng lopng Idn bang each dPn gian Id de cho thiet bj phan ufng van hanh lau hOn Vf du cho trodng hpp Id etyl diazoaxetat, mdt hpp chat cd nhieu Ong dyng nho tac nhan tdng hpp hOu cP vd ddc bidt hdu fch nho tien chat qua trinh propan vdng hda cdc alken Hpp chat rat khdng ben de cd the van chuyen vd sCf dung an toan, vi vay nd phai dope giO cae dung mdl thfch hpp Nhu cau thj tardng dd'i vdl hda chdt ndy kha Idn, nhOng tfnh ben nhiet kem ndn gidi han san xua't an todn chl Id kg/me hodc thidt bj phan Ong dung tich 50 I, hoan todn khdng CIVHC - SO / dd dd dap Ong nhu eau thoong mai Bdng cdch don gian Id c h u y i n sang thidt bj phan Cfng ddng chay lidn tyc, ngodi ta ed the tidn hdnh vlee ndng edp can thiet dd dap Ong nhu cau thj trodng ddi vdi etyl diazoaxetat Khi dp dung quy trinh hda hpc toong tg nho qua trinh me, qua trinh ddng chay trong thidt bj phan Cfng ddng chay dung tfch 50 ml cho phep san xudt etyl diazoaxetat d dang dung djeh 15% trpng lopng toluen, thfch hpp eho ca van ehuyen vd sd* dyng an toan Hidn tai, cdc thidt bi phan Cfng ddng ehay da dat cdng sudt 10 kg etyl diazoaxetat tinh khidt/ ngay, qua trinh san xudt ed thd dope nang edp Idn quy md ldn hon di dap Ong nhu cau Giam t h d i gian va chi p h i san xua't Thldt bj phan Cfng ddng chay lien tuc cung ed thd cho phep san xuat nhanh hon vd dat hidu qua cao hon ve mdt chi phf nhldu trodng hpp, vf dy san xudt thude nhudm quang erdm - ddy la loai thude nhudm dope sd dyng cho nhOng dang mdi eda kfnh ddi mdu, loai kfnh ndy ed thd ddi mau nhanh hon nhieu so vdi eac loai kfnh sCf dyng cac Idp phd vdi cac loai thud'c nhudm thdng thodng hien ddy, vd'n di vdi qud trinh me Id nhiet dp can thidt rd't eao (245°C) vd san pham san xudt d quy md ndng cap ed xu hOdng bi phdn hdy Tuy mdt nhd san xuat An Dp da cdng vide san xudt nhufng lopng Idn vat lidu ndy, nhOng dd Id vdi gidi han mdt me khoang lOOg san p h l m vd can phai thgc hidn khoang 500 me de san xuat dd lopng vdt lieu dope yeu cau Day ro rang khdng phai Id quy trinh ly todng, vi khach hdng yeu eau cung cd'p 75 kg san pham trung gian cho bodc thO to qua trinh tdng hpp bOdc eda minh Vdi mue dfch chuyen sang qua trinh ddng ehdy lien tyc, mdt dung mdi vdi dp sdi eao thfch hpp da dagc xde ^ n h tO nhdm cac glycol ete vd qua trinh da dope thgc hien thldt bi phan Cfng dang dng vdi vat lidu thep khdng gl Thdi gian lou td'i ou la phdt vdi nhiet dd phan ufng 270°C Khi thge hien phan Cfng ddng ehay thdi gian lien tyc 24 gid/ ngdy va ngdy/ tudn, thdi gian hai tuan rodi ngodi ta da san xud't dii vat lieu cho nhu cau nam san xudt eua khach hdng neu tren Chi phf san xuat giam 12% so vdi phan Cmg me, thdi gian phan dng ngan vd dope xae djnh CIVHC - SO / rd rang, nhd dd tao dieu kien xdy dung quy trinh san xuat vdi hieu qua chi phf cao Ngay nay, ed nhieu ITnh vgc ma dd cac thiet bi phan Cfng ddng ehay dd ehOng td nhdng tiu diem cda mlnh Nhong can phai nhdn manh rang eung cd nhOng qua trinh md hien tai khdng thd dagc thge hien cac thidt bj phan Ong ddng chay hodc ndu thge hien nhO vay se khdng ed Ipi so vdi cac thidt bj phan Ong me Mdt nhthig vf du Id eae phan Cfng khdng dong nhdt, dd ede dng nhd eda cae thldt bj phan Ong ddng chay vdl kfch thodc to 10 (im ddn vdi mm se ed nhldu kha ndng bj tde Nhin chung, hien cd the col cae thldt bj phan Ong ddng chay la thidt bj san xuat bd sung cho fTnh vge san xud't hda chd't tinh khidt vd hda dope, ehung tao dieu kien san xuat an toan va dat hieu qua eao ve mdt chi phi dd'i vdi nhieu dang phan Ong Khdng nghi ngd gl rang, cang cd nhidu ede edng ty hda ehdt sCf dung cac thiet bj phan Cfng ddng chay va phat tridn eac quy trinh ddng chay lien tyc, ehdng ta se chiftig kidn nhieu san phdm bat ngd vd thd vj ma thdng thodng rat khd san xuat hode san xudt quy md Idn cde qua trinh phan Ong me • TN Theo Chemistry & Industry 11/2013 ... retlnol vdi dd tinh khidt 99,9% vd san lopng 35g/gid Dd tinh khidt cao ndy gdy nhdng vdn di ridng cda nd so ket tinh to phat qua trinh boat ddng lidn tuc CIVHC - SO 3/2014 CONG NGHE MOI - SAN PHAIVI... Cfng Qua trinh san xudt mdt me 500g retlnol tinh khidt cao Id vf du dien hinh eho vdn dd nay, vi retlnol tinh khidt khdng phai Id phdn td'' de thao tae ,- nd khdng 6n dinh d nhiSt dp phan Ong vd... dp tinh khidt tren 96% Id rdt khd khdn Thaeh thOc da dooc vopt qua bang each chuyen sang chd dp phan Ong ddng chay lidn tyc Nhd dd ed thd dat san lopng 1,5 kg/ gid, vdi dp tinh khidt tren 98% Trong