Ka lehlakoreng le leng, ho qaptjoa ho fana ka mokhoa oa tlhoekiso oa 1,1, 3-trichloroacetone, moo mokhoa ona o nang le mehato e latelang.

Flash:

(1) 1,1, 3-trichloroacetone e tala e tsoakiloeng le metsi;

(2) Recrystallization ea tharollo e ka holimo ka mor'a ho ema;Moho le

(3) likristale tse tiileng tse entsoeng bocha lia tlhotloa ebe li hlatsuoa ka metsi;

Moo, ho Mohato (1), tekanyo ea boima ba 1,1, 3-trichloroacetone e boletsoeng ho bongata ba metsi ke 1.0.1-2).

Ka ho khetheha, mohatong oa (1), tekanyo ea boima ba sehlahisoa se tala sa 1,1, 3-trichloroacetone ho bongata ba metsi e ka ba 1:

(0.4-0.6), e ntlafalitsoeng hape e le 1: 0.5;Ho qaptjoa, litekanyetso tsa 1,1, 3-trichloroacetone lihlahisoa tse tala le metsi li laoloa ka holimo.

Mefuta e mengata ea bohloeki bo phahameng 1,1, 3-trichloroacetone e ka fumanoa.

Ho latela boqapi ba hajoale, mohatong oa (1), sehlahisoa le metsi a 1,1, 3-trichloroacetone tse tala li ka lokisoa ka mocheso oa 10-50 ℃.

Kopanya metsotso ea 10-30 tlas'a maemo, ebe o tlohela metsotso e 10-30;Ka ho khetheha, ho Mohato (1), ho boletse 1,1, 3-trichloropropyl

Ketone e tala e kopantsoe le metsi ka mocheso oa 30-35 ℃ ka metsotso e 25-30, ebe e ema metsotso e 10-15;Tse qapiloeng hona joale

, sebelisa 1,1, 3-trichloroacetone crude e le lisebelisoa tse tala, ka ketleleng ea karabelo, e kopantsoeng le metsi, e tsosoa ka mocheso o itseng ka mor'a ho ema.

Delamination.Ka mor'a delamination, karolo e ka tlaase ea oli e tlosoa, haholo-holo ka ho tlosa litšila tse phahameng tsa chlorine le ho siea tharollo e ka holimo bakeng sa tšebeliso ea hamorao.

Ho latela boqapi, mohatong oa (1), 1,1, 3-trichloroacetone e tala e tsoakoa le metsi hape e ka ts'oaroa.

Maemo, ao ho ona ho se nang moeli o itseng ho maemo le lisebelisoa tse susumetsang, ha feela 1,1, 3-trichloroacetone e ka ba mahoashe.

Sehlahisoa se ka kopanngoa ka ho lekana le metsi.Ka ho khetheha, tekanyo ea ho kopanya ke 100-300r / min.

Tlhahisoleseding ea hona joale, metsi a molemo ka ho fetisisa ke metsi a deionized.

Ho ea ka boqapi, mohatong oa (2), maemo a recrystallization e ka ba: mocheso ho tloha ho 0 ho isa ho 35 ℃, nako ho tloha 0.5 -

Lihora tsa 10, ka ho khetheha, recrystallization e etsoa ka tekanyo e susumetsang ea 50-300 RPM;Ka ho khetheha, reknot

Metsi a boetse a kenngoa ts'ebetsong ea crystallization, moo metsi a kenngoa ka tekanyo ea 200-600 ml / min;Tlas'a maemo ana, recrystallization bokgoni

Litholoana li ntle.

[0034] Ho feta moo, maemo a recrystallization ke: mocheso oa 10-15 ℃, nako ea lihora tsa 2-3, le maemo a recrystallization.

Kristale e tsosoa ka tekanyo ea 100-200 RPM 'me metsi a kenngoa ka tekanyo ea 300-500 ml / min.

Tlas'a maemo ana, phello ea recrystallization e molemo.

Moqaping oa hajoale, mocheso oa recrystallization o hlalositsoeng mohatong oa (2) o tlase ho feta oa 1,1, 3-trichloroacetone mohatong oa (1)

Mocheso oo sehlahisoa se kopantsoeng le metsi ka oona.

Ho ea ka boqapi, mohatong oa (3), motsoako oa karabelo kamora Mohato (2) o ka tlhotloa ka khatello e koetsoeng, kapa

Likristale tse tiileng li fumanoa ka ho tobetsa ka ho toba ka poleiti ea sieve e ka tlaase ho setsi sa motlakase.Tlhahisong ea hona joale, moea le/kapa nitrogen li sebelisoa ka mokhoa o ikhethileng

Ho hloekisa khatello, ho molemo ho sebelisa naetrojene bakeng sa ho hloekisa khatello, 'me khatello e ka ba 0.1-0.2MPa, ka ho khetheha 0.12 -

0. 18 mpa.

Ho ea ka moqapi, kristale e nang le metsi ka mor'a khatello ea khatello e hlatsuoa ka metsi, moo metsi a boletsoeng a hlatsuoang.

Ha ho na moeli o itseng, mohlala, o ka khetha 1-2kg ea ho hlatsoa metsi tlas'a boemo ba mocheso oa 2-25 ℃, 'me u fafatse.

Ha ho na moeli o tobileng oa lebelo.

Ho latela boqapi, bohloeki ba sehlahisoa sa 1,1, 3-trichloroacetone e ka ba 50-65% ka boima ba 'mele.

Maqephe a 3/6 a litaelo

5

CN 109516908 A

5

Ka lehlakoreng le leng, tlhahiso ea hona joale e fana ka folic acid e lokiselitsoeng ke mekhoa efe kapa efe e hlalositsoeng ka holimo

Tharollo ea metsi ea 1,1, 3-trichloroacetone e sebelisoa ka ho toba ho lokisa folic acid.

Ts'ebetso ea mokhoa oa ho itlhoekisa oa ho qaptjoa, joalo ka stratified extraction, crystallization filtration joalo-joalo, e ka etsoa ka mokhoa o koetsoeng.

Tikoloho-ba botsoalle, 'me haholo fokotsa tlhahiso ea metsi a litšila, ha ho litšila manyolo solvents le manyolo litšila khase;Ho phaella moo, mokhoa oa ho hloekisa

Ha ho li-solvents tse hlahisoang, 'me litšila tse phahameng tsa chlorine li tlosoa nakong ea ho hloekisa, kahoo ha ho na kotsi ea boleng ba boleng ba folic acid.

Mokhoa ona o sebelisa metsi e le motsoako oa crystallization, 'me tharollo ea metsi e hloekisitsoeng ea 1,1, 3-trichloroacetone e sebelisoa ka ho toba bakeng sa tlhahiso ea folic acid.

Kakaretso ea lihlahisoa tsa folic acid e ka eketseha ka 5% ka boima ba 'mele,' me bohloeki bo ka holimo ho 99.2% ka boima ba 'mele, bo ka fumanang boleng bo phahameng.

Ka folic acid.

Ho qaptjoa ho hlalosoa ka ho qaqileng ka ho sebelisa embodiments ka tlase.

[0042] Ka mekhoa le likarolo tse latelang, ntle le haeba ho boletsoe ka tsela e 'ngoe, thepa e sebelisoang e fumaneha ka theko ea khoebo, ntle le haeba ho boletsoe ka tsela e 'ngoe.

Mokhoa o sebelisoang ke mokhoa o tloaelehileng tšimong ena.

Moetso oa chromatography ea khase e ne e le GC-2014, e rekiloeng ho Shimadzu Company.

The 1,1, 3-trichloroacetone e lokisitsoeng ke mokhoa oa tlhoekiso oa seqapi sa hona joale [0047] se hloekisoa ka sekontiri sa 50-litre se nang le poleiti ea sieve ka tlase [0048] Pele, bohloeki ba 1,1 ke 65 % ka boima ba 'mele , 3-trichloroacetone 20Kg le metsi 10Kg ka kettle ea karabelo e tsoakiloeng ka 24 e susumetsang metsotso e 12, moo sekhahla se susumetsang ke 200r / min, ka mokhoa o susumetsang ho eketsa metsi, metsi ka tekanyo ea 300 ml / min. , 'me joale motsoako o eme metsotso e 10, o arohane le lera le tlaase la oli, tlosa litšila tse phahameng tsa chlorine;Ntlha ea bobeli, mocheso oa tharollo e ka holimo e nang le lera o ile oa theoleloa ho 5 'me o hlohlelletsa lihora tsa 2 ka tekanyo e susumetsang ea 100r / min.Joale, kristale e tiileng e ile ea fumanoa ka ho toba ka poleiti ea sieve e ka tlase ea kettle ea karabelo ka ho hloekisa khatello ea naetrojene ka khatello ea 0,1 MPa, ebe e fafatsoa le ho hlatsoa ka metsi a batang a 2 kg.Boima bo metsi ba 1,1, 3-trichloroacetone e ne e le 9.8 kg, 'me chromatographic pure (GC) e ne e le 96.8 wt% [0051] Ts'ebetso e amehang mokhoeng ona oa tlhoekiso, joalo ka static stratification, ho tlosoa ha litšila tse phahameng tsa chlorine, crystallization, ho hlatsoa le ho hlatsoa metsi, ho ka etsoa tsamaisong ea 'mele e koetsoeng, e leng botsoalle ba tikoloho,' me e fokotsa haholo ho hlahisa metsi a litšila 'me ha e hlahise litšila tsa mokelikeli oa tlhaho le khase ea litšila [0052].Ntle le moo, hobane mokhoa oa tlhoekiso ntle le ho hlahisa solvent ea organic, le chlorine e phahameng ho tlosa litšila ts'ebetsong ea tlhoekiso, ha ho na kotsi ea boleng ho boleng ba folic acid, empa hape le ka mohlala oa ts'ebetsong oa ho lokisoa ha 1, 1, 3 - folic acid sefapano se amahanngoa le metsi acetone qhibiliha ka ho toba sebelisoa ka tlhahiso, etsa hore folic acid ho ntlafatsa ka kakaretso chai 5 boima %, bohloeki ba 99 5 boima % Mohlala 2 [0054] mothofatso ena e bolela hore 1,1, 3-trichloroacetone lokiselitsoeng ke mokhoa oa tlhoekiso oa boqapi ba hona joale [0055] o hloekisoa ka 50-litre reactor e nang le poleiti ea sefene ka tlase [0056] Pele,1,1 ka bohloeki ba 50% , 3-trichloroacetone 20Kg le metsi 4Kg e tsoakiloeng. ka sekontiri, se susumetsang metsotso e 15 ho 45, lebelo le susumetsang la 300r / min, ts'ebetsong e tsosang takatso ea ho eketsa metsi, metsi ka tekanyo ea 300 ml / min, ebe motsoako o ema metsotso e 15, o arohane le lera le tlase la oli, tlosa litšila tse phahameng tsa chlorinees;Ntlha ea bobeli, mocheso oa tharollo ea lera le ka holimo ka mor'a hore stratification e theohe ho 20, 'me lebelo le susumetsang e ne e le 200r / min bakeng sa 0.5 h.Joale, kristale e tiileng e ile ea fumanoa ka ho toba ka poleiti ea sieve e ka tlaase ho mochine ka ho hloekisa khatello ea naetrojene ka khatello ea 0. 2MPa.Joale, kristale e tiileng e ile ea fafatsoa 'me ea hlatsuoa ka 1Kg ea metsi a batang a 25,' me boima bo metsi ba 1,1, 3-trichloroacetone e ne e le 8.2kg ka mokhoa oa ho fokotsa Mokhoa oa ho hloekisa o amehang ho tlosoa ha static stratification ea litšila tse phahameng tsa chlorine, crystallization, filtration le ts'ebetso ea ho hlatsoa metsi e ka etsoa ka tsamaiso ea 'mele e koetsoeng, tikoloho ea ho sebetsa e na le botsoalle,' me e fokotsa haholo tlhahiso ea metsi a litšila, ha ho na litšila tse nang le mokelikeli le khase ea litšila [0060] Ho phaella moo, kaha mokhoa o etsa joalo. ha e hlahise li-solvents tsa organic le ho tlosa litšila tse phahameng tsa chlorine nakong ea ts'ebetso ea tlhoekiso, ha ho na kotsi ea boleng ba boleng ba folic acid, mme 1,1, 3-trichloroacetone e lokiselitsoeng ke Mohlala oa 2 e qhibiliha ka metsing 'me e sebelisoa ka kotloloho ho hlahiseng folic acid, e eketsang kakaretso ea lihlahisoa tsa folic acid ka 4.9% ka boima ba 'mele le ho finyella bohloeki ba 99.tlhahiso ea hona joale [0063] e hloekisoa ka 50-litre reactor e kentsoeng ka poleiti ea sefene ka tlase [0064] Pele,1,1 ka bohloeki ba 60% , 3-trichloroacetone 20Kg e kopantsoeng le metsi 40Kg ka kettle ea karabo. , e susumetsang metsotso e 30 ho 15, tekanyo e susumetsang ea 100r / min, ts'ebetsong e tsosang takatso ea ho eketsa metsi, metsi ka tekanyo ea 500 ml / min, ebe motsoako o ema metsotso e 30, o arohane le lera le tlaase la oli. , tlosa litšila tse ngata tsa chlorine;Ntlha ea bobeli, mocheso oa tharollo ea lera le ka holimo ka mor'a hore stratification e theohe ho 10, 'me lebelo le susumetsang e ne e le 100r / min bakeng sa lihora tse 10.Ka mor'a moo, kristale e tiileng e ile ea fumanoa ka ho toba ka poleiti ea sieve e ka tlaase ho mochine ka ho hloekisa khatello ea naetrojene ka khatello ea 0.2MPa, ebe e fafatsoa le ho hlatsoa ka 1Kg ea metsi a batang a 5.Boima bo metsi ba 1,1, 3-trichloroacetone e ne e le 6.9kg, 'me chromatographic pure (GC) e ne e le 98.3% ka boima ba' mele [0067] Ts'ebetso e amehang mokhoeng ona oa tlhoekiso, joalo ka static stratification, ho tlosoa ha litšila tse phahameng tsa chlorine, crystallization. , ho hloekisa le ho hlatsoa metsi, ho ka etsoa tsamaisong ea 'mele e koetsoeng, e nang le sebaka sa ho sebetsa se nang le botsoalle,' me e fokotsa haholo ho hlahisa metsi a litšila 'me ha e hlahise litšila tsa mokelikeli le khase ea litšila [0068].Ho phaella moo, hobane mokhoa oa ho hloekisa ntle le ho hlahisa motsoako oa manyolo, le chlorine e phahameng ho tlosa litšila ts'ebetsong ea ho hloekisa, ha ho na kotsi ea boleng ba boleng ba folic acid, 'me e tla ba mohlala oa 3 ho lokisetsa 1, 1, 3 - cross- e amahanngoa le acetone, metsi a qhibilihang, a sebelisoang ka ho toba tlhahisong ea folic acid, a etsa hore folic acid e ntlafatse lihlahisoa ka kakaretso 5. 3 boima %, bohloeki ba 99. 2 boima % Bakeng sa karolo ea 1 [0070] e hloekisitsoeng 1,1, 3- trichloroacetone ho ea ka mokhoa oa mothofatso oa 1, ntle le hore mohatong oa (1), metsi ha a sebelisoe, Ho e-na le hoo, ho ne ho sebelisoa metsoako ea manyolo.Ka lebaka leo, 1,1, 3-trichloroacetone e lokiselitsoeng e ile ea qhibiliha ka metsing 'me ea sebelisoa ka ho toba ho hlahisa folic acid.Kakaretso ea lihlahisoa tsa folic acid e ile ea eketseha feela ka 2% ka boima ba 'mele' me bohloeki e ne e le 95% ka boima ba 'mele.Ho phaella moo, ka lebaka la ho kenyelletsoa ha li-solvents ka mokhoa ona oa ho hloekisa, ho na le kotsi ea boleng ba boleng ba folic acid [0071] ka tekanyo ea 2 [0072].1,1, 3-trichloroacetone e hloekisoa ho ea ka mokhoa oa Mohlala oa 1. Phapang ke hore Mohato oa (1), palo ea metsi ke 50Kg, e leng se bakang keketseho e kholo ea ho hlahisa metsi a litšila le ho fokotseha ha 1 The lihlahisoa tsa 1,1, 3-trichloroacetone likristale e ile ea qhibiliha ka metsing 'me ka ho toba e sebelisoa ho hlahisa folic acid, e le hore kakaretso ea lihlahisoa tsa folic acid e eketsehile feela ka 5.6% ka boima ba' mele le bohloeki e ne e le 99.6% ka boima ba 'mele [0073] ] khahlano le karolelano ea 3 [0074].1,1 e ile ea hloekisoa ka mokhoa oa Mohlala oa 1, 3-trichloroacetone, phapang ke hore mohato (1), heteroplastid e phahameng ea chlorine ha e tlosoe, phello ea ho lokisetsa 1,1, 3-trichloroacetone e na le e kholo. palo ea metsoako chlorinated, boleng ba folic acid kotsi [0075] Ho ea ka mohlala o ka holimo 1-3 'me ke phello ea tekanyo ea 1-3: mokhoa oa tlhoekiso ho akarelletsa ho tlohela ho ema layered kristale filthara ho tlosa phahameng chlorine litšila hlatsoa tshebetso. joalo ka tsohle empa tsamaisong e se nang moea, tikoloho e sebetsang ea botsoalle, 'me e fokotse haholo ts'ebetso ea metsi a litšila, ha e hlahise khase e litšila, mokelikeli oa lintho tse phelang le lintho tse phelang Ho phaella moo, ka ho kenya ts'ebetsong nyeoe ea 1 ho lokisoa ha 1, 1), 3-trichloroacetone. , eketsa bukeng ea 5/6 leqepheng la 7 CN 109516908 Tharollo ea metsi a 7, e sebelisoang ka ho toba ha ho etsoa tlhahiso ea folic acid, e etsa hore lihlahisoa tsohle tsa folic acid li eketsehile ka 5% ka boima ba 'mele, bohloeki ke 99.2% ka boima bo ka holimo;Ho feta moo, hobane mokhoa oa ho hloekisa ha o hlahise solvent ea tlhaho, ha ho na kotsi ea boleng ba boleng ba folic acid.Ho feta moo, mokhoa oa tlhoekiso o sebelisa metsi e le mokelikeli oa crystallization, 'me tharollo ea metsi e hloekisitsoeng ea 1,1, 3-trichloroacetone e sebelisoa ka ho toba tlhahiso ea folic acid, e fokotsa liketso tsa mahlakoreng.

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