Dhinaca kale, hal-abuurku wuxuu bixiyaa habka nadiifinta ee 1,1, 3-trichloroacetone, halkaas oo habku ka kooban yahay tallaabooyinka soo socda.

Fiiri:

(1) Ceyriin 1,1, 3-trichloroacetone oo lagu qaso biyo;

(2) Dib-u-celinta xalka sare ka dib markaad istaagto;Sidoo kale

(3) Kiristaalo adag oo dib loo soo celiyay ayaa la sifeeyaa oo lagu dhaqaa biyo;

Halkaa, Talaabada (1), saamiga miisaanka ee cayriin 1,1, 3-trichloroacetone ee la sheegay ilaa cadadka biyaha waa 10.1-2).

Sida la doorbidayo, Talaabada (1), saamiga miisaanka 1,1, 3-trichloroacetone ee alaabta ceeriin ilaa qadarka biyaha wuxuu noqon karaa 1:

(0.4-0.6), oo loo sii hagaajiyay sida 1:0.5;Hal-abuurka, qiyaasta 1,1, 3-trichloroacetone alaabta ceeriin iyo biyaha ayaa lagu xakameynayaa kuwan sare

Qiyaasta nadiifinta sare ee 1,1, 3-trichloroacetone waa la heli karaa.

Sida ku cad hindisaha hadda, tallaabada (1), 1,1, 3-trichloroacetone alaabta ceeriin iyo biyaha waxaa lagu diyaarin karaa heerkul ah 10-50 ℃

Isku qas 10-30 daqiiqo shuruudaha hoos yimaada, ka dibna u daa 10-30 daqiiqo;Sida fiican, Tallaabada (1), ayaa lagu yidhi 1,1, 3-trichlororopyl

Ketone-ka cayriin waxaa lagu qasi jiray biyo heerkul ah 30-35 ℃ 25-30 daqiiqo, ka dibna wuxuu istaagay 10-15 daqiiqo;Hal-abuurka hadda

, iyadoo la isticmaalayo 1,1, 3-trichloroacetone cayriin sida walxo ceeriin ah, oo ku jirta kiliga falcelinta, lagu qaso biyo, walaaqay heerkul go'an ka dib markaad istaagto

Delamination.Delamination ka dib, lakabka hoose ee saliidda waa la saaraa, badiyaa iyada oo la saarayo wasakhda koloriin sare oo laga tago xalka sare si loo isticmaalo dambe.

Marka loo eego hal-abuurka, tallaabada (1), cayriin 1,1, 3-trichloroacetone ayaa lagu qasi karaa biyo sidoo kale waa la walaaqi karaa.

Xaaladaha, taas oo aan lahayn xaddidaad gaar ah oo ku saabsan xaaladaha kicinta iyo qalabka, ilaa inta 1,1, 3-trichloroacetone ay noqon karto mid adag.

Alaabta ayaa si siman loogu qasi karaa biyo.Sida fiican, heerka isku-darka waa 100-300r/daqiiqo.

Hal-abuurka hadda, biyuhu waxa ay doorbidayaan biyaha fuuq-baxsan.

Marka loo eego hindisaha, tallaabada (2), xaaladaha recrystalization waxay noqon karaan: heerkulka laga bilaabo 0 ilaa 35 ℃, wakhtiga laga bilaabo 0.5 -

10 saacadood, la doorbidayo, recrystalization waxaa lagu fuliyaa heerka walaaqaya ee 50-300 RPM;Sida fiican, dib-u-kicinta

Biyaha ayaa sidoo kale lagu daraa habka crystallization, halkaas oo biyaha lagu daro heerka 200-600 ml / min;Xaaladahan hoos yimaada, waxtarka recrystalization

Miraha waa wanaagsan yihiin.

[0034] Intaa waxaa dheer, xaaladaha recrystalization waa: heerkulka 10-15 ℃, waqti 2-3 saacadood, iyo xaaladaha recrystalization.

Karistaanka waxaa lagu walaaqay 100-200 RPM biyahana waxaa lagu daraa 300-500 ml/min.

Xaaladahan, saamaynta recystallization ayaa ka fiican.

Hal-abuurka hadda, heerkulka dib-u-crystalization ee lagu sharraxay tallaabada (2) wuu ka hooseeyaa 1,1, 3-trichloroacetone ee tallaabada (1)

Heerkulka ay alaabta lagu qaso biyaha.

Marka loo eego ikhtiraacida, tallaabada (3), isku darka falcelinta ka dib Talaabada (2) waxaa lagu sifeyn karaa cadaadis xiran, ama waxay noqon kartaa

Kiristaalo adag waxaa lagu helaa iyadoo si toos ah loo cadaadiyo saxanka shaandhada ee hoose ee reactor-ka.Hal-abuurka hadda, hawo iyo/ama nitrogen ayaa la doorbidaa in la isticmaalo

Cadaadiska cadaadiska, waxaa fiican inaad isticmaasho nitrogen sifeynta cadaadiska, cadaadiska wuxuu noqon karaa 0.1-0.2MPa, doorbidaya 0.12 -

0. 18 mpa

Marka loo eego ikhtiraacida, crystal-ka degdegay ka dib shaandhaynta cadaadiska waxaa lagu dhaqaa biyo, halkaas oo biyaha la sheegay lagu dhaqo.

Ma jiro xad gaar ah, tusaale ahaan, waxaad dooran kartaa 1-2kg oo ah buufinta biyaha lagu dhaqo iyadoo la raacayo xaaladda heerkulka 2-25 ℃, iyo buufin.

Ma jiro xad gaar ah oo xawli ah.

Marka loo eego hal-abuurka, nadiifnimada 1,1, 3-trichloroacetone ee badeecada cayriin waxay noqon kartaa 50-65 % miisaan ahaan.

Bogagga 3/6 ee tilmaamaha

5

CN 109516908 A

5

Hal-abuurka hadda, dhanka kale, wuxuu sidoo kale bixiyaa folic acid kaas oo ay diyaariyeen mid ka mid ah hababka kor ku xusan

Xalka biyaha leh ee 1,1, 3-trichloroacetone ayaa si toos ah loo isticmaalaa si loogu diyaariyo folic acid.

Hawlgalka habka sifaynta ee ikhtiraacida, sida soo saarista stratified, sifaynta crystallization iyo wixii la mid ah, waxaa lagu fulin karaa nidaam xiran.

Deegaanka-saaxiibtinimo, oo si weyn u yareeya jiilka biyaha wasakhda ah, ma laha qashinka dareeraha dabiiciga ah iyo gaaska qashinka dabiiciga ah;Intaa waxaa dheer, habka nadiifinta

Ma jiro wax dareere ah oo dabiici ah oo la soo bandhigay, iyo wasakhda sare ee koloriinta ayaa laga saaraa inta lagu jiro habka nadiifinta, markaa ma jirto khatar tayo leh tayada folic acid

Habkani wuxuu u isticmaalaa biyaha sida dareeraha crystallization, iyo 1,1, 3-trichloroacetone oo la nadiifiyey oo biyo ah ayaa si toos ah loogu isticmaalaa soo saarista folic acid.

Wadarta wax-soo-saarka folic acid waxaa lagu kordhin karaa 5% miisaan ahaan, nadiifnimaduna waxay ka sarreysaa 99.2 % miisaan ahaan, taasoo heli karta tayo sare leh.

Folic acid.

Hal-abuurka ayaa si faahfaahsan loogu sharraxay qaab-dhismeedka hoose.

[0042] Qaababka soo socda iyo saamiga, ilaa si kale loo cayimin, agabka la isticmaalay waxa lagu heli karaa iibsi ganacsi, ilaa si kale loo cayimin.

Habka loo isticmaalo waa habka caadiga ah ee goobtan.

Qaabka chromatography gaaska wuxuu ahaa GC-2014, oo laga soo iibsaday Shirkadda Shimadzu.

1,1, 3-trichloroacetone oo ay diyaarisay habka sifaynta ee ikhtiraacida hadda jirta [0047] waxaa lagu nadiifiyaa reactor 50 litir ah oo ku qalabaysan saxan shaandho filter hoose ah [0048] Marka hore, nadiifinta 1,1 waa 65 % Miisaanka , 3-trichloroacetone 20Kg iyo biyo 10Kg ee kiliyaha falcelinta isku qasan 24 walaaqaya 12 daqiiqo, halkaas oo heerka walaaqaya yahay 200r/min , ka dibna isku dar ah ayaa istaagay 10 daqiiqo, oo laga soocay lakabka saliidda hoose, ka saar qashinka koloriinta sare;Marka labaad, heerkulka xalka sare ee lakabka ah ayaa hoos loo dhigay ilaa 5 waxaana la walaaqay 2 saacadood oo heerkul ah 100r / min.Kadibna, crystal adag ayaa si toos ah loo helay iyada oo loo marayo saxanka shaandhada ee hoose ee kiliyaha falcelinta by shaandhaynta cadaadiska nitrogen ee cadaadiska 0.1 MPa, ka dibna lagu buufiyo oo lagu dhaqo 2 kg biyo qabow.Miisaanka qoyan ee 1,1, 3-trichloroacetone wuxuu ahaa 9.8 kg, iyo chromatographic saafi ah (GC) wuxuu ahaa 96.8 wt % [0051] Hawlgalka ku lug leh habkan nadiifinta, sida istiraatijiyadda taagan, ka saarida wasakhda koloriin sare, crystallization, sifaynta iyo dhaqidda biyaha, waxaa lagu fulin karaa hab jirka oo xiran, kaas oo deegaanka u wanaagsan, aadna u yareynaya soo saarista biyaha wasakhda ah oo aan soo saarin qashinka dareeraha dabiiciga ah iyo gaaska qashinka dabiiciga ah [0052].Intaa waxaa dheer, sababtoo ah habka nadiifinta iyada oo aan la soo bandhigin dareeraha organic, iyo chlorine sare si looga saaro wasakhda habka nadiifinta, ma jirto khatar tayo leh oo ku saabsan tayada folic acid, laakiin sidoo kale tusaale ahaan hirgelinta diyaarinta 1, 1, 3 - folic acid cross-linked with acetone water in si toos ah loo isticmaalo wax soo saarka, ka dhigaysa folic acid si loo hagaajiyo dhalidda guud 5 miisaanka %, daahirsanaanta 99 5 miisaanka % Tusaalaha 2 [0054] Qaabkani wuxuu sheegayaa in 1,1, 3-trichloroacetone diyaarisay Habka sifaynta ee ikhtiraacida hadda [0055] waxa lagu sifeeyaa reactor 50 litir ah oo lagu rakibay saxan shaandho filter ah xagga hoose [0056] First,1,1 oo nadiif ah 50%, 3-trichloroacetone 20Kg iyo biyo 4Kg isku dhafan in reactor, walaaqaya 15 daqiiqo at 45, heerka walaaqaya ee 300r / min, in habka walaaqaya in lagu daro biyo, biyaha heerka 300 ml / min, ka dibna isku dar ah ayaa istaagay 15 daqiiqo, ka soocay lakabka saliidda hoose, ka saar koloriinta sare ee impurities;Marka labaad, heerkulka xalinta lakabka sare ka dib markii stratification ayaa hoos loo dhigay 20, iyo heerka walaaqaya wuxuu ahaa 200r / min 0.5 h.Kadibna, crystal adag ayaa si toos ah loo helay iyada oo loo marayo saxanka shaandhada ee hoose ee reactor by sifaynta cadaadiska nitrogen ee cadaadiska 0. 2MPa.Kadibna, crystal adag ayaa lagu buufiyay oo lagu maydhay 1Kg oo biyo qabow ah 25, iyo miisaanka qoyan ee 1,1, 3-trichloroacetone wuxuu ahaa 8.2kg habka dhimista Habka nadiifinta ee ku lug leh nadiifinta statification ee ka saarista wasakhda sare ee koloriinta, crystallization, shaandhaynta iyo hawlaha dhaqidda biyaha waxaa lagu fulin karaa in nidaamka jirka oo xiran, deegaanka shaqada waa saaxiibtinimo, oo si weyn u yaraynaysaa jiilka biyaha wasakhda ah, ma qashinka dareere organic iyo gaaska qashinka organic [0060] Intaa waxaa dheer, tan iyo habka sameeyo Aan soo bandhigin dareerayaasha organic waxayna ka saartaa wasakhda koloriin sare inta lagu jiro habka nadiifinta, ma jirto khatar tayo leh tayada folic acid, iyo 1,1, 3-trichloroacetone ee lagu diyaariyey Tusaalaha 2 ayaa lagu milmay biyaha waxaana si toos ah loogu isticmaalaa wax soo saarka folic acid, kordhinta wadarta guud ee folic acid 4.9% miisaan ahaan iyo gaaritaanka daahirsanaanta 99 Qaabkani waxa uu sheegayaa in 1,1, 3-trichloroacetone ay diyaarisay habka sifaynta ee tWaxa uu soo bandhigay ikhtiraacii [0063] waxaa lagu nadiifiyaa reactor 50 litir ah oo lagu rakibay saxan shaandho filter ah xagga hoose [0064] First,1,1 oo nadiif ah 60%, 3-trichloroacetone 20Kg oo lagu qaso biyo 40Kg , walaaqaya 30 daqiiqo 15, heerka walaaqaya ee 100r / min, habka walaaqaya si loogu daro biyo, biyaha heerka 500 ml / min, ka dibna isku dar ah ayaa istaagay 30 daqiiqo, oo laga soocay lakabka hoose ee saliidda , ka saar wasakhda koloriinta sare;Marka labaad, heerkulka xalinta lakabka sare ka dib markii stratification ayaa hoos loo dhigay 10, iyo heerka walaaqu wuxuu ahaa 100r / min 10 saacadood.Dabadeed, crystal adag ayaa si toos ah loo helay iyada oo loo marayo saxanka shaandho ee hoose ee reactor by sifaynta cadaadiska nitrogen ee cadaadiska 0.2MPa, ka dibna lagu buufiyo oo lagu dhaqay 1Kg of 5 biyo qabow.Miisaanka qoyan ee 1,1, 3-trichloroacetone wuxuu ahaa 6.9kg, chromatographic saafi ah (GC)na wuxuu ahaa 98.3% miisaan ahaan [0067] Hawlgalka ku lug leh habkan nadiifinta, sida istiraatijiyad taagan, ka saarista wasakhda koloriin sare, crystallization , sifaynta iyo biyaha dhaqidda, waxaa lagu fulin karaa in nidaamka jirka xiran, kaas oo leh jawi saaxiibtinimo saaxiibtinimo, oo aad u yaraynaysaa jiilka biyaha wasakhda ah oo aan soo saarin qashinka organic dareere iyo gaaska qashinka organic [0068].Intaa waxaa dheer, sababtoo ah habka nadiifinta iyada oo aan la soo bandhigin dareeraha organic, iyo chlorine sare si looga saaro wasakhda habka nadiifinta, ma jirto khatar tayo leh oo ku saabsan tayada folic acid, oo waxay noqon doontaa tusaale ahaan 3 diyaarinta 1, 1, 3 - iskutallaabta. ku xiran acetone, biyaha si ay u milaan, si toos ah loo isticmaalo wax soo saarka ee folic acid, ka dhigaysa folic acid si loo hagaajiyo dhalidda guud 5. 3 miisaanka %, daahirsanaanta 99. 2 miisaanka % Waayo, saamiga 1 [0070] la safeeyey 1,1, 3- trichloroacetone iyadoo loo eegayo habka qaabaynta 1, marka laga reebo in talaabada (1), biyaha aan la isticmaalin, Taa bedelkeeda, dareerayaasha organic ayaa la isticmaalay.Natiijo ahaan, 1,1, 3-trichloroacetone la diyaariyey ayaa lagu milmay biyaha waxaana si toos ah loogu isticmaalay soo saarista folic acid.Wadarta wax-soo-saarka folic acid waxa lagu kordhiyey keliya 2% miisaan ahaan iyo nadiifnimadu 95 % miisaan ahaan.Intaa waxaa dheer, iyada oo ay ugu wacan tahay soo bandhigida dareeraha organic ee habkan nadiifinta, waxaa jira khatar tayo leh tayada folic acid [0071] ee saamiga 2 [0072].1,1, 3-trichloroacetone waa la nadiifiyaa iyadoo loo eegayo habka Tusaalaha 1. Farqiga ayaa ah in Talaabada (1), qadarka biyuhu yahay 50Kg, taasoo keentay koror weyn oo ku yimaada soo saarida biyaha wasakhda ah iyo hoos u dhac ku yimaada 1 dhalidda 1,1, 3-trichloroacetone crystals ayaa lagu milmay biyaha waxaana si toos ah loogu isticmaalay soo saarista folic acid, sidaa darteed wadarta guud ee folic acid ayaa kaliya lagu kordhiyay 5.6% miisaan ahaan nadiiftuna waxay ahayd 99.6% miisaanka [0073] ] liddi ku ah saamiga 3 [0074].1,1 ayaa lagu nadiifiyey habka Tusaalaha 1, 3-trichloroacetone, farqiga u dhexeeya waa in tallaabada (1), koloriin heteroplastid sare aan la saarin, natiijada diyaarinta 1,1, 3-trichloroacetone waxaa ku jira tiro badan. tirada xeryahooda koloriinaysan, tayada khatarta folic acid [0075] Sida ku cad tusaalaha sare ee 1-3 waana natiijada miisaanka 1-3: habka sifaynta waxa ku jira ha u istaago filter-ka kristal ee lakabka ah si meesha looga saaro wasakhda sare ee koloriinta sida dhammaan laakiin nidaamka hawada, jawi shaqo oo saaxiibtinimo leh, oo si weyn u yareeyey dhacdooyinka biyaha wasakhda ah, ma soo saaraan gaaska qashinka ah, dareeraha organic iyo organic Intaa waxaa dheer, iyada oo la fulinayo kiiska 1 diyaarinta 1, 1) , 3-trichloroacetone , ku dar buugga 5/6 bogga 7 CN 109516908 A 7 xal biyaha, oo si toos ah loo isticmaalo soo saarista folic acid, ka dhigi wadarta guud ee folic acid kordhay 5 % by miisaanka, daahirsanaanta waa 99.2 % miisaanka kor ku xusan;Waxaa intaa dheer, sababtoo ah habka nadiifinta ma soo bandhigo dareeraha organic, ma jirto khatar tayo leh tayada folic acid.Waxaa intaa dheer, habka nadiifinta waxay isticmaashaa biyaha sida dareeraha crystallization, iyo xalalka aqueous ee la nadiifiyey ee 1,1, 3-trichloroacetone si toos ah ayaa loo isticmaalaa soo saarista folic acid, yaraynta falcelinta dhinaca

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