A gefe guda, ƙirƙira ta samar da hanyar tsarkakewa ta 1,1, 3-trichloroacetone, inda hanyar ta ƙunshi matakai masu zuwa
Wasiƙa:
(1) Ɗanyen 1, 1, 3-trichloroacetone da aka haɗa da ruwa;
(2) Sake kunna maganin saman bayan ya tsaya;
(3) ana tace lu'ulu'u masu ƙarfi da aka sake yin amfani da su sannan a wanke su da ruwa;
A cikin Mataki na (1), rabon nauyin da aka ambata na ɗanyen 1, 1, 3-trichloroacetone zuwa adadin ruwa shine 1
0.1-2).
Zai fi kyau, a Mataki na (1), rabon nauyin samfurin ɗanyen mai na 1, 1, 3-trichloroacetone zuwa adadin ruwa zai iya zama 1:
(0.4-0.6), an ƙara inganta shi azaman 1:0.5; A cikin ƙirƙira, ana sarrafa yawan samfurin ɗanyen mai na 1,1, 3-trichloroacetone da ruwa a cikin abin da ke sama.
Ana iya samun kewayon tsarki mai girma 1,1,3-trichloroacetone.
A bisa ga wannan ƙirƙira, a mataki na (1), ana iya shirya samfurin ɗanyen mai na 1, 1, 3-trichloroacetone da ruwa a zafin ℃ 10-50
A gauraya na minti 10-30 a ƙarƙashin yanayin, sannan a bar shi ya tsaya na minti 10-30; Zai fi kyau, a Mataki na (1), in ji 1, 1, 3-trichloropropyl
An gauraya ɗanyen ketone ɗin da ruwa a zafin 30-35℃ na tsawon mintuna 25-30, sannan aka bar shi na mintuna 10-15; A cikin wannan ƙirƙira, an haɗa shi da ruwa a zafin 30-35℃ na tsawon mintuna 25-30, sannan aka bar shi na mintuna 10-15;
, ta amfani da ɗanyen 1, 1, 3-trichloroacetone a matsayin kayan da aka sarrafa, a cikin kettle na amsawa, a gauraya da ruwa, a juya a wani zafin jiki bayan ya tsaya
Ragewar ƙasa. Bayan ragewar ƙasa, ana cire ƙananan man fetur, galibi ta hanyar cire ƙazanta mai yawan sinadarin chlorine sannan a bar ruwan sama don amfani daga baya.
A bisa ga wannan ƙirƙira, a mataki na (1), ana haɗa ɗanyen 1,1, 3-trichloroacetone da ruwa kuma ana iya juyawa shi.
Yanayi, wanda babu takamaiman iyakancewa akan yanayin motsawa da kayan aiki, matuƙar 1, 1, 3-trichloroacetone na iya zama mai kauri
Ana iya haɗa samfurin daidai gwargwado da ruwa. Zai fi kyau a haɗa shi da ruwa 100-300r/min.
A cikin wannan ƙirƙira, ruwan ya fi dacewa a cire shi daga jiki.
A bisa ga wannan ƙirƙira, a mataki na (2), yanayin sake saitawa na iya zama: zafin jiki daga 0 zuwa 35℃, lokaci daga 0.5 -
Awa 10, zai fi kyau a yi amfani da na'urar sake kunna wutar a cikin saurin juyawa na 50-300 RPM; Zai fi kyau a yi amfani da na'urar sake kunna wutar a cikin mintuna 10 kawai.
Ana kuma ƙara ruwa a cikin tsarin lu'ulu'u, inda ake ƙara ruwan a cikin adadin 200-600 ml/min; A ƙarƙashin waɗannan yanayi, ingancin sake yin amfani da shi
'Ya'yan itace suna da kyau.
[0034] Bugu da ƙari, yanayin sake kunnawa shine: zafin jiki na 10-15℃, lokacin awanni 2-3, da yanayin sake kunnawa
Ana jujjuya lu'ulu'un a cikin saurin gudu na 100-200 RPM sannan a ƙara ruwan a cikin saurin 300-500 ml/min.
A ƙarƙashin waɗannan yanayi, tasirin sake yin amfani da shi ya fi kyau.
A cikin wannan ƙirƙira, zafin sake sake fasalin da aka bayyana a mataki na (2) ya yi ƙasa da na 1,1, 3-trichloroacetone a mataki na (1)
Zafin da aka haɗa samfurin da ruwa.
A cewar wannan ƙirƙira, a Mataki na (3), ana iya tace cakuda amsawar bayan Mataki na (2) ta hanyar matsi mai rufewa, ko kuma a iya tace shi ta hanyar matsi mai rufewa, ko kuma a iya tace shi ta hanyar matsi mai rufewa.
Ana samun lu'ulu'u masu ƙarfi ta hanyar danna kai tsaye ta cikin farantin sieve da ke ƙasan reactor ɗin. A cikin wannan ƙirƙira, ana amfani da iska da/ko nitrogen sosai.
Tacewar matsi, ya fi kyau a yi amfani da nitrogen don tace matsi, kuma matsin lambar na iya zama 0.1-0.2MPa, zai fi dacewa 0.12 -
0. 18 mpa.
A cewar wannan ƙirƙira, ana wanke lu'ulu'u mai fashewa bayan tacewa da ruwa, inda ake wanke ruwan da aka ambata.
Babu takamaiman iyaka, misali, za ku iya zaɓar 1-2kg na wanke feshi na ruwa a ƙarƙashin yanayin zafin jiki na 2-25℃, sannan ku fesa, sannan ku fesa.
Babu takamaiman iyaka ta gudu.
A cewar wannan ƙirƙira, tsarkin samfurin ɗanyen mai na 1,1, 3-trichloroacetone na iya zama kashi 50-65% na nauyi.
Shafuka 3/6 na koyarwa
5
CN 109516908 A
5
Wannan ƙirƙira ta yanzu, a gefe guda kuma, tana samar da sinadarin folic acid wanda aka shirya ta kowace hanya da aka bayyana a sama.
Ana amfani da maganin ruwa na 1,1, 3-trichloroacetone kai tsaye don shirya folic acid.
Ana iya aiwatar da aikin hanyar tsarkakewa ta wannan ƙirƙira, kamar cirewa mai tsari, tacewa ta hanyar lu'ulu'u da sauransu, a cikin tsarin rufewa.
Yana da kyau ga muhalli, kuma yana rage yawan samar da ruwan sharar gida, babu sharar da ke cikin sinadarai masu guba da kuma iskar sharar gida ta halitta; Bugu da ƙari, hanyar tsarkakewa
Ba a shigar da sinadarai masu narkewar halitta ba, kuma ana cire yawan gurɓataccen sinadarin chlorine yayin aikin tsarkakewa, don haka babu haɗarin inganci ga ingancin folic acid.
Hanyar tana amfani da ruwa a matsayin sinadarin crystallization, kuma ana amfani da maganin ruwa mai tsabta na 1,1, 3-trichloroacetone kai tsaye don samar da folic acid.
Jimlar yawan folic acid za a iya ƙarawa da kashi 5% ta nauyi, kuma tsarkin ya wuce kashi 99.2% ta nauyi, wanda zai iya samun inganci mai kyau.
Na folic acid.
An bayyana wannan ƙirƙira dalla-dalla ta hanyar amfani da misalai da ke ƙasa.
[0042] A cikin waɗannan misalai da ma'auni, sai dai idan an ƙayyade akasin haka, kayan da ake amfani da su suna samuwa ta hanyar siyan kasuwanci, sai dai idan an ƙayyade akasin haka
Hanyar da aka yi amfani da ita ita ce hanyar da aka saba amfani da ita a wannan fanni.
An yi amfani da samfurin chromatography na gas ɗin GC-2014, wanda aka saya daga Kamfanin Shimadzu.
An shirya 1,1, 3-trichloroacetone ta hanyar hanyar tsarkakewa ta wannan ƙirƙira [0047] a cikin wani reactor mai lita 50 wanda aka sanya masa farantin sieve a ƙasan [0048]. Da farko, tsarkin 1,1 shine kashi 65% na nauyi, 3-trichloroacetone 20Kg da ruwa 10Kg a cikin kettle na amsawa wanda aka gauraya a cikin 24 yana juyawa na tsawon mintuna 12, inda saurin juyawa shine 200r/min, a cikin tsarin juyawa don ƙara ruwa, ruwan a cikin adadin 300 ml/min, sannan cakuda ya tsaya na mintuna 10, an raba shi da ƙaramin layin mai, an cire ƙazanta mai yawan chlorine; Na biyu, an rage zafin ruwan saman da aka yi wa layi zuwa 5 kuma an gauraya na tsawon awanni 2 a saurin juyawa na 100r/min. Bayan haka, an samo lu'ulu'u mai ƙarfi kai tsaye ta cikin farantin sieve a ƙasan kettle ɗin amsawa ta hanyar tace matsi na nitrogen a matsin lamba na 0.1 MPa, sannan aka fesa aka wanke da ruwan sanyi na kilogiram 2. Nauyin jika na 1,1, 3-trichloroacetone shine kilogiram 9.8, kuma tsarkin chromatographic (GC) shine 96.8 wt% [0051] Aikin da ke cikin wannan hanyar tsarkakewa, kamar rarrabuwar kai tsaye, cire ƙazanta masu yawan chlorine, lu'ulu'u, tacewa da wanke ruwa, ana iya aiwatar da shi a cikin tsarin jiki mai rufewa, wanda ke da kyau ga muhalli, kuma yana rage yawan samar da ruwan sharar gida kuma baya samar da sharar da ke narkewa da iskar sharar gida ta halitta [0052]. Bugu da ƙari, saboda hanyar tsarkakewa ba tare da gabatar da sinadarin sinadarai na halitta ba, da kuma yawan sinadarin chlorine don cire ƙazanta a cikin tsarin tsarkakewa, babu haɗarin inganci akan ingancin folic acid, amma kuma ta hanyar aiwatar da samfurin 1, 1, 3 – folic acid da aka haɗa da ruwan acetone wanda aka narkar da shi kai tsaye ana samarwa, yana sa folic acid ya inganta yawan amfanin ƙasa 5%, tsarkin 99 5 % nauyi % Misali na 2 [0054] Wannan misali ya bayyana cewa 1, 1, 3-trichloroacetone da aka shirya ta hanyar tsarkakewa ta wannan ƙirƙira [0055] an tsarkake shi a cikin reactor mai lita 50 wanda aka sanye da farantin sieve na tacewa a ƙasan [0056] Da farko, 1, 1 tare da tsarkin 50% , 3-trichloroacetone 20Kg da ruwa 4Kg da aka gauraya a cikin reactor, ana juyawa na minti 15 a 45, saurin juyawa na 300r/min, a cikin tsarin juyawa don ƙara ruwa, ruwan a cikin ƙimar 300 ml/min, sannan cakuda ya tsaya Na tsawon mintuna 15, an raba shi da ƙaramin mai, an cire ƙazanta mai yawa daga chlorine; Na biyu, an rage zafin ruwan saman bayan an raba shi zuwa 20, kuma saurin juyawa shine 200r/min na tsawon awanni 0.5. Sannan, an samo lu'ulu'u mai ƙarfi kai tsaye ta cikin farantin sieve a ƙasan reactor ta hanyar tace matsin lamba na nitrogen a matsin lamba na 0.2MPa. Sannan, an fesa lu'ulu'u mai ƙarfi kuma an wanke shi da kilogiram 1 na ruwan sanyi 25, kuma nauyin jika na 1,1, 3-trichloroacetone ya kai kilogiram 8.2 ta hanyar ragewa. Hanyar tsarkakewa da ke tattare da cire datti mai yawan chlorine, crystallization, tacewa da ayyukan wanke ruwa za a iya aiwatar da su a cikin tsarin jiki mai rufewa, yanayin aiki yana da kyau, kuma yana rage yawan samar da ruwan sharar gida, babu sharar mai narkewar kwayoyin halitta da iskar sharar kwayoyin halitta [0060] Bugu da ƙari, tunda hanyar ba ta gabatar da sinadarai masu narkewar kwayoyin halitta ba kuma tana cire datti mai yawa na chlorine yayin aikin tsarkakewa, babu haɗarin inganci ga ingancin folic acid, kuma 1,1, 3-trichloroacetone da aka shirya ta Misali na 2 ana narkar da shi a cikin ruwa kuma ana amfani da shi kai tsaye wajen samar da folic acid, yana ƙara yawan yawan folic acid da kashi 4.9% ta nauyi kuma ya cimma tsarkin 99. Wannan misali ya bayyana cewa 1,1, 3-trichloroacetone da aka shirya ta hanyar hanyar tsarkakewa ta wannan ƙirƙira [0063] an tsarkake shi a cikin wani reactor mai lita 50. An sanya farantin sieve mai tacewa a ƙasan [0064] Da farko,1,1 tare da tsarkin 60% , 3-trichloroacetone 20Kg da aka gauraya da ruwa 40Kg a cikin kettle na amsawa, ana juyawa na minti 30 a 15, saurin juyawa na 100r/min, a cikin tsarin juyawa don ƙara ruwa, ruwan a 500 ml/min, sannan cakuda ya tsaya na minti 30, an raba shi da ƙasan mai, an cire ƙazanta mai yawa na chlorine; Na biyu, an rage zafin ruwan saman Layer bayan raba shi zuwa 10, kuma saurin juyawa shine 100r/min na tsawon awanni 10. Sannan, an samo lu'ulu'u mai ƙarfi kai tsaye ta cikin farantin sieve a ƙasan reactor ta hanyar tace matsi na nitrogen a 0.2MPa, sannan a fesa a wanke da 1Kg na ruwan sanyi 5. Nauyin jika na 1,1, 3-trichloroacetone shine 6.9kg, kuma chromatographic pure (GC) shine 98.3% ta nauyi [0067] Aikin da aka yi a cikin wannan hanyar tsarkakewa, kamar rarrabuwar kai tsaye, cire ƙazanta masu yawan chlorine, lu'ulu'u, tacewa da wanke ruwa, ana iya aiwatar da shi a cikin tsarin jiki mai rufewa, wanda ke da yanayin aiki mai kyau, kuma yana rage yawan samar da ruwan sharar gida kuma baya samar da sharar da ke narkewa da iskar sharar gida ta halitta [0068]. Bugu da ƙari, saboda hanyar tsarkakewa ba tare da gabatar da sinadarin sinadarai na halitta ba, da kuma yawan sinadarin chlorine don cire ƙazanta a cikin tsarin tsarkakewa, babu haɗarin inganci akan ingancin folic acid, kuma zai zama misali 3 shiri na 1, 1, 3 - wanda aka haɗa shi da acetone, ruwa don narkewa, wanda ake amfani da shi kai tsaye wajen samar da folic acid, yana sa folic acid ya inganta yawan amfanin ƙasa 5.3 %, tsarkin 99. 2 % Domin rabo 1 [0070] tsarkake 1, 1, 3-trichloroacetone bisa ga hanyar misali 1, sai dai a mataki na (1), ba a yi amfani da ruwa ba. Madadin haka, an yi amfani da sinadaran sinadarai na halitta. Sakamakon haka, an narkar da 1, 1, 3-trichloroacetone da aka shirya a cikin ruwa kuma an yi amfani da shi kai tsaye wajen samar da folic acid. Jimlar yawan folic acid ya karu da kashi 2% kawai ta nauyi kuma tsarkin ya kasance kashi 95% ta nauyi. Bugu da ƙari, saboda shigar da sinadarai masu narkewa a cikin wannan hanyar tsarkakewa, akwai haɗarin inganci ga ingancin folic acid [0071] a cikin rabo na 2 [0072]. Ana tsarkake 1,1, 3-trichloroacetone bisa ga hanyar da ke cikin Misali na 1. Bambancin shine a Mataki na (1), adadin ruwan shine 50Kg, wanda ya haifar da ƙaruwa mai yawa a cikin samar da ruwan sharar gida da raguwar 1. An narkar da yawan lu'ulu'u 1,1, 3-trichloroacetone a cikin ruwa kuma an yi amfani da shi kai tsaye wajen samar da folic acid, don haka jimlar yawan folic acid ya ƙaru da kashi 5.6% kawai ta nauyi kuma tsarkin ya kasance kashi 99.6% ta nauyi [0073] idan aka kwatanta da rabon 3 [0074]. An tsarkake 1,1 ta hanyar hanyar Misali na 1, 3-trichloroacetone, bambancin shine a mataki na (1), ba a cire babban sinadarin chlorine heteroplastid ba, sakamakon shirya 1,1, 3-trichloroacetone ya ƙunshi adadi mai yawa na mahaɗan chlorine, ingancin haɗarin folic acid [0075] Dangane da misalin da ke sama 1-3 kuma shine sakamakon sikelin 1-3: hanyar tsarkakewa ta ƙunshi barin matattarar lu'ulu'u mai layi don cire ƙazanta mai yawan chlorine kamar duk wani abu banda tsarin hana iska, yanayin aiki mai kyau, da kuma rage yawan ruwan sharar gida sosai, baya samar da iskar gas mai sharar gida, mai narkewar halitta da kuma mai halitta. Bugu da ƙari, ta hanyar aiwatar da shari'a ta 1, shiri na 1, 1), 3-trichloroacetone, ƙara a cikin littafin shafi na 5/6 7 CN 109516908 Maganin ruwa na 7, wanda ake amfani da shi kai tsaye wajen samar da folic acid, yana sa jimlar yawan folic acid ya karu da kashi 5% ta nauyi, tsarki shine 99.2 % ta nauyi a sama; Bugu da ƙari, saboda hanyar tsarkakewa ba ta gabatar da sinadarin narkewar halitta ba, babu haɗarin inganci ga ingancin folic acid. Bugu da ƙari, hanyar tsarkakewa tana amfani da ruwa a matsayin sinadarin narkewar crystallization, kuma ana amfani da maganin ruwa mai tsabta na 1,1, 3-trichloroacetone kai tsaye wajen samar da folic acid, wanda ke rage tasirin sakamako.
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