A gefe guda, ƙirƙirar tana ba da hanyar tsarkakewa na 1,1, 3-trichloroacetone, inda hanyar ta ƙunshi matakai masu zuwa.
Filashi:
(1) Danyen 1,1, 3-trichloroacetone gauraye da ruwa;
(2) Recrystallization na babban bayani bayan tsayawa; Har da
(3) daskararrun lu'ulu'u da aka sake yi ana tace su kuma a wanke su da ruwa;
A ciki, a cikin Mataki na (1), ma'aunin nauyi na ɗanyen 1,1, 3-trichloroacetone da aka faɗi zuwa adadin ruwa shine 1.
0.1-2).
Zai fi dacewa, a cikin Mataki (1), rabon nauyin ɗanyen samfurin 1,1, 3-trichloroacetone zuwa adadin ruwa zai iya zama 1:
(0.4-0.6), an ƙara ingantawa kamar 1: 0.5; A cikin ƙirƙirar, adadin ɗanyen samfurin 1,1, 3-trichloroacetone da ruwa ana sarrafa shi a sama.
Za a iya samun kewayon babban tsarki 1,1, 3-trichloroacetone.
Dangane da abin da aka ƙirƙira a yanzu, a cikin mataki (1), samfurin ɗanyen samfurin 1,1, 3-trichloroacetone da ruwa ana iya shirya shi a zazzabi na 10-50 ℃.
Mix don minti 10-30 a ƙarƙashin yanayin, sa'an nan kuma bari tsaya na minti 10-30; Zai fi dacewa, a cikin Mataki na (1), in ji 1,1, 3-trichloropropyl
An haxa danyen ketone da ruwa a zafin jiki na 30-35 ℃ na mintuna 25-30, sannan ya tsaya na mintuna 10-15; A cikin ƙirƙira na yanzu
, Yin amfani da danyen 1,1, 3-trichloroacetone a matsayin albarkatun kasa, a cikin kettle dauki, gauraye da ruwa, motsawa a wani zazzabi bayan tsayawa.
Delamination. Bayan an lalatar da shi, ana cire ɓangarorin mai na ƙasa, galibi ta hanyar cire ƙazantaccen sinadarin chlorine da barin babban maganin don amfani daga baya.
Bisa ga ƙirƙirar, a mataki (1), ɗanyen 1,1, 3-trichloroacetone yana haɗe da ruwa kuma ana iya motsa shi.
Yanayi, wanda babu takamaiman iyakancewa akan yanayin motsawa da kayan aiki, muddin 1,1, 3-trichloroacetone na iya zama m.
Za'a iya haɗa samfurin daidai da ruwa. Zai fi dacewa, ƙimar haɗuwa shine 100-300r / min.
A cikin ƙirƙira na yanzu, ruwan ya fi dacewa da ruwa mai lalata.
Bisa ga ƙirƙira, a mataki (2), yanayin recrystallization na iya zama: zazzabi daga 0 zuwa 35 ℃, lokaci daga 0.5 -
10 hours, zai fi dacewa, da recrystallization ne da za'ayi a wani stirring kudi na 50-300 RPM; Zai fi dacewa, reknot
Hakanan ana ƙara ruwa a cikin tsari na crystallization, inda aka ƙara ruwa a cikin adadin 200-600 ml / min; A ƙarƙashin waɗannan sharuɗɗan, ingantaccen recrystallization
'Ya'yan itacen yana da kyau.
[0034] Bugu da ari mafi kyau duka, yanayin recrystallization sune: zazzabi na 10-15 ℃, lokacin sa'o'i 2-3, da yanayin recrystallization.
Ana motsa crystal a cikin adadin 100-200 RPM kuma an ƙara ruwa a cikin adadin 300-500 ml / min.
A ƙarƙashin waɗannan yanayi, tasirin recrystallization ya fi kyau.
A cikin abin da aka ƙirƙira na yanzu, yanayin recrystallization da aka kwatanta a mataki (2) ya yi ƙasa da na 1,1, 3-trichloroacetone a mataki (1)
Yanayin zafin jiki wanda samfurin ya haɗu da ruwa.
Bisa ga ƙirƙirar, a cikin Mataki na (3), cakudawar amsa bayan Mataki na (2) ana iya tacewa ta hanyar rufewa, ko kuma ana iya zama
Ana samun lu'ulu'u masu ƙarfi ta danna kai tsaye ta farantin sieve a ƙasan reactor. A cikin ƙirƙira na yanzu, an fi son amfani da iska da/ko nitrogen
Matsa lamba tacewa, yana da kyau a yi amfani da nitrogen don matsa lamba tacewa, kuma matsa lamba na iya zama 0.1-0.2MPa, zai fi dacewa 0.12 -
0.18 mpa.
Bisa ga ƙirƙirar, kristal da aka haɗe bayan an tace matsi ana wanke shi da ruwa, inda aka wanke ruwan da aka faɗa.
Babu takamaiman iyaka, alal misali, zaku iya zaɓar 1-2kg na wankewar ruwa a ƙarƙashin yanayin zafin jiki na 2-25 ℃, da fesa.
Babu takamaiman iyakar gudu.
Dangane da ƙirƙira, tsabtar ɗanyen samfurin 1,1, 3-trichloroacetone na iya zama 50-65% ta nauyi.
Shafukan 3/6 na koyarwa
5
Bayani na CN109516908
5
Ƙirƙirar da aka kirkira, a daya bangaren kuma, tana samar da sinadarin folic acid wanda aka shirya ta kowace irin hanyoyin 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 hanyar tsarkakewa na ƙirƙira, kamar haɓakar haɓaka, tacewa crystallization da sauransu, a cikin rufaffiyar tsarin.
Muhalli-friendly, da kuma ƙwarai rage samar da sharar gida ruwa, babu sharar Organic kaushi da kwayoyin sharar gas; Bugu da ƙari, hanyar tsarkakewa
Ba a gabatar da kaushi na halitta ba, kuma ana cire ƙazantattun chlorine yayin aikin tsarkakewa, don haka babu haɗarin ingancin ingancin folic acid.
Hanyar tana amfani da ruwa azaman ƙwaƙƙwalwar crystallization, kuma ana amfani da ingantaccen maganin ruwa na 1,1, 3-trichloroacetone kai tsaye don samar da folic acid.
Jimlar yawan amfanin ƙasa na folic acid za a iya ƙarawa da 5% ta nauyi, kuma tsarkin yana sama da 99.2% ta nauyi, wanda zai iya samun babban inganci.
Da folic acid.
An kwatanta ƙirƙirar daki-daki ta hanyar abubuwan da ke ƙasa.
[0042] A cikin abubuwa masu zuwa da ma'auni, sai dai in an kayyade, ana samun kayan da ake amfani da su ta hanyar siyan kasuwanci, sai dai in an kayyade.
Hanyar da ake amfani da ita ita ce hanyar al'ada a wannan filin.
Samfurin chromatography gas shine GC-2014, wanda aka saya daga Kamfanin Shimadzu.
1,1, 3-trichloroacetone da aka shirya ta hanyar tsarkakewa na yanzu [0047] ana tsarkake shi a cikin injin mai lita 50 sanye take da farantin tacewa a ƙasa [0048] Na farko, tsarkin 1,1 shine 65. % ta nauyi , 3-trichloroacetone 20Kg da ruwa 10Kg a cikin tukunyar amsawa gauraye a cikin 24 motsawa na minti 12, inda adadin kuzari shine 200r / min, a cikin tsari don ƙara ruwa, ruwa a cikin wani kudi na 300 ml / min. , sa'an nan kuma cakuda ya tsaya na minti 10, ya rabu da ƙananan man fetur, cire ƙananan chlorine; Abu na biyu, an saukar da zafin jiki na babban bayani mai laushi zuwa 5 kuma an motsa shi tsawon sa'o'i 2 a cikin adadin kuzari na 100r / min. Sa'an nan, da m crystal aka samu kai tsaye ta hanyar sieve farantin a kasa na amsa kettle ta nitrogen matsa lamba tacewa a matsa lamba na 0.1 MPa, sa'an nan kuma fesa da kuma wanke da 2 kg ruwan sanyi. Nauyin rigar na 1,1, 3-trichloroacetone shine 9.8 kg, kuma chromatographic tsarki (GC) shine 96.8 wt % [0051] Ayyukan da ke cikin wannan hanyar tsarkakewa, kamar tsattsauran ra'ayi, kawar da ƙazantattun chlorine, crystallization, tacewa da wanke ruwa, ana iya aiwatar da su a cikin rufaffiyar tsarin jiki, wanda ke da alaƙa da muhalli, kuma yana rage haɓakar samar da ruwan sha da yawa kuma baya haifar da ɓacin rai da iskar gas [0052]. Bugu da ƙari, saboda hanyar tsarkakewa ba tare da gabatar da kwayoyin halitta ba, da kuma babban chlorine don cire ƙazanta a cikin tsarin tsarkakewa, babu wani haɗari mai inganci akan ingancin folic acid, amma kuma ta hanyar aiwatar da misali na shirye-shiryen 1, 1, 3 - folic acid giciye tare da acetone ruwa narkar da kai tsaye amfani da samarwa, sa folic acid don inganta overall yawan amfanin ƙasa 5 nauyi %, da tsarki na 99 5 nauyi % Misali 2 [0054] Wannan embodiment ya bayyana cewa 1,1, 3-trichloroacetone shirya ta hanyar tsarkakewa na yanzu [0055] ana tsarkake shi a cikin injin mai 50-lita sanye take da farantin tacewa a ƙasa [0056] Na farko,1,1 tare da tsaftar 50%, 3-trichloroacetone 20Kg da ruwa 4Kg gauraye. a cikin reactor, motsawa na mintina 15 a 45, nauyin motsawa na 300r / min, a cikin tsari don ƙara ruwa, ruwa a cikin adadin 300 ml / min, sa'an nan kuma cakuda ya tsaya na mintina 15, an raba shi da ruwa. ƙananan man fetur Layer, cire high chlorine impurities; Abu na biyu, yawan zafin jiki na bayani na babba bayan an saukar da stratification zuwa 20, kuma adadin kuzari shine 200r / min na 0.5 h. Sa'an nan, da m crystal aka samu kai tsaye ta sieve farantin a kasa na reactor ta nitrogen matsa lamba tacewa a matsa lamba na 0. 2MPa. Sa'an nan, da m crystal aka fesa da kuma wanke da 1Kg na 25 ruwan sanyi, da kuma rigar nauyi na 1,1, 3-trichloroacetone ya 8.2kg ta hanyar ragewa Hanyar tsarkakewa da hannu a cikin a tsaye stratification kau da high chlorine impurities. crystallization, tacewa da kuma aikin wanke ruwa a cikin Rufaffen tsarin jiki, yanayin aiki yana da abokantaka, kuma yana rage yawan samar da ruwa mai sharar gida, babu sharar kwayoyin halitta da iskar gas [0060] Bugu da ƙari, tun da hanyar ta yi. ba gabatar da kaushi na halitta ba kuma yana kawar da ƙazantattun chlorine yayin aikin tsarkakewa, babu haɗarin ingancin ingancin folic acid, kuma 1,1, 3-trichloroacetone da aka shirya ta Misali 2 an narkar da shi cikin ruwa kuma ana amfani dashi kai tsaye a cikin samar da folic acid, yana ƙara yawan adadin folic acid da kashi 4.9 cikin nauyi da kuma samun tsaftar 99 Wannan sigar ta bayyana cewa 1,1, 3-trichloroacetone wanda aka shirya ta hanyar tsarkakewa na sabon ƙirƙira [0063] an tsarkake shi a cikin 50 -litre reactor Fitted tare da tace sieve farantin a kasa [0064] Na farko,1,1 tare da tsarki na 60% , 3-trichloroacetone 20Kg gauraye da ruwa 40Kg a cikin shan taba, yana motsawa na minti 30 a 15, yawan motsawa. na 100r / min, a cikin tsarin motsawa don ƙara ruwa, ruwa a cikin adadin 500 ml / min, sa'an nan kuma cakuda ya tsaya na minti 30, ya rabu da ƙananan man fetur, cire ƙananan chlorine; Abu na biyu, yawan zafin jiki na bayani na babba bayan an saukar da stratification zuwa 10, kuma adadin kuzari ya kasance 100r / min na awanni 10. Sa'an nan, da m crystal aka samu kai tsaye ta sieve farantin a kasa na reactor ta nitrogen matsa lamba tacewa a matsa lamba na 0.2MPa, sa'an nan kuma fesa da kuma wanke da 1Kg na 5 ruwan sanyi. Nauyin rigar na 1,1, 3-trichloroacetone shine 6.9kg, kuma chromatographic tsarki (GC) shine 98.3% ta nauyi [0067] Ayyukan da ke cikin wannan hanyar tsarkakewa, kamar tsattsauran ra'ayi, kawar da ƙazantattun chlorine, crystallization. , tacewa da wanke ruwa, ana iya aiwatar da su a cikin rufaffiyar tsarin jiki, wanda ke da yanayin aiki na abokantaka, kuma yana rage yawan samar da ruwa mai sharar gida kuma baya haifar da ɓacin rai da iskar gas [0068]. Bugu da ƙari, saboda hanyar tsarkakewa ba tare da gabatar da kwayoyin halitta ba, da kuma babban chlorine don cire ƙazanta a cikin tsarin tsarkakewa, babu wani haɗari mai inganci akan ingancin folic acid, kuma zai zama misali 3 shirye-shiryen 1, 1, 3 - giciye- an danganta shi da acetone, ruwa don narkewa, ana amfani da shi kai tsaye wajen samar da folic acid, yana sa folic acid don haɓaka yawan amfanin ƙasa gabaɗaya 5. 3 nauyi %, tsarki na 99. 2 nauyi % Domin rabo 1 [0070] tsarkake 1,1, 3- trichloroacetone bisa ga hanyar tsari na 1, sai dai a mataki (1), ba a amfani da ruwa ba, maimakon haka, an yi amfani da kaushi na halitta. A 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 amfanin gona na folic acid an ƙaru ne kawai da kashi 2 cikin 100 ta nauyi kuma tsarki ya kasance 95 % ta nauyi. Bugu da kari, saboda gabatarwar kwayoyin kaushi a cikin wannan hanyar tsarkakewa, akwai hadarin inganci ga ingancin folic acid [0071] daidai da 2 [0072]. Ana tsarkake 1,1, 3-trichloroacetone bisa ga hanyar a cikin Misalin 1. Bambanci shine cewa a cikin Mataki na (1), adadin ruwa shine 50Kg, yana haifar da karuwa mai yawa a cikin samar da ruwa mai tsabta da raguwar 1 The yawan amfanin ƙasa na 1,1, 3-trichloroacetone lu'ulu'u an narkar da shi cikin ruwa kuma an yi amfani da shi kai tsaye wajen samar da folic acid, don haka jimlar yawan amfanin folic acid kawai ya karu da 5.6% ta nauyi kuma tsarki ya kasance 99.6% ta nauyi [0073] ] a kan rabo na 3 [0074]. 1,1 an tsarkake shi ta hanyar Misalin 1, 3-trichloroacetone, bambanci shine cewa a cikin mataki (1), ba a cire babban heteroplastid chlorine ba, sakamakon shirye-shiryen 1,1, 3-trichloroacetone ya ƙunshi babban abu. adadin mahadi na chlorinated, ingancin haɗarin folic acid [0075] Dangane da misalin da ke sama na 1-3 kuma shine sakamakon sikelin 1-3: hanyar tsarkakewa ya haɗa da barin matattarar ƙira mai ɗorewa don cire manyan ayyukan wankin chlorine. kamar su duka amma a cikin tsarin iska, yanayin aiki na abokantaka, da kuma rage yawan abin da ya faru na ruwa mai sharar gida, baya haifar da iskar gas, kwayoyin halitta da kwayoyin halitta Bugu da ƙari, ta hanyar aiwatar da yanayin 1 da shirye-shiryen 1, 1) , 3-trichloroacetone. , ƙara a cikin littafin 5/6 shafi na 7 CN 109516908 A 7 maganin ruwa, wanda aka yi amfani da shi kai tsaye wajen samar da folic acid, ya sa yawan amfanin folic acid ya karu da kashi 5 cikin 100 da nauyi, tsarki ya kai kashi 99.2 % bisa nauyi; Haka kuma, saboda hanyar tsarkakewa ba ta gabatar da kaushi na halitta ba, babu haɗarin ingancin ingancin folic acid. Bugu da ƙari, hanyar tsarkakewa tana amfani da ruwa a matsayin mai narkewar crystallization, kuma ana amfani da maganin ruwa mai tsabta na 1,1, 3-trichloroacetone kai tsaye wajen samar da folic acid, yana rage halayen gefe.
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