Ma ka lima hoʻokahi, hāʻawi ka mea hana i kahi ʻano hoʻomaʻemaʻe o 1,1, 3-trichloroacetone, kahi i loaʻa ai ke ʻano i nā pae aʻe.

Flash:

(1) Crude 1,1, 3-trichloroacetone i hui pū ʻia me ka wai;

(2) Recrystallization o ka hopena luna ma hope o ke ku ana; A ʻo kekahi

(3) ua kānana ʻia a holoi ʻia me ka wai;

No laila, ma ka ʻanuʻu (1), ʻo ka ratio paona o ka palaka 1,1, 3-trichloroacetone i ʻōlelo ʻia i ka nui o ka wai he 1.0.1-2).

ʻOi aku ka maikaʻi, ma ka ʻanuʻu (1), ʻo ka ratio paona o ka huahana crude 1,1, 3-trichloroacetone i ka nui o ka wai hiki ke 1:

(0.4-0.6), hoʻonui hou ʻia e like me 1:0.5; I loko o ka mea hou, ua mālama ʻia ke ʻano o 1,1, 3-trichloroacetone crude huahana a me ka wai ma luna.

Hiki ke loaʻa ka laulā o ka maʻemaʻe kiʻekiʻe 1,1, 3-trichloroacetone.

Wahi a ka mea hou i kēia manawa, ma ka ʻanuʻu (1), hiki ke hoʻomākaukau ʻia ka 1,1, 3-trichloroacetone crude huahana a me ka wai ma kahi mahana o 10-50 ℃

E hui no 10-30 mau minuke ma lalo o nā kūlana, a laila e kū no 10-30 mau minuke; ʻOi aku ka maikaʻi, ma ka Step (1), i ʻōlelo ʻia 1,1, 3-trichloropropyl

Ua hui ʻia ka ketone crude me ka wai ma kahi mahana o 30-35 ℃ no 25-30 mau minuke, a laila kū no 10-15 mau minuke; I ka mea hou i keia wa

, e hoʻohana ana i ka 1,1, 3-trichloroacetone crude e like me ka mea maka, i loko o ka ipu aniani, hui pū ʻia me ka wai, hoʻoulu ʻia i kahi mahana ma hope o ke kū ʻana.

Delamination. Ma hope o ka delamination, hoʻoneʻe ʻia ka papa ʻaila haʻahaʻa, ʻoi loa ma ka wehe ʻana i nā haumia chlorine kiʻekiʻe a waiho i ka hopena o luna no ka hoʻohana ʻana ma hope.

Wahi a ka mea hou, ma ka ʻanuʻu (1), ua hui pū ʻia ka crude 1,1, 3-trichloroacetone me ka wai a hiki ke hoʻoulu ʻia.

ʻO nā kūlana, ʻaʻohe palena kikoʻī i nā kūlana hoʻouluulu a me nā mea hana, ʻoiai ka lōʻihi o ka 1,1, 3-trichloroacetone hiki ke koʻikoʻi.

Hiki ke hui like ka huahana me ka wai. ʻOi aku ka maikaʻi, ʻo ka helu hui ʻana he 100-300r / min.

I kēia mea hou, ʻoi aku ka maikaʻi o ka wai deionized.

Wahi a ka mea hou, ma ka ʻanuʻu (2), ʻo nā kūlana recrystallization paha: ka mahana mai 0 a 35 ℃, manawa mai 0.5 -

10 mau hola, ʻoi aku ka maikaʻi, hoʻokō ʻia ka recrystallization ma kahi wikiwiki o 50-300 RPM; ʻOi aku ka maikaʻi, ʻo ka reknot

Hoʻohui pūʻia ka wai i ke kaʻina hana crystallization, kahi i hoʻohuiʻia ai ka wai ma kahi o 200-600 ml / min; Ma lalo o kēia mau kūlana, ka pono o ka recrystallization

Maikaʻi nā hua.

[0034] ʻOi aku ka maikaʻi, nā kūlana recrystallization: kahi mahana o 10-15 ℃, kahi manawa o 2-3 mau hola, a me nā kūlana recrystallization.

Hoʻouluʻia ka'ōmole ma kahi o 100-200 RPM a hoʻohuiʻia ka wai ma kahi o 300-500 ml / min.

Ma lalo o kēia mau kūlana, ʻoi aku ka maikaʻi o ka hopena recrystallization.

I kēia mea hou, ʻoi aku ka haʻahaʻa o ka mahana recrystallization i hōʻike ʻia ma ka ʻanuʻu (2) ma mua o ka 1,1, 3-trichloroacetone ma ka ʻanuʻu (1)

ʻO ka mahana i hui ʻia ka huahana me ka wai.

Wahi a ka mea hou, ma ka ʻanuʻu (3), hiki ke kānana ʻia ka hui ʻana ma hope o ka ʻanuʻu (2).

Loaʻa nā kristal paʻa ma ke kaomi pololei ʻana ma o ka sieve plate ma lalo o ka reactor. I kēia mea hou, hoʻohana maikaʻi ʻia ka ea a/a i ʻole nitrogen

ʻO ka kānana kaomi, ʻoi aku ka maikaʻi o ka hoʻohana ʻana i ka nitrogen no ka kānana kaomi, a hiki i ke kaomi ke 0.1-0.2MPa, ʻoi aku ka maikaʻi o 0.12 -

0. 18 mpa.

Wahi a ka mea i hana ʻia, holoi ʻia ka kristal i hoʻoheheʻe ʻia ma hope o ka kānana kaomi ʻana me ka wai, kahi e holoi ʻia ai ka wai i ʻōlelo ʻia.

ʻAʻohe palena kikoʻī, no ka laʻana, hiki iā ʻoe ke koho i ka 1-2kg o ka holoi ʻana i ka wai ma lalo o ke kūlana o ka mahana o 2-25 ℃, a me ka pīpī.

ʻAʻohe palena wikiwiki.

Wahi a ka mea hou, hiki i ka 50-65% ka maʻemaʻe o ka 1,1, 3-trichloroacetone crude huahana.

Nā ʻaoʻao 3/6 o ke aʻo ʻana

5

CN 109516908 A

5

ʻO ka mea hou i kēia manawa, ma kekahi ʻaoʻao, hāʻawi pū kekahi i ka waikawa folic i hoʻomākaukau ʻia e kekahi o nā ʻano i hōʻike ʻia ma luna

Hoʻohana pololei ʻia kahi hopena wai o 1,1, 3-trichloroacetone e hoʻomākaukau ai i ka waikawa folic.

ʻO ka hana o ke ʻano hoʻomaʻemaʻe o ka mea hou, e like me ka stratified extraction, crystallization filtration a pēlā aku, hiki ke hana ʻia i loko o kahi ʻōnaehana pani.

Pilikia kaiapuni, a hoemi loa i ka hana ana i ka wai palau, aohe mea hoohehee a me ke kinoea kino; Eia kekahi, ke ʻano hoʻomaʻemaʻe

ʻAʻole hoʻokomo ʻia nā mea hoʻoheheʻe organik, a ua wehe ʻia nā haumia chlorine kiʻekiʻe i ka wā o ka hoʻomaʻemaʻe ʻana, no laila ʻaʻohe pilikia maikaʻi i ka maikaʻi o ka folic acid.

Hoʻohana ke ʻano i ka wai ma ke ʻano he crystallization solvent, a hoʻohana pololei ʻia ka wai hoʻomaʻemaʻe ʻia o 1,1, 3-trichloroacetone no ka hana ʻana i ka waikawa folic.

Hiki ke hoʻonui ʻia ka nui o ka waikawa folic e 5% ma ke kaupaona, a ʻoi aku ka maʻemaʻe ma luna o 99.2% ma ke kaupaona, hiki ke loaʻa i ke ʻano kiʻekiʻe.

ʻO ka waikawa folic.

Ua wehewehe kikoʻī ʻia ka mea i ʻike ʻia ma o nā hoʻohālike ma lalo nei.

[0042] Ma nā ʻano like ʻole a me nā ʻāpana like ʻole, ke ʻole i kuhikuhi ʻia, loaʻa nā mea i hoʻohana ʻia ma o ke kūʻai ʻana aku, ke ʻole i kuhikuhi ʻia.

ʻO ke ʻano i hoʻohana ʻia ʻo ke ʻano hana maʻamau i kēia kahua.

ʻO GC-2014 ke kumu hoʻohālike kinoea chromatography, i kūʻai ʻia mai Shimadzu Company.

ʻO ka 1,1, 3-trichloroacetone i hoʻomākaukau ʻia e ke ʻano hoʻomaʻemaʻe o kēia mea hou [0047] ua hoʻomaʻemaʻe ʻia i loko o kahi reactor 50-lita i hoʻolako ʻia me kahi kānana kānana ma lalo [0048] ʻO ka mua, ʻo ka maʻemaʻe o 1,1 he 65 % ma ke kaumaha , 3-trichloroacetone 20Kg a me ka wai 10Kg i loko o ka hopena kettle i hui pū ʻia i 24 hoʻoulu ʻia no 12 mau minuke, kahi o ka hoʻouluulu ʻana he 200r/min, i ke kaʻina hana e hoʻohui i ka wai, ka wai ma kahi o 300 ml / min. , a laila kū ka hui ʻana no 10 mau minuke, hoʻokaʻawale ʻia mai ka papa ʻaila haʻahaʻa, e wehe i nā haumia chlorine kiʻekiʻe; ʻO ka lua, ua hoʻohaʻahaʻa ʻia ka mahana o ka hopena o luna i 5 a hoʻoulu ʻia no 2 mau hola ma ka wikiwiki o 100r / min. A laila, ua loaʻa pololei ke aniani paʻa ma o ka kānana papa ma lalo o ka ipu hoʻoheheʻe ʻia e ka kānana kaomi ʻana o ka nitrogen ma ke kaomi o 0.1 MPa, a laila kāpī ʻia a holoi ʻia me 2 kg wai anuanu. ʻO ke kaumaha wai o 1,1, 3-trichloroacetone he 9.8 kg, a ʻo ka chromatographic pure (GC) he 96.8 wt % [0051] ʻO ka hana i komo i kēia ʻano hoʻomaʻemaʻe, e like me ka stratification static, ka wehe ʻana i nā haumia chlorine kiʻekiʻe, crystallization, ʻO ka kānana a me ka holoi wai, hiki ke hana ʻia i loko o kahi ʻōnaehana kino paʻa, ʻo ia ka mea pili i ke kaiapuni, a hoʻemi nui i ka hana ʻana o ka wai ʻōpala a ʻaʻole hoʻopuka i ka ʻōpala organik a me nā kinoea ʻōpala [0052]. Eia kekahi, no ka mea, ʻo ke ʻano hoʻomaʻemaʻe me ka ʻole o ka hoʻokomo ʻana i ka mea hoʻoheheʻe organik, a me ka chlorine kiʻekiʻe e wehe i nā haumia i ke kaʻina hoʻomaʻemaʻe, ʻaʻohe pilikia maikaʻi i ka maikaʻi o ka folic acid, akā ma o ka hoʻokō hoʻohālike o ka hoʻomākaukau ʻana o 1, 1, 3 - folic acid cross-linked me ka acetone wai i hoʻoheheʻe ʻia i hoʻohana pono ʻia i ka hana ʻana, hana i ka folic acid e hoʻomaikaʻi i ka hua holoʻokoʻa 5 paona %, ka maʻemaʻe o 99 5 paona % Laʻana 2 [0054] Ke ʻōlelo nei kēia ʻano he 1,1, 3-trichloroacetone i hoʻomākaukau ʻia e ua hoʻomaʻemaʻe ʻia ke ʻano hoʻomaʻemaʻe o ka mea hou [0055] i loko o kahi reactor 50-lita i hoʻolako ʻia me kahi kānana kānana ma lalo [0056] ʻO ka mua, 1,1 me ka maʻemaʻe o 50% , 3-trichloroacetone 20Kg a me ka wai 4Kg hui pū ʻia. i loko o ka reactor, e hoʻoulu ana no 15 mau minuke ma 45, ka 300r / min ka hoʻouluʻana, i ka hoʻouluʻana e hoʻonui i ka wai, ka wai ma kahi o 300 ml / min, a laila kū ka hui no 15 mau minuke, i hoʻokaʻawaleʻia mai ka papa ʻaila haʻahaʻa, wehe i nā haumia chlorine kiʻekiʻe; ʻO ka lua, ua hoʻohaʻahaʻa ʻia ka mahana o ka hopena papa luna ma hope o ka stratification i 20, a ʻo ka hoʻoulu ʻana ʻo 200r / min no 0.5 h. A laila, ua loaʻa pololei ke aniani paʻa ma o ka sieve plate ma ka lalo o ka reactor e ka kānana kaomi ʻana o ka nitrogen ma ke kaomi o 0. 2MPa. A laila, kāpīpī ʻia ka aniani paʻa a holoi ʻia me 1Kg o 25 wai anuanu, a ʻo ke kaumaha o 1,1, 3-trichloroacetone he 8.2kg ma ke ʻano o ka hoʻohaʻahaʻa ʻana. hiki ke hana i ka crystallization, kānana a me ka holoi ʻana i ka wai ma kahi ʻōnaehana kino paʻa, ʻoluʻolu ke ʻano hana, a hoʻohaʻahaʻa loa i ka hana ʻana o ka wai ʻōpala, ʻaʻohe mea hoʻoheheʻe organik a me nā kinoea ʻōpala organik [0060] Eia kekahi, ʻoiai ke ʻano hana. ʻaʻole hoʻokomo i nā mea hoʻoheheʻe organik a wehe i nā haumia chlorine kiʻekiʻe i ka wā o ka hoʻomaʻemaʻe ʻana, ʻaʻohe pilikia maikaʻi i ka maikaʻi o ka folic acid, a ʻo ka 1,1, 3-trichloroacetone i hoʻomākaukau ʻia e ka laʻana 2 ua hoʻoheheʻe ʻia i ka wai a hoʻohana pololei ʻia i ka hana ʻana o folic acid, e hoonui ana i ka huina hoonui o ka waika folic e 4.9% ma ke kaumaha a loaa ka maemae o 99 Ua hoike mai keia mea i hoomaemaeia ka 1,1, 3-trichloroacetone i hoomakaukauia e ke ano hoomaemae o ka mea i hanaia i keia manawa [0063] ma kahi 50 -lire reactor i hoʻokomo ʻia me kahi kānana kānana pā ma lalo [0064] ʻO ka mua, 1,1 me ka maʻemaʻe o 60%, 3-trichloroacetone 20Kg i hui pū ʻia me ka wai 40Kg i loko o ka ipu hoʻonā, hoʻoulu ʻia no 30 mau minuke ma 15, ka wikiwiki o ka hoʻoulu ʻana. o 100r / min, i loko o ka hoʻouluulu kaʻina e hoʻohui i ka wai, ka wai ma ka 500 ml / min, a laila ka hui 'ana ku no 30 minuke, kaawale mai ka lalo aila papa, e wehe kiʻekiʻe chlorine haumia; ʻO ka lua, ua hoʻohaʻahaʻa ʻia ka mahana o ka hopena papa luna ma hope o ka stratification i 10, a ʻo ka hoʻoulu ʻana ʻo 100r / min no 10 mau hola. A laila, ua loaʻa pololei ke aniani paʻa ma o ka sieve plate ma ka lalo o ka reactor e ka kānana kaomi ʻana o ka nitrogen ma ke kaomi o 0.2MPa, a laila kāpī ʻia a holoi ʻia me 1Kg o 5 wai anuanu. ʻO ke kaumaha wai o 1,1, 3-trichloroacetone he 6.9kg, a ʻo ka chromatographic pure (GC) he 98.3% ma ke kaumaha [0067] ʻO ka hana i komo i kēia ʻano hoʻomaʻemaʻe, e like me ka stratification static, ka wehe ʻana i nā haumia chlorine kiʻekiʻe, crystallization , ka kānana a me ka holoi wai, hiki ke hana ʻia i loko o kahi ʻōnaehana kino paʻa, nona kahi ʻano hana aloha, a hoʻemi nui i ka hana ʻana o ka wai ʻōpala a ʻaʻole e hoʻohua i nā mea hoʻoheheʻe organik a me nā kinoea hoʻoneʻe kino [0068]. Eia kekahi, no ka mea, ʻo ke ʻano hoʻomaʻemaʻe me ka ʻole o ka hoʻokomo ʻana i ka mea hoʻoheheʻe organik, a me ka chlorine kiʻekiʻe e wehe i nā haumia i loko o ke kaʻina hoʻomaʻemaʻe, ʻaʻohe pilikia maikaʻi i ka maikaʻi o ka folic acid, a ʻo ia ka laʻana 3 hoʻomākaukau o 1, 1, 3 - cross- pili me ka acetone, ka wai e hoʻoheheʻe ʻia, hoʻohana pololei ʻia i ka hana ʻana i ka waikawa folic, hana i ka waikawa folic e hoʻomaikaʻi i ka hua holoʻokoʻa 5. 3 paona %, ka maʻemaʻe o 99. 2 paona % No ka māhele 1 [0070] hoʻomaʻemaʻe 1,1, 3- trichloroacetone e like me ke ʻano o ke ʻano 1, koe wale nō ma ka ʻanuʻu (1), ʻaʻole hoʻohana ʻia ka wai, akā, ua hoʻohana ʻia nā mea hoʻoheheʻe organik. ʻO ka hopena, ua hoʻoheheʻe ʻia ka 1,1, 3-trichloroacetone i hoʻomākaukau ʻia i ka wai a hoʻohana pololei ʻia i ka hana ʻana i ka waikawa folic. Ua hoʻonui ʻia ka huina o ka waikawa folic e 2% ma ke kaumaha a ʻo ka maʻemaʻe he 95% ma ke kaupaona. Eia kekahi, ma muli o ka hoʻokomo ʻia ʻana o nā mea hoʻoheheʻe organik i kēia ʻano hoʻomaʻemaʻe, aia kahi pilikia maikaʻi i ka maikaʻi o ka waikawa folic [0071] i ka helu 2 [0072]. Hoʻomaʻemaʻe ʻia ka 1,1, 3-trichloroacetone e like me ke ʻano o ka Laʻana 1. ʻO ka ʻokoʻa ʻo ia ma ka ʻanuʻu (1), ʻo ka nui o ka wai he 50Kg, ʻo ia ka hopena o ka hoʻonui nui ʻana o ka wai ʻino a me ka emi ʻana o 1 The ua hoʻoheheʻe ʻia ka hua o 1,1, 3-trichloroacetone crystals i ka wai a hoʻohana pololei ʻia i ka hana ʻana o ka folic acid, no laila ua hoʻonui ʻia ka nui o ka waikawa folic e 5.6% ma ke kaupaona a ʻo ka maʻemaʻe he 99.6% ma ke kaupaona [0073]. ] kū'ē i ka lakio o 3 [0074]. Ua hoʻomaʻemaʻe ʻia ʻo 1,1 ma ke ʻano o ka laʻana 1, 3-trichloroacetone, ʻo ka ʻokoʻa ma ka pae (1), ʻaʻole i wehe ʻia ka heteroplastid chlorine kiʻekiʻe, ʻo ka hopena o ka hoʻomākaukau ʻana o 1,1, 3-trichloroacetone he nui. ka helu o nā pūhui chlorinated, ka maikaʻi o ka folic acid risk [0075] E like me ka laʻana ma luna nei 1-3 a ʻo ia ka hopena o ka pālākiō o 1-3: ʻo ke ʻano hoʻomaʻemaʻe e pili ana i ka hoʻokuʻu ʻana i kahi kānana kristal e hoʻoneʻe i nā hana holoi holoi chlorine kiʻekiʻe. e like me nā mea a pau akā, i loko o ka airtight nenoaiu, aloha kaiapuni hana, a me ka nui hoemi i ka incidence o ka neoneo wai,ʻaʻole e hana pau kinoea, organic solvent a me ka organic Eia kekahi, ma ka hoʻokō 'ana i ka hihia 1 ka hoomakaukau ana o 1, 1) , 3-trichloroacetone. , hoʻohui i loko o ka puke 5/6 ʻaoʻao 7 CN 109516908 A 7 wai hoʻonā, hoʻohana pololei ʻia i ka hana ʻana i ka waikawa folic, e hoʻonui i ka huina o ka waikawa folic i 5% ma ke kaupaona, ʻo 99.2% ka maʻemaʻe ma ke kaumaha ma luna; Eia kekahi, no ka mea, ʻaʻole i hoʻolauna ke ʻano hoʻomaʻemaʻe i ka solvent organik, ʻaʻohe pilikia o ka maikaʻi o ka maikaʻi o ka waikawa folic. Eia kekahi, hoʻohana ke ʻano hoʻomaʻemaʻe i ka wai e like me ka crystallization solvent, a me ka hoʻomaʻemaʻe aqueous solution o 1,1, 3-trichloroacetone i hoʻohana pololei ʻia i ka hana ʻana i ka waikawa folic, e hōʻemi ana i nā hopena ʻaoʻao.

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