Ma kekahi ʻaoʻao, hāʻawi ka mea i hana ʻia i kahi ʻano hoʻomaʻemaʻe o 1,1, 3-trichloroacetone, kahi e loaʻa ai i ke ʻano nā ʻanuʻu aʻe.

ʻĀlohilohi:

(1) ʻO ka 1,1, 3-trichloroacetone maka i kāwili ʻia me ka wai;

(2) Hoʻopili hou ʻana o ka hopena o luna ma hope o ke kū ʻana; A me

(3) ua kānana ʻia nā kristal paʻa i hoʻopili hou ʻia a holoi ʻia me ka wai;

Ma laila, ma ka Pae (1), ʻo ka lakio kaumaha o ka 1,1, 3-trichloroacetone maka i ʻōlelo ʻia i ka nui o ka wai he 10.1-2).

ʻOi aku ka maikaʻi, ma ka Pae (1), ʻo ka lakio kaumaha o ka huahana maka 1,1, 3-trichloroacetone i ka nui o ka wai hiki ke 1:

(0.4-0.6), hoʻomaikaʻi hou ʻia e like me 1:0.5; I ka mea i hana ʻia, ua kāohi ʻia ka nui o ka huahana maka 1,1, 3-trichloroacetone a me ka wai ma luna.

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

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

E kāwili 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 Pae (1), ʻōlelo ʻia ʻo 1,1, 3-trichloropropyl

Ua hui ʻia ke ketone maka me ka wai ma ka mahana o 30-35 ℃ no 25-30 mau minuke, a laila kū no 10-15 mau minuke; I kēia hana hou

, me ka hoʻohana ʻana i ka 1,1, 3-trichloroacetone maka ma ke ʻano he mea maka, i loko o ka ipu hao hopena, i hui pū ʻia me ka wai, i hoʻoulu ʻia ma kahi mahana ma hope o ke kū ʻana

Delamination. Ma hope o ka delamination, wehe ʻia ka papa aila haʻahaʻa, ʻo ia hoʻi ma ka wehe ʻana i nā haumia chlorine kiʻekiʻe a waiho i ka hopena o luna no ka hoʻohana ma hope.

Wahi a ka mea i hana ʻia, ma ka hana (1), ua hui pū ʻia ka 1,1, 3-trichloroacetone maka me ka wai a hiki ke hoʻoulu ʻia.

Nā kūlana, kahi ʻaʻohe palena kikoʻī i nā kūlana hoʻoulu a me nā lako, inā hiki ke ʻāwili ʻia ka 1,1, 3-trichloroacetone

Hiki ke hoʻohui like ʻia ka huahana me ka wai. ʻOi aku ka maikaʻi o ka hoʻohuihui ʻana he 100-300r/min.

Ma kēia mea i hana ʻia, ʻoi aku ka maikaʻi o ka wai i ka wai deionized.

Wahi a ka mea i hana ʻia, ma ke kaʻina hana (2), hiki i nā kūlana recrystallization: mahana mai 0 a 35 ℃, manawa mai 0.5 -

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

Hoʻohui ʻia ka wai i ke kaʻina hana crystallization, kahi i hoʻohui ʻia ai ka wai ma ka wikiwiki o 200-600 ml/min; Ma lalo o kēia mau kūlana, ʻoi aku ka maikaʻi o ka recrystallization

Maikaʻi ka hua.

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

Hoʻoulu ʻia ke aniani ma ka wikiwiki o 100-200 RPM a hoʻohui ʻia ka wai ma ka wikiwiki o 300-500 ml/min.

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

Ma kēia mea i hana ʻia, ʻoi aku ka haʻahaʻa o ka mahana recrystallization i wehewehe ʻia ma ka pae (2) ma mua o ka 1,1, 3-trichloroacetone ma ka pae (1)

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

Wahi a ka mea i hana ʻia, ma ka Pae (3), hiki ke kānana ʻia ka hui hopena ma hope o ka Pae (2) e ke kaomi pani, a i ʻole hiki ke

Loaʻa nā kristal paʻa ma ke kaomi pololei ʻana ma o ka papa kānana ma lalo o ka reactor. Ma kēia mea i hana ʻia, ʻoi aku ka maikaʻi o ka hoʻohana ʻana i ka ea a me/a i ʻole ka naikokene

Kānana kaomi, ʻoi aku ka maikaʻi o ka hoʻohana ʻana i ka naikokene 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, ua holoi ʻia ke kristal i hoʻoheheʻe ʻia ma hope o ka kānana ʻana me ka wai, kahi i 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 wai pīpī holoi ma lalo o ke kūlana o ka mahana o 2-25 ℃, a pīpī

ʻAʻohe palena wikiwiki kikoʻī.

Wahi a ka mea i hana ʻia, ʻo ka maʻemaʻe o ka huahana maka 1,1, 3-trichloroacetone he 50-65% paha ma ke kaumaha.

ʻAoʻao 3/6 o ke aʻo ʻana

5

CN 109516908 A

5

Ma ka ʻaoʻao ʻē aʻe, hāʻawi pū ka mea i hana ʻia i kēia mea i kahi 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 i ka waikawa folic.

Hiki ke hoʻokō ʻia ka hana o ke ʻano hoʻomaʻemaʻe o ka mea i hana ʻia, e like me ka unuhi stratified, ka kānana crystallization a pēlā aku, i loko o kahi ʻōnaehana pani.

ʻOluʻolu i ke kaiapuni, a hoʻemi nui i ka hana ʻana o ka wai ʻōpala, ʻaʻohe mea hoʻoheheʻe organik a me nā kinoea ʻōpala organik; Eia kekahi, ke ʻano hoʻomaʻemaʻe

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

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

Hiki ke hoʻonui ʻia ka huina o ka waikawa folic ma 5% ma ke kaumaha, a ʻoi aku ka maʻemaʻe ma mua o 99.2% ma ke kaumaha, hiki ke loaʻa ka maikaʻi kiʻekiʻe.

ʻO ka waikawa folic.

Ua wehewehe kikoʻī ʻia ka mea i hana ʻia ma o nā hoʻokō ʻana ma lalo nei.

[0042] Ma nā hoʻokō a me nā ʻāpana ma lalo nei, ke ʻole i kuhikuhi ʻia, loaʻa nā mea i hoʻohana ʻia ma ke kūʻai ʻana i nā ʻoihana, ke ʻole i kuhikuhi ʻia

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

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

ʻO ka 1,1, 3-trichloroacetone i hoʻomākaukau ʻia e ke ʻano hoʻomaʻemaʻe o kēia mea i hana ʻia [0047] ua hoʻomaʻemaʻe ʻia i loko o kahi reactor 50-lita i lako me kahi papa kānana kānana ma lalo [0048] ʻO ka mea mua, ʻo ka maʻemaʻe o 1,1 he 65% ma ke kaumaha, 3-trichloroacetone 20Kg a me ka wai 10Kg i loko o ka ipuhao hopena i hui pū ʻia i 24 mau minuke e hoʻoulu ana no 12 mau minuke, kahi o ka wikiwiki o ka hoʻoulu ʻana he 200r/min, i ke kaʻina hana hoʻoulu e hoʻohui i ka wai, ka wai ma ka wikiwiki o 300 ml/min, a laila kū ka hui no 10 mau minuke, hoʻokaʻawale ʻia mai ka papa aila haʻahaʻa, e wehe i nā haumia chlorine kiʻekiʻe; ʻO ka lua, ua hoʻohaʻahaʻa ʻia ka mahana o ka hopena luna i 5 a hoʻoulu ʻia no 2 mau hola ma ka wikiwiki o ka hoʻoulu ʻana o 100r/min. A laila, ua loaʻa pololei ke kristal paʻa ma o ka papa kānana ma lalo o ka ipu hoʻoheheʻe hopena ma o ka kānana kaomi nitrogen ma ke kaomi o 0.1 MPa, a laila pīpī ʻia a holoi ʻia me 2 kg wai anuanu. ʻO ke kaumaha pulu 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 loko o kēia ʻano hoʻomaʻemaʻe, e like me ka stratification static, ka wehe ʻana i nā haumia chlorine kiʻekiʻe, ka crystallization, ka kānana a me ka holoi wai, hiki ke hoʻokō ʻia i loko o kahi ʻōnaehana kino pani, kahi mea aloha i ke kaiapuni, a hoʻemi nui i ka hana ʻana o ka wai ʻōpala a ʻaʻole ia e hana i ka ʻōpala organik solvent a me ke kinoea ʻōpala organik [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 hana hoʻomaʻemaʻe, ʻaʻohe pilikia maikaʻi ma ka maikaʻi o ka waikawa folic, akā ma o ka hoʻohālike hoʻokō o ka hoʻomākaukau ʻana o 1, 1, 3 - ka waikawa folic i hoʻopili ʻia me ka wai acetone i hoʻoheheʻe pololei ʻia i ka hana ʻana, e hoʻomaikaʻi ai ka waikawa folic i ka hua holoʻokoʻa 5 % kaumaha, ka maʻemaʻe o 99 5 % kaumaha Laʻana 2 [0054] Ke ʻōlelo nei kēia hoʻokō ʻana ua hoʻomaʻemaʻe ʻia ka 1,1, 3-trichloroacetone i hoʻomākaukau ʻia e ke ʻano hoʻomaʻemaʻe o kēia mea i hana ʻia [0055] i loko o kahi reactor 50-lita i lako me kahi papa kānana kānana ma lalo [0056] ʻO ka mua,1,1 me ka maʻemaʻe o 50%, 3-trichloroacetone 20Kg a me ka wai 4Kg i hui pū ʻia i loko o ka reactor, e hoʻoulu ana no 15 mau minuke ma 45, ka wikiwiki o ka hoʻoulu ʻana o 300r/min, i ke kaʻina hana hoʻoulu e hoʻohui i ka wai, ka wai ma ka wikiwiki o 300 ml/min, a laila kū ka hui ʻana no 15 mau minuke, hoʻokaʻawale ʻia mai ka papa aila haʻahaʻa, e wehe i nā haumia chlorine kiʻekiʻe; ʻO ka lua, ua hoʻohaʻahaʻa ʻia ka mahana o ka hopena o ka papa luna ma hope o ka stratification i 20, a ʻo ka nui o ka hoʻoulu ʻana he 200r/min no 0.5 h. A laila, ua loaʻa pololei ke kristal paʻa ma o ka papa sieve ma lalo o ka reactor ma o ka kānana kaomi nitrogen ma ke kaomi o 0.2MPa. A laila, ua pīpī ʻia ke kristal paʻa a holoi ʻia me 1Kg o 25 wai anuanu, a ʻo ke kaumaha pulu o 1,1, 3-trichloroacetone he 8.2kg ma ke ʻano o ka hōʻemi ʻana. Hiki ke hoʻokō ʻia ke ʻano hoʻomaʻemaʻe i komo i ka wehe ʻana o ka static stratification o nā haumia chlorine kiʻekiʻe, crystallization, kānana a me nā hana holoi wai i loko o kahi ʻōnaehana kino pani, he aloha ke kaiapuni hana, a hoʻemi nui i ka hana ʻana o ka wai ʻōpala, ʻaʻohe ʻōpala organic solvent a me ke kinoea ʻōpala organic [0060]. Eia kekahi, ʻoiai ʻaʻole hoʻokomo ke ʻano i nā solvents organik a wehe i nā haumia chlorine kiʻekiʻe i ka wā o ke kaʻina hana hoʻomaʻemaʻe, ʻaʻohe pilikia maikaʻi i ka maikaʻi o ka waikawa folic, a ua hoʻoheheʻe ʻia ka 1,1, 3-trichloroacetone i hoʻomākaukau ʻia e ka Laʻana 2 i ka wai a hoʻohana pololei ʻia i ka hana ʻana o ka waikawa folic, e hoʻonui ana i ka huina o ka waikawa folic ma 4.9% ma ke kaumaha a hoʻokō i ka maʻemaʻe o 99. Ke ʻōlelo nei kēia hoʻokō ʻana ua hoʻomaʻemaʻe ʻia ka 1,1, 3-trichloroacetone i hoʻomākaukau ʻia e ke ʻano hoʻomaʻemaʻe o kēia mea i hana ʻia [0063] i loko o kahi 50-lita. ʻO ka mea hana i hoʻolako ʻia me kahi papa kānana kānana ma lalo [0064] ʻO ka mea mua,1,1 me ka maʻemaʻe o 60%, 3-trichloroacetone 20Kg i hui pū ʻia me ka wai 40Kg i loko o ka ipuhao hopena, e hoʻoulu ana no 30 mau minuke ma 15, ʻo ka wikiwiki o ka hoʻoulu ʻana o 100r/min, i ke kaʻina hana hoʻoulu e hoʻohui i ka wai, ʻo ka wai ma ka wikiwiki o 500 ml/min, a laila kū ka hui no 30 mau minuke, hoʻokaʻawale ʻia mai ka papa aila haʻahaʻa, e 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 10, a ʻo ka wikiwiki o ka hoʻoulu ʻana he 100r/min no 10 mau hola. A laila, ua loaʻa pololei ke kristal paʻa ma o ka papa sieve ma lalo o ka mea hana ma o ka kānana kaomi nitrogen ma ke kaomi o 0.2MPa, a laila pīpī ʻia a holoi ʻia me 1Kg o 5 wai anuanu. ʻO ke kaumaha pulu 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 loko o kēia ʻano hoʻomaʻemaʻe, e like me ka stratification static, ka wehe ʻana i nā haumia chlorine kiʻekiʻe, ka crystallization, ka kānana a me ka holoi wai, hiki ke hoʻokō ʻia i loko o kahi ʻōnaehana kino pani, kahi i loaʻa kahi ʻano hana aloha, a hoʻemi nui i ka hana ʻana o ka wai ʻōpala a ʻaʻole ia e hana i ka ʻōpala organik solvent a me ke kinoea ʻōpala organik [0068]. Eia kekahi, no ka mea, ʻo ke ʻano hoʻomaʻemaʻe me ka ʻole o ka hoʻokomo ʻana i ka solvent organik, a me ka chlorine kiʻekiʻe e wehe i nā haumia i ke kaʻina hana hoʻomaʻemaʻe, ʻaʻohe pilikia maikaʻi ma ka maikaʻi o ka waikawa folic, a e laʻa me 3 ka hoʻomākaukau ʻana o 1, 1, 3 - cross-linked me ka acetone, wai e hoʻoheheʻe, hoʻohana pololei ʻia i ka hana ʻana o ka waikawa folic, e hoʻomaikaʻi ai ka waikawa folic i ka hua holoʻokoʻa 5. 3 kaumaha %, ka maʻemaʻe o 99. 2 kaumaha % No ka hapa 1 [0070] i hoʻomaʻemaʻe ʻia 1,1, 3-trichloroacetone e like me ke ʻano o ka embodiment 1, koe wale nō ma ka hana (1), ʻaʻole i hoʻohana ʻia ka wai, Akā, ua hoʻohana ʻia nā solvent organik. ʻO ka hopena, ua hoʻoheheʻe ʻia ka 1,1, 3-trichloroacetone i hoʻomākaukau ʻia i loko o ka wai a hoʻohana pololei ʻia i ka hana ʻana o ka waikawa folic. Ua hoʻonui wale ʻia ka huina o ka waikawa folic e 2% ma ke kaumaha a ʻo ka maʻemaʻe he 95% ma ke kaumaha. 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] ma ka like 2 [0072]. Hoʻomaʻemaʻe ʻia ka 1,1, 3-trichloroacetone e like me ke ʻano ma ka Laʻana 1. ʻO ka ʻokoʻa, ma ka Pae (1), ʻo ka nui o ka wai he 50Kg, e hopena ana i ka hoʻonui nui ʻana o ka hana ʻana o ka wai hoʻoneoneo a me ka emi ʻana o 1 Ua hoʻoheheʻe ʻia ka hua o nā kristal 1,1, 3-trichloroacetone i loko o ka wai a hoʻohana pololei ʻia i ka hana ʻana o ka waikawa folic, no laila ua hoʻonui wale ʻia ka hua holoʻokoʻa o ka waikawa folic ma 5.6% ma ke kaumaha a ʻo ka maʻemaʻe he 99.6% ma ke kaumaha [0073] e kūʻē i ka lakio o 3 [0074]. Ua hoʻomaʻemaʻe ʻia ʻo 1,1 e ke ʻano o ka Laʻana 1, 3-trichloroacetone, ʻo ka ʻokoʻa ma ka hana (1), ʻaʻole i wehe ʻia ka heteroplastid chlorine kiʻekiʻe, ʻo ka hopena o ka hoʻomākaukau ʻana o 1,1, 3-trichloroacetone he nui ka nui o nā hui chlorinated, ʻo ke ʻano o ka pilikia o ka waikawa folic [0075] Wahi a ka laʻana ma luna 1-3 a ʻo ia ka hopena o ka pālākiō o 1-3: ʻo ke ʻano hoʻomaʻemaʻe e pili ana i ka waiho ʻana i ka kānana kristal papa e wehe i nā haumia chlorine kiʻekiʻe i nā hana holoi e like me nā mea āpau akā i loko o ka ʻōnaehana airtight, kahi hana aloha, a ua hoʻemi nui ʻia ka hanana o ka wai ʻōpala, ʻaʻole ia e hana i ka ʻōpala kinoea, ka mea hoʻoheheʻe organik a me ka organik. Eia kekahi, ma ka hoʻokō ʻana i ka hihia 1 ka hoʻomākaukau ʻana o 1, 1), 3-trichloroacetone, e hoʻohui i loko o ka puke 5/6 ʻaoʻao 7 CN 109516908 A 7 wai hoʻonā, i hoʻohana pololei ʻia i ka hana ʻana o ka waikawa folic, e hoʻonui i ka huina o ka waikawa folic 5% ma ke kaumaha, ʻo ka maʻemaʻe he 99.2% ma ke kaumaha ma luna; Eia kekahi, no ka mea, ʻaʻole hoʻokomo ke ʻano hoʻomaʻemaʻe i ka mea hoʻoheheʻe organik, ʻaʻohe pilikia maikaʻi i ka maikaʻi o ka waikawa folic. Eia kekahi, hoʻohana ke ʻano hoʻomaʻemaʻe i ka wai ma ke ʻano he mea hoʻoheheʻe crystallization, a hoʻohana pololei ʻia ka hopena wai i hoʻomaʻemaʻe ʻia o 1,1, 3-trichloroacetone i ka hana ʻana o ka waikawa folic, e hōʻemi ana i nā hopena ʻaoʻao.

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