I tetahi taha, ka whakaratohia e te hangahanga he tikanga purenga o te 1,1, 3-trichloroacetone, kei roto i te tikanga nga waahanga e whai ake nei

Kohiko:

(1) Maharahara 1,1, 3-trichloroacetone i konatunatua ki te wai;

(2) Recrystallization o te otinga o runga i muri i te tu; Me te

(3) ka tātarihia nga tioata totoka rerystallized ka horoi ki te wai;

Na, i te Hipanga (1), ko te tauwehenga o te taumaha o te 1,1, 3-trichloroacetone ki te nui o te wai he 10.1-2).

He pai ake, i te Hipanga (1), ko te tauwehenga o te taumaha o te 1,1, 3-trichloroacetone hua masivesivá ki te nui o te wai ka taea te 1:

(0.4-0.6), he mea pai ake hei 1:0.5; I roto i te tenenga, te inenga o 1,1, 3-trichloroacetone hua masivesivá me te wai te whakahaere i roto i runga ake.

Ko te awhe o te parakore teitei 1,1, 3-trichloroacetone ka taea te whiwhi.

E ai ki te hanga o naianei, i te taahiraa (1), ka taea te whakarite i te 1,1, 3-trichloroacetone hua masivesivá me te wai i te mahana o te 10-50 ℃

Whakaranuhia mo te 10-30 meneti i raro i nga tikanga, ka waiho mo te 10-30 meneti; He pai ake, i te Hipanga (1), i kii te 1,1, 3-trichloropropyl

I konatunatuahia te ketone ki te wai i te mahana o te 30-35 ℃ mo te 25-30 meneti, ka tu mo te 10-15 meneti; I roto i te tenenga o naianei

, te whakamahi i te 1,1, 3-trichloroacetone masivesivá hei rauemi mata, i roto i te hohenga tauhohenga, i konatunatua ki te wai, i whakakorikoria ki tetahi pāmahana i muri i te tu.

Te whakamaarama. I muri i te whakamaaramatanga, ka tangohia te paparanga hinu o raro, ko te nuinga ma te tango i nga poke o te maota teitei me te waiho i te otinga o runga hei whakamahi i muri mai.

E ai ki te tenenga, i te taahiraa (1), ka konatunatua te 1,1, 3-trichloroacetone ki te wai, ka taea hoki te whakakorikori.

Nga tikanga, karekau he herenga motuhake mo nga ahuatanga whakaohooho me nga taputapu, mena ka taea e te 1,1, 3-trichloroacetone te marumaru.

Ka taea te whakakotahi i te hua ki te wai. He pai ake, ko te 100-300r / min te reiti whakauru.

I roto i te tenenga o naianei, he pai ake te wai kua whakakorehia te wai.

E ai ki te tenenga, i roto i te taahiraa (2), ko nga tikanga rerystallization pea: te mahana mai i te 0 ki te 35 ℃, te wa mai i te 0.5 -

10 haora, he pai ake, ka mahia te rerystallization i te tere whakaoho o 50-300 RPM; He pai ake, ko te reknot

Ka tapirihia ano te wai i roto i te tukanga whakatioatanga, ka whakauruhia te wai i te tere o te 200-600 ml / min; I raro i enei tikanga, rerystallization tōtika

He pai nga hua.

[0034] I tua atu i te pai rawa atu, ko nga tikanga rerystallization ko: te mahana o te 10-15 ℃, te wa o te 2-3 haora, me nga tikanga rerystallization.

Ka whakaohohia te karaihe i te tere o te 100-200 RPM ka whakauruhia te wai i te tere o te 300-500 ml / min.

I raro i enei tikanga, he pai ake te painga o te whakamaarama.

I roto i te tenenga o naianei, he iti ake te whakamahana whakamaaramatanga e whakaahuatia ana i te taahiraa (2) i tera o te 1,1, 3-trichloroacetone i te taahiraa (1)

Te pāmahana i konatunatua te hua ki te wai.

E ai ki te tenenga, i te Hipanga (3), ko te ranunga tauhohenga i muri i te Hipanga (2) ka taea te tātari ma te pehanga kati, ka taea ranei

Ka whiwhi nga tioata totoka ma te pehi tika i te pereti tatari kei raro o te reactor. I roto i tenei mea hanga, he pai ake te whakamahi i te hau me te hauota/ranei

Te tātari pehanga, he pai ake te whakamahi hauota mo te tātari pehanga, a ko te pehanga ka taea te 0.1-0.2MPa, he pai ki te 0.12 -

0. 18 mpa.

E ai ki te tenenga, ka horoia te karaihe i muri i te filtration pehanga ki te wai, ka horoia taua wai.

Kaore he rohe motuhake, hei tauira, ka taea e koe te whiriwhiri i te 1-2kg o te rehu wai horoi i raro i te ahua o te pāmahana o te 2-25 ℃, me te rehu.

Karekau he rohe tere motuhake.

E ai ki te tenenga, te ma o te 1,1, 3-trichloroacetone hua masivesivá kia 50-65 % i te taimaha.

Nga wharangi 3/6 o nga tohutohu

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CN 109516908 A

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Ko te hangahanga o tenei wa, i tetahi atu taha, ka whakarato ano i te waikawa folic e mahia ana e tetahi o nga tikanga kua whakaahuahia i runga ake nei

Ko te wairewa wai o te 1,1, 3-trichloroacetone ka whakamahia tika hei whakarite i te waikawa folic.

Ko te mahi o te tikanga purenga o te tenenga, penei i te tangohanga stratified, te filtration crystallization me etahi atu, ka taea te whakahaere i roto i te punaha kati.

He pai ki te taiao, me te tino whakaiti i te whakatipuranga o te wai para, kaore he para whakarewa pararopi me te hau para pararopi; I tua atu, te tikanga purenga

Kaore he whakarewa pararopi e whakauruhia, ka tangohia nga poke o te maota nui i te wa e purea ana, na reira kaore he raru o te kounga ki te kounga o te waikawa folic.

Ko te tikanga ka whakamahia te wai hei whakarewa whakatioatanga, ka whakamahia tika te otinga wai o te 1,1, 3-trichloroacetone mo te hanga waikawa folic.

Ko te katoa o te hua o te waikawa folic ka taea te whakanui ake i te 5 % ma te taumaha, a ko te ma kei runga ake i te 99.2 % i te taumaha, ka taea te whiwhi i te kounga teitei.

O te waikawa folic.

Ko te mea hanga e whakaahuahia ana ma nga ahuatanga o raro.

[0042] I roto i nga ahuatanga me nga waahanga e whai ake nei, mena kaore i tohua, ka waatea nga taonga i whakamahia ma te hoko arumoni, mena kaore i tohua.

Ko te tikanga e whakamahia ana ko te tikanga tikanga i tenei mara.

Ko te tauira chromatography hau ko GC-2014, i hokona mai i te Kamupene Shimadzu.

Ko te 1,1, 3-trichloroacetone i mahia e te tikanga purenga o te hanga o naianei [0047] ka purea i roto i te reactor 50-rita me te pereti tatari i raro [0048] Tuatahi, ko te parakore o te 1,1 he 65 % i te taimaha , 3-trichloroacetone 20Kg me te wai 10Kg i roto i te kettle tauhohenga i konatunatua i roto i te 24 whakaoho mo te 12 meneti, te wahi i te tere whakaoho ko 200r/min, i roto i te tukanga whakaoho ki te tāpiri wai, te wai i te tere o 300 ml / min , katahi ka tu te ranunga mo te 10 meneti, ka wehea mai i te paparanga hinu o raro, tango i nga poke maota teitei; Tuarua, ka whakahekehia te pāmahana o te wairewa o runga paparanga ki te 5 ka oho mo te 2 haora i te tere whakaoho o 100r/min. Na, ka whiwhi tika te karaihe totoka i roto i te pereti tatari i raro o te ketere tauhohenga ma te filtration pehanga hauota i te pehanga 0.1 MPa, katahi ka mapuhia ka horoi ki te 2 kg wai matao. Ko te taimaha maku o 1,1, 3-trichloroacetone he 9.8 kg, me te chromatographic pure (GC) ko 96.8 wt % [0051] Ko te mahi i roto i tenei tikanga purenga, penei i te stratification pateko, te tango i nga poke o te maota teitei, te tioata, te filtration me te horoi wai, ka taea te whakahaere i roto i te punaha tinana kati, he pai ki te taiao, me te tino whakaiti i te whakatipuranga o te wai para me te kore e whakaputa i te whakarewa para pararopi me te hau para pararutiki [0052]. I tua atu, na te mea ko te tikanga purenga me te kore e whakauru i te whakarewa pararopi, me te maota nui ki te tango i nga poke i roto i te tukanga purenga, kaore he raruraru o te kounga o te waikawa folic, engari na te tauira whakatinanatanga o te whakaritenga o te 1, 1, 3 - Ko te waikawa folic e hono ana ki te wai acetone ka rewa tika ki te hanga, ka hanga te waikawa folic ki te whakapai ake i te hua katoa 5 te taumaha %, te parakore o te 99 5 te taumaha % Tauira 2 [0054] E kii ana tenei ahuatanga ko te 1,1, 3-trichloroacetone i mahia e te ko te tikanga purenga o te hanga o naianei [0055] ka purea i roto i te reactor 50-rita me te pereti tatari i raro [0056] Tuatahi, 1,1 me te parakore o 50% , 3-trichloroacetone 20Kg me te wai 4Kg whakauru. i roto i te reactor, te whakaoho mo te 15 meneti i te 45, te tere whakaoho o 300r/min, i roto i te tukanga whakaoho ki te tāpiri wai, te wai i te tere o 300 ml / min, a ka tu te ranunga mo te 15 meneti, wehea i te paparanga hinu raro, tango poke maota tiketike; Tuarua, ko te pāmahana o te otinga paparanga o runga i muri i te stratification i whakahekehia ki te 20, a ko te tere whakaoho he 200r/min mo te 0.5 haora. Na, ko te karaihe totoka i whiwhi tika mai i te pereti tatari i raro o te reactor na te filtration pehanga hauota i te pehanga 0. 2MPa. Na, ka maputia te karaihe totoka me te horoi ki te 1Kg o te 25 wai matao, me te taimaha maku o 1,1, 3-trichloroacetone ko 8.2kg na te tikanga o te whakaiti Ko te tikanga purenga e uru ana ki te tangohanga stratification pateko o nga poke o te maota teitei, ka taea te whakahaere i te whakamaaramatanga, te tātari me te horoi horoi wai i roto i te punaha tinana kati, he hoa te taiao mahi, he tino whakaiti i te whakaputanga o te wai para, kaore he para whakarewa pararopi me te hau para pararopi [0060] I tua atu, na te mea ka mahia e te tikanga. kaua e whakauru i nga whakarewa pararopi me te tango i nga poke o te maota nui i te wa o te purenga, kaore he raru o te kounga ki te kounga o te waikawa folic, a ko te 1,1, 3-trichloroacetone kua whakaritea e te Tauira 2 ka memeha ki te wai ka whakamahia tika ki te hanga o waikawa folic, te whakanui ake i te hua katoa o te waikawa folic i te 4.9% i te taumaha me te whakatutuki i te parakore o te 99 E kii ana tenei ahuatanga ko te 1,1, 3-trichloroacetone i mahia e te tikanga purenga o te tenenga o naianei [0063] kua purea i roto i te 50 -Rita reactor kua whakauruhia ki te pereti tatari i raro [0064] Tuatahi, 1,1 me te ma o 60% , 3-trichloroacetone 20Kg i konatunatua ki te wai 40Kg i roto i te kettle tauhohenga, me te whakaoho mo te 30 meneti i te 15, te tere whakaoho. o 100r / min, i roto i te tukanga whakaoho ki te tāpiri wai, te wai i te tere o te 500 ml / min, a ka tu te ranunga mo te 30 meneti, wehea i te paparanga hinu raro, tango poke maota tiketike; Tuarua, ka whakahekehia te pāmahana o te otinga paparanga o runga i muri i te stratification ki te 10, a ko te tere whakaoho he 100r/min mo te 10 haora. Na, i whiwhi tika te karaihe totoka i roto i te pereti tatari i raro o te reactor i te filtration pehanga hauota i te pehanga o 0.2MPa, katahi ka mapuhia ka horoi ki te 1Kg o te 5 wai matao. Ko te taimaha maku o 1,1, 3-trichloroacetone he 6.9kg, a ko te chromatographic pure (GC) he 98.3% te taumaha [0067] Ko te mahi i roto i tenei tikanga purenga, penei i te stratification static, te tango i nga poke o te maota teitei, te tioata , te filtration me te horoi wai, ka taea te whakahaere i roto i te punaha tinana kati, he taiao mahi hoa, me te tino whakaiti i te whakatipuranga o te wai para me te kore e whakaputa i te whakarewa pararopi para me te hau para pararutiki [0068]. I tua atu, no te mea te tikanga purenga kahore te whakauru whakarewa organic, me te māota tiketike ki te tango poke i roto i te tukanga purenga, kahore he mōrearea kounga i runga i te kounga o te waikawa folic, a ka waiho hei tauira 3 faaineineraa o 1, 1, 3 - ripeka- hono ki te acetone, te wai ki te memeha, whakamahia tika i roto i te hanga o te waikawa folic, hanga waikawa folic ki te whakapai ake te hua katoa 5. 3 taimaha %, te parakore o 99. 2 taimaha % Mo te wahanga 1 [0070] purea 1,1, 3- trichloroacetone rite ki te tikanga o te whakatinanatanga 1, haunga i te taahiraa (1), kaore i te whakamahia te wai, Engari, ka whakamahia nga whakarewa pararopi. Ko te hua o tenei, ko te 1,1, 3-trichloroacetone kua oti te whakarite, ka rewa ki te wai, ka whakamahia tika ki te hanga waikawa folic. Ko te katoa o nga hua o te waikawa folic i piki noa ma te 2% i te taumaha, a ko te maatanga he 95% i te taumaha. I tua atu, na te whakaurunga o nga whakarewa pararopi i roto i tenei tikanga purenga, he tupono te kounga ki te kounga o te waikawa folic [0071] i te wahanga 2 [0072]. Ko te 1,1, 3-trichloroacetone ka purea i runga i te tikanga o te Tauira 1. Ko te rerekee ko i te Hipanga (1), ko te nui o te wai ko te 50Kg, na te mea he nui te pikinga o te hanga wai para me te heke o te 1 The ko te hua o te 1,1, 3-trichloroacetone tioata i rewa i roto i te wai me te whakamahi tika i roto i te hanga o te waikawa folic, na ko te hua katoa o te waikawa folic i piki noa e 5.6% i te taumaha me te ma ko 99.6% te taumaha [0073] ] ki te ōwehenga o te 3 [0074]. 1,1 i purea e te tikanga o te Tauira 1, 3-trichloroacetone, ko te rereke i te taahiraa (1), kaore i tangohia te heteroplastid chlorine teitei, ko te hua o te whakaritenga o te 1,1, 3-trichloroacetone kei roto he nui. te maha o nga pūhui maota, te kounga o te mate o te waikawa folic [0075] E ai ki te tauira o runga ake nei 1-3 me te hua o te tauine o te 1-3: ko te tikanga purenga me waiho he tātari karaihe paparanga hei tango i nga mahi horoi maatai ​​teitei. pērā i te katoa engari i roto i te pūnaha rangi, te taiao mahi hoa, me te tino whakaiti i te pā o te wai para, e kore e whakaputa i te hau ururua, whakarewa organic me te organic I tua atu, na roto i te whakatinana take 1 te faaineineraa o 1, 1) , 3-trichloroacetone , tāpirihia i roto i te pukapuka 5/6 whārangi 7 CN 109516908 He wairewa wai 7, ka whakamahia tika i roto i te hanga o te waikawa folic, kia piki ake te hua katoa o te waikawa folic ki te 5 % ma te taumaha, ko te ma ko te 99.2 % te taumaha o runga; I tua atu, na te mea kaore te tikanga purenga e whakauru i te whakarewa pararopi, kaore he raru o te kounga o te waikawa folic. Ano, ko te tikanga purenga e whakamahi ana i te wai hei whakarewa whakamaaramatanga, a ko te otinga aqueous pure o 1,1, 3-trichloroacetone ka whakamahia tika i roto i te hanga o te waikawa folic, te whakaiti i nga tauhohenga taha.

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