N'otu aka ahụ, ihe mepụtara na-enye usoro nchacha nke 1,1, 3-trichloroacetone, ebe usoro ahụ nwere usoro ndị a.

Flash:

(1) Crude 1,1, 3-trichloroacetone agwakọta na mmiri;

(2) Recrystallization nke ihe ngwọta dị elu mgbe ọ kwụsịrị; Yana

(3) a na-ehichapụ kristal siri ike nke recrystallized ma jiri mmiri saa ya;

N'ime ya, na Nzọụkwụ (1), nha nha nke crude 1,1, 3-trichloroacetone kwuru na oke mmiri bụ 1.0.1-2).

Ọkacha mma, na Nzọụkwụ (1), nha nha nke ngwaahịa 1,1, 3-trichloroacetone crude na oke mmiri nwere ike ịbụ 1:

(0.4-0.6), emeziwanye ka 1: 0.5; N'ime ihe mepụtara, a na-achịkwa usoro 1,1, 3-trichloroacetone crude ngwaahịa na mmiri na nke dị n'elu.

Enwere ike nweta oke ịdị ọcha dị elu 1,1, 3-trichloroacetone.

Dị ka ihe dị ugbu a mepụtara, na nzọụkwụ (1), 1,1, 3-trichloroacetone crude ngwaahịa na mmiri nwere ike kwadebere na okpomọkụ nke 10-50 ℃.

Mix maka nkeji 10-30 n'okpuru ọnọdụ, wee hapụ 10-30 nkeji; Ọkachamma, na Nzọụkwụ (1), kwuru 1,1, 3-trichloropropyl

A gwakọtara ketone crude na mmiri na okpomọkụ nke 30-35 ℃ maka nkeji 25-30, wee guzoro maka nkeji 10-15; Na nke ugbu a mepụtara

, na-eji 1,1, 3-trichloroacetone crude dị ka akụrụngwa, na kettle mmeghachi omume, agwakọta na mmiri, kpaliri na ụfọdụ okpomọkụ mgbe guzosiri ike.

Delamination. Mgbe delamination gasịrị, a na-ewepụ oyi akwa mmanụ dị ala, tumadi site na iwepu adịghị ọcha chlorine dị elu ma hapụ ihe ngwọta dị elu maka ojiji emechaa.

Dị ka ihe mepụtara si kwuo, na nzọụkwụ (1), a na-agwakọta crude 1,1, 3-trichloroacetone na mmiri ma nwee ike ịkpali ya.

Ọnọdụ, nke enweghị mmachi akọwapụtara na ọnọdụ mkpali na akụrụngwa, ọ bụrụhaala na 1,1, 3-trichloroacetone nwere ike ịdị oke njọ.

Enwere ike ịgwakọta ngwaahịa ahụ na mmiri nke ọma. Ọkacha mma, ọnụego ngwakọta bụ 100-300r / min.

N'ime ihe a na-emepụta ugbu a, mmiri na-akacha mma bụ mmiri deionized.

Dị ka ihe mepụtara, na nzọụkwụ (2), na recrystallization ọnọdụ nwere ike ịbụ: okpomọkụ si 0 ka 35 ℃, oge si 0,5 -

10 awa, ọkacha mma, a na-eme recrystallization na ọnụego mkpali nke 50-300 RPM; Ọkacha mma, reknot

A na-agbakwunye mmiri na usoro kristal, ebe a na-agbakwunye mmiri na ọnụego 200-600 ml / min; N'okpuru ọnọdụ ndị a, arụmọrụ recrystalization

Mkpụrụ dị mma.

[0034] Ọzọkwa kacha mma, ọnọdụ recrystallization bụ: okpomọkụ nke 10-15 ℃, oge nke 2-3 awa, na ọnọdụ recrystallization.

A na-akpali kristal na ọnụego 100-200 RPM na mmiri na-agbakwunye na ọnụego 300-500 ml / min.

N'okpuru ọnọdụ ndị a, mmetụta recrystallization ka mma.

N'ime mmepụta ihe ugbu a, okpomọkụ recrystallization akọwara na nzọụkwụ (2) dị ala karịa nke 1,1, 3-trichloroacetone na nzọụkwụ (1)

Ọnọdụ okpomọkụ nke ngwaahịa a na-agwakọta na mmiri.

Dị ka ihe mepụtara si kwuo, na Nzọụkwụ (3), ngwakọta mmeghachi omume mgbe nzọụkwụ (2) gachara nwere ike ịchachaa site na nrụgide mechiri emechi, ma ọ bụ nwere ike

A na-enweta kristal siri ike site na ịpị ozugbo site na efere sieve na ala nke reactor. N'ime mmepụta ihe ugbu a, ikuku na/ma ọ bụ nitrogen na-akacha mma iji

Nrụgide nrụgide, ọ ka mma iji nitrogen maka nzacha nrụgide, na nrụgide nwere ike ịbụ 0.1-0.2MPa, ọkachamma 0.12 -

0.18 mpa.

Dị ka ihe ọhụrụ ahụ si kwuo, a na-asacha kristal a na-agbapụta mgbe a rụchara nrụgide na mmiri, ebe a na-asacha mmiri ahụ kwuru.

Enweghị oke a kapịrị ọnụ, dịka ọmụmaatụ, ị nwere ike ịhọrọ 1-2kg mmiri ịsa mmiri n'okpuru ọnọdụ okpomọkụ nke 2-25 ℃, na ịgba.

Enweghị oke oke ọsọ.

Dị ka ihe mepụtara si kwuo, ịdị ọcha nke ngwaahịa crude 1,1, 3-trichloroacetone nwere ike ịbụ 50-65% site na ibu.

Peeji nke 3/6 nke ntụziaka

5

CN 109516908 A

5

N'aka nke ọzọ, ihe mepụtara ugbu a, na-enyekwa folic acid nke a kwadebere site na ụzọ ọ bụla akọwara n'elu

A na-eji ngwọta mmiri nke 1,1, 3-trichloroacetone eme ihe ozugbo iji kwadebe folic acid.

Arụ ọrụ nke usoro nchacha nke ihe mepụtara, dị ka stratified mmịpụta, crystallization filtration na na, nwere ike rụrụ na a mechiri emechi usoro.

Environment-enyi na enyi, na-ebelata nke ukwuu ọgbọ nke mmiri mkpofu, ọ dịghị n'efu organic solvents na organic mkpofu gas; Na mgbakwunye, usoro nchacha

A naghị ewebata ihe mgbaze organic, a na-ewepụkwa adịghị ọcha chlorine dị elu n'oge a na-eme ka ọ dị ọcha, yabụ enweghị ihe egwu dị mma maka ogo folic acid.

Usoro a na-eji mmiri dị ka ihe mgbaze kristal, na ngwọta mmiri dị ọcha nke 1,1, 3-trichloroacetone na-eji ya eme ihe maka mmepụta folic acid.

Mkpokọta mkpụrụ nke folic acid nwere ike ịbawanye site na 5% n'ịdị arọ, ịdị ọcha dị elu karịa 99.2% site na ibu, nke nwere ike nweta ogo dị elu.

Nke folic acid.

A na-akọwapụta ihe mepụtara n'ụzọ zuru ezu site n'ụdị n'okpuru.

[0042] N'ime usoro na oke ndị a, ọ gwụla ma akọwapụtara n'ụzọ ọzọ, ihe eji eme ihe dị site na ịzụrụ ahịa, ọ gwụla ma akọwapụtara ya.

Usoro a na-eji bụ usoro a na-emekarị na mpaghara a.

Ụdị chromatography gas bụ GC-2014, nke a zụtara n'aka Shimadzu Company.

A na-asachapụ 1,1, 3-trichloroacetone site na usoro nchacha nke ihe a na-emepụta ugbu a [0047] na reactor 50-lita nke nwere efere sieve na ala [0048] Nke mbụ, ịdị ọcha nke 1,1 bụ 65. % n'ịdị arọ, 3-trichloroacetone 20Kg na mmiri 10Kg na kettle mmeghachi omume agwakọta na 24 na-akpali akpali maka 12 nkeji, ebe ọnụ ọgụgụ na-akpali akpali bụ 200r / min, na-akpali akpali iji tinye mmiri, mmiri na a ọnụego 300 ml / min. , mgbe ahụ ngwakọta ahụ guzoro maka nkeji 10, kewapụrụ ya na oyi akwa mmanụ ala, wepụ akwa chlorine adịghị ọcha; Nke abuo, a na-ebelata okpomọkụ nke ngwọta elu nke oyi akwa na 5 ma mee ka awa 2 mee ihe na-akpali akpali nke 100r / min. Mgbe ahụ, a na-enweta kristal siri ike ozugbo site na efere sieve dị na ala nke kettle mmeghachi omume site na nzacha nrụgide nitrogen na nrụgide nke 0.1 MPa, wee fesa ya na mmiri oyi 2 n'arọ. Mmiri mmiri nke 1,1, 3-trichloroacetone bụ 9.8 kg, na chromatographic dị ọcha (GC) bụ 96.8 wt % [0051] Ọrụ a gụnyere na usoro nchacha a, dị ka static stratification, mwepụ nke nnukwu chlorine adịghị ọcha, crystallization, filtration na mmiri ịsacha, nwere ike rụrụ na a mechiri emechi ahụ usoro, nke na gburugburu ebe obibi enyi na enyi, na-ebelata nke ukwuu ọgbọ nke mmiri mkpofu na-adịghị emepụta n'efu organic mgbaze na organic mkpofu gas [0052]. Tụkwasị na nke ahụ, n'ihi na usoro nchacha na-enweghị iwebata ihe mgbaze organic, na chlorine dị elu iji wepụ ihe ndị na-adịghị ọcha na usoro nchacha, ọ dịghị ihe ize ndụ dị mma na àgwà folic acid, kamakwa site na ihe atụ mmejuputa nke nkwadebe nke 1, 1, 3 - folic acid cross-linked na acetone mmiri etisasịwo ozugbo eji na mmepụta, na-eme folic acid imeziwanye mkpokọta mkpụrụ 5 arọ %, ịdị ọcha nke 99 5 arọ % Ihe Nlereanya 2 [0054] Nke a n'ụdị na-ekwu na 1,1, 3-trichloroacetone kwadebere site na. A na-asachapụ usoro nchacha nke ihe a na-emepụta ugbu a [0055] na reactor 50-lita nke nwere efere sieve dị na ala [0056] Mbụ, 1,1 na ịdị ọcha nke 50%, 3-trichloroacetone 20Kg na mmiri 4Kg agwakọta. na reactor, na-akpali 15 nkeji na 45, na-akpali akpali nke 300r / min, na-akpali akpali usoro iji tinye mmiri, mmiri na a ọnụego nke 300 ml / min, na mgbe ahụ, ngwakọta guzoro 15 nkeji, kewapụrụ na. ala mmanụ oyi akwa, wepụ akwa chlorine adịghị ọcha; Nke abuo, okpomọkụ nke elu oyi akwa ngwọta mgbe stratification e wedara 20, na mkpali ọnụego bụ 200r / min maka 0,5 h. Mgbe ahụ, a na-enweta kristal siri ike ozugbo site na efere sieve dị na ala nke reactor site na nzacha nrụgide nitrogen na nrụgide nke 0. 2MPa. Mgbe ahụ, a na-efesa kristal siri ike ma sachaa ya na 1Kg nke mmiri oyi 25, na ịdị arọ nke 1,1, 3-trichloroacetone bụ 8.2kg site na usoro nke mbelata Usoro nke ịdị ọcha gụnyere na static stratification mwepụ nke nnukwu chlorine adịghị ọcha, crystallization, filtration na mmiri ịsacha ọrụ nwere ike rụrụ na A mechiri emechi ahụ usoro, na-arụ ọrụ gburugburu ebe obibi enyi na enyi, na ukwuu ibelata ọgbọ nke mmiri mkpofu, ọ dịghị n'efu organic ihe mgbaze na organic mkpofu gas [0060] Na mgbakwunye, ebe ọ bụ na usoro na-eme. adịghị ewebata ihe mgbaze organic ma wepụ ihe adịghị chlorine dị elu n'oge a na-eme ka ọ dị ọcha, ọ dịghị ihe ize ndụ dị mma maka ịdị mma folic acid, na 1,1, 3-trichloroacetone nke ihe atụ 2 kwadebere na-agbaze na mmiri ma jiri ya mee ihe na mmepụta nke folic acid, na-abawanye mkpokọta folic acid site na 4.9% site n'ịdị arọ na imezu ịdị ọcha nke 99 Usoro a na-ekwu na 1,1, 3-trichloroacetone nke a kwadebere site na usoro nchacha nke ihe ọhụrụ a rụpụtara [0063] na-asachapụ na 50. -liter reactor dabara na nzacha sieve efere na ala [0064] Nke mbụ,1,1 na ịdị ọcha nke 60% , 3-trichloroacetone 20Kg gwakọtara na mmiri 40Kg n'ime kettle mmeghachi omume, na-akpali 30 nkeji na 15, na-akpali akpali ọnụego. nke 100r / min, na usoro mkpali iji tinye mmiri, mmiri na ọnụego 500 ml / min, mgbe ahụ, ngwakọta ahụ guzoro maka nkeji 30, kewapụrụ ya na akwa mmanụ ala, wepụ akwa chlorine adịghị ọcha; Nke abuo, okpomọkụ nke elu oyi akwa ngwọta mgbe stratification e wedara 10, na mkpali ọnụego bụ 100r / min maka 10 awa. Mgbe ahụ, a na-enweta kristal siri ike ozugbo site na efere sieve dị na ala nke reactor site na nzacha ikuku nitrogen na nrụgide nke 0.2MPa, wee fesaa ma saa ya na 1Kg nke 5 mmiri oyi. Ibu mmiri nke 1,1, 3-trichloroacetone bụ 6.9kg, na chromatographic dị ọcha (GC) bụ 98.3% n'ịdị arọ [0067] Ọrụ metụtara na usoro nchacha a, dị ka static stratification, mwepụ nke nnukwu chlorine adịghị ọcha, crystallization. , filtration na mmiri ịsacha, nwere ike rụrụ na a mechiri emechi ahụ usoro, nke nwere enyi na enyi na-arụ ọrụ gburugburu ebe obibi, na-ebelata nke ukwuu ọgbọ nke mmiri mkpofu na-adịghị emepụta n'efu organic mgbaze na organic mkpofu gas [0068]. Tụkwasị na nke ahụ, n'ihi na usoro nchacha na-enweghị iwebata ihe mgbaze organic, na chlorine dị elu iji wepụ ihe ndị na-adịghị ọcha na usoro nchacha, ọ dịghị ihe ize ndụ dị mma na àgwà folic acid, ọ ga-abụkwa ihe atụ 3 nkwadebe nke 1, 1, 3 - cross- ejikọrọ na acetone, mmiri igbari, kpọmkwem na-eji na mmepụta nke folic acid, na-eme ka folic acid melite mkpokọta mkpụrụ 5. 3 arọ %, ịdị ọcha nke 99. 2 arọ % N'ihi na nha 1 [0070] dị ọcha 1,1, 3- trichloroacetone dị ka usoro embodiment 1 si dị, ma e wezụga na na nzọụkwụ (1), a naghị eji mmiri eme ihe, kama nke ahụ, a na-eji ihe ndị na-emepụta ihe na-emepụta ihe. N'ihi ya, a kwadebere 1,1, 3-trichloroacetone na mmiri ma jiri ya mee ihe ozugbo na mmepụta folic acid. Mkpokọta mkpụrụ nke folic acid bụ naanị 2% ji ịdị arọ mụbaa yana ịdị ọcha bụ 95% site n'ịdị arọ. Tụkwasị na nke ahụ, n'ihi iwebata ihe ndị na-edozi ahụ na usoro nchacha a, enwere ihe ize ndụ dị mma na ogo folic acid [0071] na nha 2 [0072]. A na-eme ka 1,1, 3-trichloroacetone dị ọcha dị ka usoro dị na Ihe Nlereanya 1. Ihe dị iche bụ na na Nzọụkwụ (1), ọnụ ọgụgụ mmiri dị 50Kg, na-eme ka mmụba dị ukwuu na ọgbọ nke mmiri mkpofu na mbelata 1 The A gbazere mkpụrụ nke 1,1, 3-trichloroacetone kristal n'ime mmiri ma jiri ya mee ihe na mmepụta folic acid, nke mere na mkpokọta folic acid mụbara naanị site na 5.6% site n'ịdị arọ na ịdị ọcha bụ 99.6% n'ịdị arọ [0073] ] megidere oke nke 3 [0074]. 1,1 dị ọcha site na usoro ihe atụ 1, 3-trichloroacetone, ihe dị iche bụ na na nzọụkwụ (1), a naghị ewepụ chlorine heteroplastid dị elu, nsonaazụ nke nkwadebe nke 1,1, 3-trichloroacetone nwere nnukwu ihe. ọnụ ọgụgụ nke chlorinated ogige, àgwà nke folic acid ize ndụ [0075] Dị ka ihe atụ n'elu 1-3 na bụ n'ihi na ọnụ ọgụgụ nke 1-3: usoro ọcha na-agụnye ka guzo layered crystal filter iji wepụ akwa chlorine adịghị ọcha ọrụ ịsa. dị ka ihe niile ma na airtight usoro, enyi na enyi na-arụ ọrụ gburugburu ebe obibi, na nke ukwuu ibelata ihe omume nke mmiri mkpofu, adịghị emepụta gas efu, organic ihe mgbaze na organic Na mgbakwunye, site na mmejuputa ikpe 1 nkwadebe nke 1, 1), 3-trichloroacetone. , tinye n'akwụkwọ 5/6 page 7 CN 109516908 A 7 mmiri ngwọta, kpọmkwem eji na mmepụta nke folic acid, na-eme ka ngụkọta mkpụrụ nke folic acid mụbara 5 % site arọ, ịdị ọcha bụ 99.2 % site arọ n'elu; Ọzọkwa, n'ihi na usoro nchacha adịghị ewebata organic mgbaze, ọ dịghị mma ihe ize ndụ na àgwà nke folic acid. Ọzọkwa, usoro nchacha ahụ na-eji mmiri dị ka ihe mgbaze kristal, na ngwọta mmiri dị ọcha nke 1,1, 3-trichloroacetone na-eji ya eme ihe na mmepụta folic acid, na-ebelata mmeghachi omume n'akụkụ.

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