N'otu aka, ihe mepụtara ahụ na-enye usoro nhicha nke 1,1, 3-trichloroacetone, ebe usoro ahụ gụnyere usoro ndị a

Ọkụ:

(1) Ntụ ọka 1, 1, 3-trichloroacetone agwakọtara ya na mmiri;

(2) Ịmegharị ihe ngwọta dị n'elu mgbe ọ kwụchara; Nakwa

(3) a na-asacha kristal siri ike ndị a rụgharịrị ọhụrụ ma jiri mmiri saa ha;

N'ebe a, na Nzọụkwụ (1), oke ibu nke 1, 1, 3-trichloroacetone dị nro na oke mmiri bụ 10.1-2).

Ọ kacha mma, na Nzọụkwụ (1), oke ibu nke ngwaahịa 1, 1, 3-trichloroacetone na oke mmiri nwere ike ịbụ 1:

(0.4-0.6), nke e mere ka ọ dịkwuo mma dịka 1:0.5; N'ihe mepụtara ya, a na-achịkwa usoro nke ngwaahịa 1,1, 3-trichloroacetone na mmiri n'ime ihe ndị dị n'elu.

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

Dịka ihe mepụtara ugbu a si dị, na nzọụkwụ (1), enwere ike ịkwadebe ngwaahịa 1,1, 3-trichloroacetone na mmiri na okpomọkụ nke 10-50℃

Gwakọta ya ruo nkeji iri ruo iri atọ n'ọnọdụ ahụ, wee hapụ ya ka ọ nọrọ ruo nkeji iri ruo iri atọ; Ọ ka mma, na Nzọụkwụ (1), 1, 1, 3-trichloropropyl kwuru

A gwakọtara ketone a na mmiri na okpomọkụ nke 30-35℃ maka nkeji 25-30, wee nọrọ ruo nkeji 10-15; N'ihe mepụtara a, a na-emepụta ya ugbu a.

, jiri 1, 1, 3-trichloroacetone crude dị ka ihe eji arụ ọrụ, n'ime ketulu mmeghachi omume, agwakọtara ya na mmiri, wee kpalie ya na okpomọkụ ụfọdụ mgbe ọ kwụchara

Mkpọcha. Mgbe e mechara mkpọcha, a na-ewepụ obere mmanụ dị n'okpuru ya, ọkachasị site n'iwepụ ihe ndị na-adịghị mma dị na chlorine ma hapụ mmiri dị n'elu ya ka e jiri ya mee ihe ma emechaa.

Dịka ihe mepụtara si kwuo, na nzọụkwụ (1), a na-agwakọta 1,1, 3-trichloroacetone dị nro na mmiri ma nwee ike ịkpalite ya.

Ọnọdụ, ebe enweghị mmachi kpọmkwem na ọnọdụ na akụrụngwa na-akpali akpali, ma ọ bụrụhaala na 1, 1, 3-trichloroacetone nwere ike ịdị oke njọ

A pụrụ ịgwakọta ngwaahịa a na mmiri nke ọma. Ọ kacha mma ka ọ bụrụ na a na-agwakọta ya nke ọma, ọ ga-adị mma ka ọ bụrụ 100-300r/min.

N'ihe a mepụtara ugbu a, mmiri ahụ bụ mmiri e mere ka ọ dị ọcha.

Dịka ihe mepụtara si dị, na nzọụkwụ (2), ọnọdụ imegharị ihe nwere ike ịbụ: okpomọkụ site na 0 ruo 35℃, oge site na 0.5 -

Awa iri, ọkachasị, a na-emegharịgharị ahụ na ọsọ mkpali nke 50-300 RPM; ọ kacha mma, a na-emegharị ya na knot.

A na-etinyekwa mmiri n'usoro nhazi kristal, ebe a na-agbakwunye mmiri ahụ na ọnụego nke 200-600 ml/min; N'ọnọdụ ndị a, arụmọrụ nhazigharị

Mkpụrụ osisi dị mma.

[0034] Ọzọkwa, ọnọdụ imegharị ihe bụ: okpomọkụ nke 10-15℃, oge nke awa 2-3, na ọnọdụ imegharị ihe

A na-akpali kristal ahụ na ọsọ nke 100-200 RPM, a na-agbakwụnyekwa mmiri ahụ na ọnụego nke 300-500 ml/min.

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

N'ihe mepụtara a, okpomọkụ imegharị ihe nke a kọwara na nzọụkwụ (2) dị ala karịa nke 1,1, 3-trichloroacetone na nzọụkwụ (1)

Okpomọkụ nke a na-agwakọta ngwaahịa ahụ na mmiri.

Dịka ihe mepụtara si dị, na Nzọụkwụ (3), enwere ike ịchacha ngwakọta mmeghachi omume mgbe Nzọụkwụ (2) gasịrị site na nrụgide mechiri emechi, ma ọ bụ enwere ike ịcha ya.

A na-enweta kristal siri ike site na ịpị ozugbo site na efere sieve dị n'ala nke ihe nrụpụta ahụ. N'ihe mepụtara a, a na-eji ikuku na/ma ọ bụ nitrogen eme ihe nke ọma.

Nhicha nrụgide, ọ ka mma iji nitrogen maka nzacha nrụgide, nrụgide ahụ nwekwara ike ịbụ 0.1-0.2MPa, ọkachasị 0.12 -

0. 18 mpa.

Dịka ihe mepụtara si kwuo, a na-eji mmiri saa kristal ahụ e tinyere mgbe a sachara ya n'ime mmiri, ebe a na-asa mmiri ahụ.

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

Enweghị oke ọsọ kpọmkwem.

Dịka ihe mepụtara si kwuo, ịdị ọcha nke ngwaahịa 1,1, 3-trichloroacetone dị ọcha nwere ike ịbụ pasent 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 e ji ụzọ ọ bụla akọwara n'elu kwadebe.

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

Enwere ike ime usoro nhicha nke ihe mepụtara ahụ, dị ka mwepụ nke a na-ahazi, nzacha kristal na ihe ndị ọzọ, na sistemụ mechiri emechi.

Ọ dị mma maka gburugburu ebe obibi, ma belata mmepụta nke mmiri mkpofu nke ukwuu, enweghị ihe mkpofu organic na gas mkpofu organic; Na mgbakwunye, usoro nhicha ahụ

A naghị ewepụta ihe mgbaze organic, a na-ewepụkwa ihe ndị na-adịghị mma dị na chlorine n'oge a na-eme ka ọ dị ọcha, yabụ enweghị ihe egwu dị na àgwà folic acid.

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

Oke ibu nke folic acid nwere ike ịbawanye site na 5%, ịdị ọcha ya karịrị 99.2%, nke nwere ike nweta oke mma.

Mkpụrụ nke folic acid.

A kọwara ihe mepụtara ahụ nke ọma site na iji ihe atụ ndị dị n'okpuru.

[0042] N'ụdị na nha ndị a, ọ gwụla ma akọwapụtara ya n'ụzọ ọzọ, a na-enweta ihe eji eme ihe site na nzụta azụmaahịa, belụsọ ma akọwapụtara ya n'ụzọ ọzọ.

Usoro e ji mee ihe bụ usoro nkịtị n'ọhịa a.

Ihe nlereanya gas chromatography bụ GC-2014, nke ụlọ ọrụ Shimadzu zụtara.

A na-asacha 1,1, 3-trichloroacetone nke e ji usoro nhicha nke ihe mepụtara a mee [0047] n'ime ihe na-eme ka mmiri dị lita 50 nke nwere efere nzacha n'ala [0048]. Nke mbụ, ịdị ọcha nke 1,1 bụ 65% site na ibu, 3-trichloroacetone 20Kg na mmiri 10Kg n'ime kettle mmeghachi omume nke a gwakọtara na 24 na-akpali ruo nkeji 12, ebe ọnụego mkpali ahụ bụ 200r/min, na usoro mkpali iji tinye mmiri, mmiri ahụ na ọnụego nke 300 ml /min, wee gwakọta ya ruo nkeji 10, kewapụrụ ya na oyi akwa mmanụ dị ala, wepụ ihe ndị na-adịghị ọcha chlorine dị elu; Nke abụọ, a wedara okpomọkụ nke ihe ngwọta elu dị n'elu ka ọ bụrụ 5 ma kpalie ya ruo awa 2 na ọnụego mkpali nke 100r/min. Mgbe ahụ, e nwetara kristal siri ike ozugbo site na efere sieve dị n'ala ketulu mmeghachi omume site na nzacha nrụgide nitrogen na nrụgide nke 0.1 MPa, wee fesa ma saa ya na mmiri oyi nke kilogram 2. Ibu mmiri nke 1,1, 3-trichloroacetone bụ kilogram 9.8, chromatographic pure (GC) bụkwa 96.8 wt% [0051] A pụrụ ime ọrụ dị na usoro nhicha a, dị ka nhazi static, iwepụ ihe ndị na-adịghị ọcha chlorine dị elu, kristal, nzacha na ịsa mmiri, na sistemụ ahụ mechiri emechi, nke na-adịghị emerụ gburugburu ebe obibi, ma na-ebelata mmepụta nke mmiri mkpofu nke ukwuu ma anaghị emepụta ihe mgbaze organic na gas mkpofu organic [0052]. Tinyere nke ahụ, n'ihi na usoro nhicha ahụ na-enweghị itinye ihe mgbaze organic, yana nnukwu chlorine iji wepụ ihe na-adịghị ọcha n'ime usoro nhicha ahụ, enweghị ihe egwu dị mma na ịdị mma nke folic acid, kamakwa site na ihe atụ mmejuputa nke nkwadebe nke 1, 1, 3 - folic acid cross-linked with acetone water gbazere directly used in production, na-eme ka folic acid ka mma mmepụta zuru oke 5 ibu %, ịdị ọcha nke 99 5 ibu % Ihe atụ 2 [0054] Ihe atụ a na-ekwu na a na-asacha 1, 1, 3-trichloroacetone nke usoro nhicha nke ihe mepụtara a [0055] na reactor lita 50 nke nwere efere nzacha na ala [0056] Nke mbụ, 1,1 nwere ịdị ọcha nke 50%, 3-trichloroacetone 20Kg na mmiri 4Kg agwakọtara na reactor, na-akpali maka nkeji 15 na 45, ọnụego mkpali nke 300r/min, na usoro mkpali iji tinye mmiri, mmiri ahụ na ọnụego nke 300 ml /min, wee gwakọta ya. ruo nkeji iri na ise, kewapụrụ ya na oyi akwa mmanụ dị ala, wepụ ihe ndị na-adịghị ọcha chlorine dị elu; Nke abụọ, a wedara okpomọkụ nke ihe ngwọta oyi akwa elu mgbe ekewasịrị ya ruo 20, ọnụego mkpali ahụ bụkwa 200r/min maka awa 0.5. Mgbe ahụ, e nwetara kristal siri ike ozugbo site na efere sieve dị n'ala nke ihe nrụpụta site na nzacha nrụgide nitrogen na nrụgide nke 0.2MPa. Mgbe ahụ, a fesa kristal siri ike ma jiri 1Kg nke mmiri oyi 25 saa ya, oke mmiri nke 1,1, 3-trichloroacetone dịkwa 8.2kg site na usoro mbelata. Usoro nhicha nke gụnyere iwepụ ihe ruru unyi chlorine dị elu, kristal, nzacha na ọrụ ịsa mmiri nwere ike ime na sistemụ ahụ mechiri emechi, ebe ọrụ ahụ dị mma, ma belata mmepụta nke mmiri mkpofu, enweghị ihe mkpofu organic na gas mkpofu organic [0060] Na mgbakwunye, ebe ọ bụ na usoro ahụ anaghị ewebata ihe mgbaze organic ma wepụ ihe ruru unyi chlorine dị elu n'oge usoro nhicha ahụ, enweghị ihe egwu dị mma maka ịdị mma nke folic acid, a na-agbazekwa 1,1, 3-trichloroacetone nke Ihe atụ 2 kwadebere na mmiri ma jiri ya ozugbo na mmepụta nke folic acid, na-eme ka mkpokọta mkpụrụ nke folic acid dịkwuo elu site na 4.9% site na ibu ma na-enweta ịdị ọcha nke 99 Ihe atụ a na-ekwu na a na-asacha 1,1, 3-trichloroacetone nke usoro nhicha nke ihe mepụtara ugbu a [0063] na reactor lita 50 Ejiri efere nzacha sieve dị n'ala [0064] Nke mbụ, 1,1 nke dị ọcha nke 60%, 3-trichloroacetone 20Kg agwakọtara ya na mmiri 40Kg n'ime ketulu mmeghachi omume, na-akpali ya ruo nkeji 30 na 15, ọnụego mkpali nke 100r/min, na usoro mkpali iji tinye mmiri, mmiri ahụ na ọnụego nke 500 ml /min, wee jikọta ya ruo nkeji 30, kewapụrụ ya na oyi akwa mmanụ dị ala, wepụ ihe na-adịghị ọcha chlorine dị elu; Nke abụọ, a wedara okpomọkụ nke ihe ngwọta oyi akwa elu mgbe ekewachara ya ruo 10, ọnụego mkpali ahụ bụkwa 100r/min maka awa 10. Mgbe ahụ, e nwetara kristal siri ike ozugbo site na efere sieve dị n'ala nke ihe nrụpụta site na nzacha nrụgide nitrogen na nrụgide nke 0.2MPa, wee fesa ya ma saa ya na 1Kg nke mmiri oyi 5. Ibu mmiri nke 1,1, 3-trichloroacetone bụ 6.9kg, chromatographic pure (GC) dịkwa 98.3% site na ibu [0067] Ọrụ dị na usoro nhicha a, dị ka static stratification, iwepụ ihe ndị na-adịghị ọcha chlorine dị elu, kristal, nzacha na ịsa mmiri, enwere ike ime na sistemu ahụ mechiri emechi, nke nwere gburugburu ebe ọrụ enyi na enyi, ma na-ebelata mmepụta nke mmiri mkpofu nke ukwuu ma anaghị emepụta ihe mkpofu organic na gas mkpofu organic [0068]. Tinyere nke ahụ, n'ihi na usoro nhicha ahụ na-enweghị itinye ihe mgbaze organic, yana nnukwu chlorine iji wepụ ihe na-adịghị ọcha n'ime usoro nhicha ahụ, enweghị ihe egwu dị mma na ịdị mma nke folic acid, ọ ga-abụkwa dịka ọmụmaatụ nkwadebe 3 nke 1, 1, 3 - jikọtara ya na acetone, mmiri ga-agbaze, ejiri ya ozugbo na mmepụta folic acid, na-eme ka folic acid ka mma mmepụta zuru oke 5. 3 ibu %, ịdị ọcha nke 99. 2 ibu % Maka nha 1 [0070] 1, 1, 3-trichloroacetone dị ọcha dịka usoro nke ihe atụ 1 si dị, ewezuga na nzọụkwụ (1), anaghị eji mmiri eme ihe, Kama nke ahụ, ejiri ihe mgbaze organic mee ihe. N'ihi ya, a gbazere 1, 1, 3-trichloroacetone a kwadebere na mmiri ma jiri ya ozugbo na mmepụta nke folic acid. Mkpokọta mkpụrụ nke folic acid mụbara naanị site na 2% site na ibu na ịdị ọcha bụ 95% site na ibu. Tinyere nke a, n'ihi ntinye nke ihe mgbaze organic n'ime usoro nhicha a, enwere ihe egwu dị mma maka ịdị mma nke folic acid [0071] na nha 2 [0072]. A na-asacha 1,1, 3-trichloroacetone dịka usoro dị na Ihe atụ 1 si dị. Ihe dị iche bụ na na Nzọụkwụ (1), ọnụọgụ mmiri bụ 50Kg, nke butere mmụba dị ukwuu na mmepụta nke mmiri mkpofu na mbelata nke 1. A gbazere kristal 1,1, 3-trichloroacetone na mmiri ma jiri ya ozugbo na mmepụta nke folic acid, nke mere na mkpokọta mmepụta nke folic acid mụbara naanị site na 5.6% site na ibu na ịdị ọcha bụ 99.6% site na ibu [0073] megide nha nke 3 [0074]. E mere ka 1,1 dị ọcha site na usoro nke Ihe atụ 1, 3-trichloroacetone, ihe dị iche bụ na na nzọụkwụ (1), anaghị ewepụ chlorine heteroplastid dị elu, nsonaazụ nke nkwadebe nke 1, 1, 3-trichloroacetone nwere ọtụtụ ihe mejupụtara chlorine, ịdị mma nke ihe egwu folic acid [0075] Dịka ihe atụ 1-3 dị n'elu si dị ma ọ bụ nsonaazụ nke nha nke 1-3: usoro nhicha ahụ gụnyere ịhapụ nzacha kristal a na-eji akwa iji wepụ ihe ruru unyi chlorine dị elu n'ịsa ihe dịka ihe niile ma e wezụga sistemụ ikuku na-adịghị emerụ ahụ, gburugburu ebe ọrụ enyi na enyi, ma belata oke mmiri mkpofu, anaghị emepụta gas mkpofu, ihe mgbaze organic na organic. Na mgbakwunye, site na itinye ikpe 1 n'ọrụ nkwadebe nke 1, 1), 3-trichloroacetone, tinye na akwụkwọ 5/6 peeji nke 7 CN 109516908 A 7 mmiri ngwọta, ejiri ozugbo na mmepụta nke folic acid, na-eme ka mkpokọta mkpụrụ nke folic acid mụbaa 5% site na ibu, ịdị ọcha bụ 99.2 % site na ibu dị n'elu; Ọzọkwa, n'ihi na usoro nhicha ahụ anaghị ewebata ihe mgbaze organic, enweghị ihe egwu dị mma maka ịdị mma nke folic acid. Ọzọkwa, usoro nhicha ahụ na-eji mmiri dị ka ihe mgbaze kristal, a na-ejikwa mmiri dị ọcha nke 1,1, 3-trichloroacetone ozugbo na mmepụta nke folic acid, na-ebelata mmeghachi omume ndị na-adịghị mma.

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