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Mgbakwunye n'ichepụta na-agbanwe ụzọ na-eme nnyocha na industrialists chepụta na-arụpụta chemical ngwaọrụ izute ha kpọmkwem mkpa.In ọrụ a, anyị na-akọ mbụ ihe atụ nke a eruba reactor kpụrụ site siri ike-ala metal mpempe akwụkwọ lamination Usoro Ultrasonic Additive Manufacturing (UAM) na kpọmkwem Integrated catalytic akụkụ na-aghọta element.Ọ bụghị nanị na UAM technology imeri ọtụtụ n'ime adịghị ike ugbu a jikọtara ya na mgbakwunye, ike nke usoro nke chemical na-abawanye nke ukwuu usoro nke ike nke usoro nke chemical na-abawanye nke ukwuu. 1,4-disubstituted 1,2,3-triazole ogige e ọma synthesized na kacha site a Cu-mediated Huisgen 1,3-dipolar cycloaddition mmeghachi omume site na iji UAM chemistry set-up.Site na leveraging na pụrụ iche Njirimara nke UAM na-aga n'ihu na-agba ọsọ nhazi, ngwaọrụ na-enwe ike catalyze na-aga n'ihu na-emeghachi omume ma na-enye ezigbo oge nzaghachi.
N'ihi na ya ịrịba uru n'elu ya nnukwu counterpart, eruba kemịkalụ bụ ihe dị mkpa na-eto eto ubi na ma agụmakwụkwọ na ulo oru ntọala n'ihi ya ike dịkwuo selectivity na arụmọrụ nke chemical synthesis.This gbatịrị si mfe organic molekul formation1 ka ọgwụ ogige2,3 na eke ngwaahịa4,5,6.Ihe karịrị 50% mmeghachi omume na kemịkalụ dị mma na ụlọ ọrụ ọgwụ nwere ike irite uru site na iji nhazi nhazi na-aga n'ihu7.
N'afọ ndị na-adịbeghị anya, a na-arị elu na-arị elu na-arịwanye elu iji dochie anya ihe nkiri ma ọ bụ na-emepụta ihe dị iche iche na-emepụta ihe dị iche iche "8. Mbipụta usoro dị ka stereolitography (sl) 9,10,11, nkwụnye ego dị iche iche nke ngwaọrụ dị iche iche nke m na ubi a17, 18, 19, 19, 19, 19, 19.
N'ihi na-amụba ojiji nke eruba kemịkalụ na mma Njirimara metụtara AM, e nwere mkpa inyocha ọzọ elu usoro na-enyere ndị ọrụ na-emepụta eruba mmeghachi omume arịa na enwekwukwa chemical na analytical capabilities.These usoro kwesịrị ime ka ndị ọrụ họrọ si a nso nke ukwuu siri ike ma ọ bụ arụ ọrụ ihe ike nke na-ejizi a dịgasị iche iche nke mmeghachi omume ọnọdụ, ma na-kwado dị iche iche mmepụta si na ngwaọrụ na-ekwe ka mmepụta ụdị na nyocha ngwaọrụ.
Otu mmako n'ichepụta usoro nke nwere ikike ịzụlite omenala chemical reactors bụ Ultrasonic Additive Manufacturing (UAM) .This siri ike-ala mpempe akwụkwọ lamination Usoro na-emetụta ultrasonic oscillations ka mkpa metal foils iji sonyere ha ọnụ oyi akwa site oyi akwa na minimal nnukwu kpo oku na a elu ogo nke plastic eruba 21 , 22 , 23 .N'adịghị ka ọtụtụ ndị ọzọ na-arụ ọrụ teknụzụ, Ubried nwere ike ịbụ n'ichepụta teknụzụ AM, na-adịghị ka ọtụtụ ndị ọzọ na-arụ ọrụ teknụzụ, Ubried . situ periodic computer numerical control (CNC) egwe ọka ma ọ bụ laser machining na-akọwa net udi nke a oyi akwa nke bonded ihe 24, 25. Nke a pụtara na onye ọrụ na-adịghị ejedebeghị site na nsogbu ndị metụtara wepụ ihe fọdụrụ raw ewu ihe si obere mmiri mmiri ọwa, nke bụ mgbe ikpe na ntụ ntụ na mmiri mmiri AM Systems26,27,28.This imewe nnwere onwe na-agbatịkwa na otu ihe na-eme ka agbụ usoro nwere ike ime ka otu ihe na-eme ka a na-ahọrọ UAM. oke nke ihe nchikota n'ofè gbazee usoro pụtara na n'ibu na chemical chọrọ nke kpọmkwem ngwa nwere ike mma met.In mgbakwunye na siri ike steeti bonding, ọzọ onu zutere n'oge ultrasonic bonding bụ elu eruba nke plastic ihe na dịtụ ala okpomọkụ29,30,31,32,33.This pụrụ iche atụmatụ nke UAM nwere ike ikwado Embedding nke n'ibu / thermal ọcha n'etiti metal n'ígwé na-enweghị mebiri emebi ihe ọmụma oge na-arụ ọrụ na-eme ka ihe mmetụta site na metal n'ígwé na-enweghị mebiri emebi.U. tics.
Ọrụ ndị na-ede akwụkwọ gara aga32 gosipụtara ikike nke usoro UAM iji mepụta ihe owuwu microfluidic 3D dị mma na ikike nghọta jikọtara ọnụ. Nke a bụ ngwaọrụ nlekota naanị. Akwụkwọ a na-egosi ihe atụ mbụ nke microfluidic chemical reactor nke UAM mere;ngwaọrụ na-arụ ọrụ nke na-abụghị nanị na-enyocha kamakwa na-eme ka njikọ kemịkal na-emepụta ihe site na ihe ndị na-emepụta ihe na-emepụta ihe. Ngwa ahụ na-ejikọta ọtụtụ uru jikọtara ya na nkà na ụzụ UAM na 3D chemical ngwaọrụ n'ichepụta, dị ka: ikike iji tọghata zuru ezu 3D aghụghọ kpọmkwem site na kọmputa-enyere imewe (CAD) ụdị n'ime ngwaahịa;ọtụtụ ihe na-emepụta ihe iji jikọta elu okpomọkụ conductivity na catalytic ihe;na embedding thermal sensọ ozugbo n'etiti reagent iyi maka kpọmkwem mmeghachi omume okpomọkụ nlekota na control.Togosi ọrụ nke chernobyl, a ọbá akwụkwọ nke pharmaceutically mkpa 1,4-disubstituted 1,2,3-triazole ogige e synthesized site ọla kọpa-catalyzed Huisgen 1,3-dipolar cyclosgen 1,3-dipolar cycloadization ihe na-emepe ohere ọhụrụ na kọmputa na-emepụta ihe na nkà mmụta sayensị. ohere maka kemistri site na nyocha multidisciplinary.
A zụtara ihe mgbaze niile na reagents n'aka Sigma-Aldrich, Alfa Aesar, TCI ma ọ bụ Fischer Scientific ma jiri ya mee ihe n'ebughị ụzọ dị ọcha. (CD3) 2SO dị ka ihe mgbaze. Emere mmeghachi omume niile site na iji Uniqsis FlowSyn flow chemistry platform.
A na-eji UAM na-emepụta ngwaọrụ niile n'ime ọmụmụ ihe a. E mepụtara nkà na ụzụ na 1999, na nkọwa nkà na ụzụ ya, ihe ndị na-arụ ọrụ na mmepe ebe ọ bụ na e nwere ike mụọ ya site na ihe ndị e bipụtara na-esonụ34,35,36,37. The Device (Figure 1) e emejuputa atumatu site na iji ihe ultra-elu ike, 9kW SonicLayer 4000s ® usoro ihe na-emepụta ihe, USA-usoro ihe eji eme ihe. 110 na Al 6061.Cu-110 nwere nnukwu ọla kọpa (opekempe 99.9% ọla kọpa), na-eme ka ọ bụrụ ezigbo onye nyocha maka mmeghachi omume ọla kọpa-catalyzed, ya mere a na-eji ya dị ka "oyi na-arụ ọrụ n'ime microreactor.A na-eji Al 6061 O dị ka ihe "oke", na-etinyekwa oyi akwa eji eme nyocha;Ngwa mgbakwunye ihe inyeaka Alloy na ọnọdụ anneal jikọtara ya na oyi akwa Cu-110.Al 6061 O bụ ihe egosipụtara na ọ dabara nke ọma na usoro UAM38, 39, 40, 41 wee nwalee wee hụ na ọ kwụsiri ike na reagents ejiri rụọ ọrụ a.Nchikota nke Al 6061 O na Cu-110 ka a na-ewerekwa dị ka ihe jikọrọ ihe maka UAM ma bụrụ ihe kwesịrị ekwesị maka ọmụmụ ihe a.38,42 Edepụtara ngwaọrụ ndị a na tebụl 1 n'okpuru.
Usoro nrụpụta ihe nrụpụta (1) Al 6061 mkpụrụ (2) imepụta ọwa ala ka edobere ka ọ bụrụ ọla kọpa (3) Ntinye nke thermocouples n'etiti ọkwa (4) Ọwa kachasị (5) Ntinye na ntinye (6) Monolithic reactor.
Nkà ihe ọmụma nke imewe nke mmiri mmiri ụzọ bụ iji a convoluted ụzọ mee ka mmiri dị anya na-ejegharị n'ime mgbawa, mgbe na-edebe mgbawa na a njikwa size. Nke a na-abawanye n'ebe dị anya na-achọsi ike na-amụba catalyst / reagent mmekọrịta oge na-enye magburu onwe ngwaahịa na-amịpụta.The ibe na-eji 90 ° ehulata na njedebe nke ụzọ kwụ ọtọ na-eme ka ọgba aghara nke 4 na-amụba n'ime oge na-amụba n'ime ngwa ngwa na kọntaktị na-amụba n'ime oge na-amụba n'ime mmiri ozuzo 4 na kọntaktị). nke nwere ike nweta, na reactor imewe atụmatụ abụọ reagent inlets jikọtara na Y-junction tupu abanye serpentine Ịgwakọta ngalaba. Nke atọ ntinye, nke intersects iyi nke ọkara site na ya obibi, gụnyere na imewe nke ga-eme n'ọdịnihu multistep mmeghachi omume syntheses.
Ọwa niile nwere profaịlụ square (enweghị akụkụ akụkụ), nsonaazụ nke igwe igwe CNC nke oge a na-eji mepụta geometry nke ọwa. A na-ahọrọ akụkụ ọwa iji hụ na mmepụta olu dị elu (maka microreactor) dị elu, ebe ọ bụ obere iji kwado mmekọrịta ihu igwe (ndị na-eme ihe ike) maka ọtụtụ mmiri mmiri dị n'ime ya. nha kwesịrị ekwesị dabere na ahụmịhe ndị ode akwụkwọ gara aga na ọwa igwe-fluidic 5 bụ ihe mmeghachi omume 7 nke ihe mejupụtara 7.5. µm na mkpokọta reactor olu bụ 1 ml. Njikọ agbakwunyere (1/4″ — 28 UNF eri) gụnyere n'ime imewe iji kwe ka ngwa ngwa kemịkalụ na-eruba na-emekọrịta ihe.Ogo nke ọwa na-ejedebe site na ọkpụrụkpụ nke ihe foil, ihe eji arụ ọrụ ya, na njikọ njikọ ejiri na ultrasonics.N'otu obosara dị iche iche maka ihe e nyere, ihe ahụ "ga-adaba" n'ime ọwa ahụ e kere eke.E nwere ugbu a ọ dịghị kpọmkwem ihe nlereanya maka nke a ngụkọta oge, otú kacha ọwa obosara maka a nyere ihe na imewe kpebisiri ike experimentally;na nke a, obosara nke 750 μm agaghị eme ka sag.
A na-ekpebi ụdị (square) nke ọwa site na iji onye na-egbu osisi square. Ụdị na nha nke ọwa nwere ike gbanwee site na igwe CNC na-eji ngwá ọrụ ịkpụ dị iche iche iji nweta ọnụego dị iche iche na njirimara dị iche iche. Ihe atụ nke ịmepụta ọwa nke na-agbagharị agbagharị na-eji 125 μm ngwá ọrụ nwere ike ịchọta ọrụ nke Monaghan45. Mgbe a na-etinye akwa mkpuchi na-edozi ahụ n'ime ihe eji eme ihe na-emepụta ihe na-emepụta ihe na-emepụta ihe na-emepụta ihe na-emepụta ihe na-emepụta ihe na-emepụta ihe n'elu ọwa nke a na-emepụta ihe na-emepụta ihe na-emepụta ihe na-emepụta ihe na-emepụta ihe na-emepụta ihe na-emepụta ihe na-emepụta ihe na-emepụta ihe na-emepụta ihe. iji nọgide na-enwe symmetry nke ọwa ahụ, a na-eji ihe ngosi square mee ihe.
N'oge a na-eme atụmatụ nkwụsịtụ n'ichepụta, thermocouple okpomọkụ nyocha (Ụdị K) na-agbanye ozugbo n'ime ngwaọrụ n'etiti otu ọwa elu na nke dị ala (Nyocha 1 - Nkeji 3) Ndị a thermocouples nwere ike nyochaa mgbanwe okpomọkụ site na -200 ruo 1350 Celsius.
A na-eme usoro ntinye nke ígwè site na mpi UAM na-eji 25.4 mm n'obosara, 150 micron nnukwu mpempe akwụkwọ.nha nke ihe nkwụnye ego buru ibu karịa ngwaahịa ikpeazụ dị ka usoro nkwụsịtụ na-emepụta ihe ntanetị ikpeazụ. A na-eji machining CNC eme ihe na-emepụta ihe na-emepụta ihe na-emepụta ihe na-emepụta ihe na-eme ka ọ bụrụ ihe na-emepụta ihe na-eme ka ọ bụrụ ihe na-emepụta ihe na-emepụta ihe na-eme ka ọ bụrụ ihe na-eme ka ultrasonic na-emepụta ihe na-eme ka ọ bụrụ ihe eji eme ihe n'oge nile nke ihe eji eme ihe na ọwa. okokụre akụkụ ga-ezute CNC imecha egwe ọka ziri ezi level.The ọwa obosara eji maka ngwaọrụ a bụ obere iji hụ na foil ihe adịghị "sag" n'ime mmiri mmiri ọwa, otú ọwa na-ekwusi a square cross-section.Possible gaps na foil ihe na UAM usoro parameters e kpebisiri ike experimentally site a n'ichepụta ibe (Fabrisonic LLC, USA).
Nnyocha egosiwo na obere mgbasa ozi elemental na-eme na UAM bonding interface 46, 47 na-enweghị ọgwụgwọ okpomọkụ ọzọ, ya mere maka ngwaọrụ ndị dị na ọrụ a, Cu-110 oyi akwa na-anọgide na-adị iche na Al 6061 oyi akwa na-agbanwe na mberede.
Wụnye pre-calibrated 250 psi (1724 kPa) back pressure regulator (BPR) na ntinye nke reactor na mgbapụta mmiri site na reactor na ọnụego nke 0.1 ka 1 mL min-1. A na-enyocha nrụgide na-arụ ọrụ site na iji FlowSyn wuru n'ime usoro nrụgide ihe mmetụta iji chọpụta na usoro ahụ nwere ike ịnọgide na-enwe nrụgide n'etiti ihe ọ bụla na-eme ka ọ bụrụ ihe na-eme ka ọ bụrụ ihe na-eme ka ọ dị iche iche na-eme ka okpomọkụ dị n'etiti ihe ọ bụla na-eme ka ọ dị iche iche. The thermocouples agbakwunyere n'ime reactor na ndị agbakwunyere n'ime FlowSyn mgbawa kpo oku efere.Nke a na-enweta site n'ịgbanwe na programmable hotplate okpomọkụ n'etiti 100 na 150 Celsius C na 25 Celsius C increments na-achọpụtakwa ihe ọ bụla dị iche n'etiti mmemme na ndekọ okpomọkụ. Nke a nwetara site na iji tc-08 data data, Cambridge, UKPccoico.
A na-emezi ọnọdụ mmeghachi omume cycloaddition nke phenylacetylene na iodoethane (Atụmatụ 1-Cycloaddition of phenylacetylene na iodoethane Scheme 1- Cycloaddition of phenylacetylene na iodoethane) .A na-emezi njikarịcha a site na nhazi zuru oke nke mmepụta ihe nke nnwale (DOE) mgbe ọ na-abịarute paramita 2 site na iji usoro mmepụta ihe na-agbanwe agbanwe nke nnwale (DOE). .
A na-akwadebe ihe ngwọta dị iche iche nke sodium azide (0.25 M, 4: 1 DMF: H2O), iodoethane (0.25 M, DMF), na phenylacetylene (0.125 M, DMF) . A 1.5 mL aliquot nke ọ bụla ngwọta na-agwakọta na pumped site reactor na ihe nlereanya eruba ọnụego na okpomọkụ nke triazole. ma kpebisie ike site na chromatography mmiri mmiri dị elu (HPLC) .N'ihi na nkwụsi ike nke nyocha, a na-enyocha mmeghachi omume niile naanị mgbe ngwakọta mmeghachi omume hapụrụ reactor. The parameter ranges ahọrọ maka njikarịcha na-egosi na Tebụl 2.
All samples e nyochara iji a Chromaster HPLC usoro (VWR, PA, USA) esịnede a quaternary mgbapụta, kọlụm oven, variable wavelength UV detector na autosampler.The kọlụm bụ ihe nhata 5 C18 (VWR, PA, USA), 4.6 × 100 mm na size, 5 µm.0 mm na size, 5 µm. ol: mmiri na ọnụego nke 1.5 mL.min-1. The injection olu bụ 5 µL na onye na-achọpụta wavelength bụ 254 nm. The% elu ebe maka DOE sample a gbakọọ site n'elu ebe nke residual alkyne na triazole ngwaahịa naanị.Injection nke mmalite ihe na-enye ohere njirimara nke dị mkpa ọnụ ọgụgụ.
Njikọta mmepụta nyocha nke reactor na software MODDE DOE (Umetrics, Malmö, Sweden) kwere ka nyocha nke ọma nke usoro nsonaazụ na mkpebi siri ike nke ọnọdụ mmeghachi omume kachasị mma maka cycloaddition a. Ịgba ọsọ na-arụ ọrụ na-arụ ọrụ na ịhọrọ usoro ihe nlereanya niile dị mkpa na-ewepụta usoro mmeghachi omume nke e mere iji mee ka ebe kachasị elu nke ngwaahịa dị elu mgbe ị na-ebelata ebe mmalite nke acety.
A na-enweta oxidation nke ọla kọpa n'elu n'ime ụlọ mmeghachi omume catalytic site na iji ngwọta nke hydrogen peroxide (36%) na-asọfe site na ọnụ ụlọ mmeghachi omume (ọnụego ntinye = 0.4 mL min-1, oge obibi = 2.5 min) tupu njikọ nke ọbá akwụkwọ triazole ọ bụla.
Ozugbo achọpụtara ọnọdụ kachasị mma, a na-etinye ha n'ụdị acetylene na haloalkane dị iche iche iji kwe ka nchịkọta nke obere ụlọ akwụkwọ ọbá akwụkwọ, si otú a na-eme ka ikike itinye ọnọdụ ndị a n'ọtụtụ dịgasị iche iche nke reagents (Nyocha 1).2).
Kwadebe ngwọta dị iche iche nke sodium azide (0.25 M, 4: 1 DMF: H2O), haloalkanes (0.25 M, DMF) na alkynes (0.125 M, DMF) .3 mL aliquots nke ọ bụla ngwọta e gwakọtara na pumped site reactor na 75 µL.min-1 na 150 ° C na-anakọta na mkpokọta nke viyl 1. acetate. A na-eji mmiri 3 × 10 mL sachaa ihe nlele ahụ. A na-ejikọta akwa mmiri na-ekpo ọkụ ma wepụ ya na 10 ml nke ethyl acetate;Mgbe ahụ, a na-ejikọta akwa akwa organic, na-asa ya na 3 x 10 mL nke brine, nke a mịrị amị n'elu MgSO4 ma kpochaa, mgbe ahụ, a na-ewepụ ihe mgbaze na vacuo. A na-ehichapụ ihe nlele ahụ site na kọlụm chromatography na silica gel site na iji ethyl acetate tupu nyocha site na nchikota HPLC, 1H NMR, 13C NMR na nnukwu mkpebi HR-MS.
Enwetara ụdịdị ụdịdị niile site na iji Thermofischer precision Orbitrap mkpebi mass spectrometer nwere ESI dị ka isi iyi ionization. A na-eji acetonitrile kwadebere ihe nlele niile dịka ihe mgbaze.
A na-eme nyocha TLC na efere silica na-akwado aluminom. A na-ahụta efere site na ìhè UV (254 nm) ma ọ bụ vanillin ntụpọ na kpo oku.
A na-enyocha ihe nlele niile site na iji usoro VWR Chromaster (VWR International Ltd., Leighton Buzzard, UK) nke nwere autosampler, kọlụm oven oven binary pump and one wavelength detector.The kọlụm eji bụ ACE Equivalence 5 C18 (150 × 4.6 mm, Advanced Chromatography Technologies Ltd., Aberdeen, Scotland).
Injections (5 µL) e mere kpọmkwem site diluted crude mmeghachi omume ngwakọta (1:10 dilution) na nyochaa na mmiri: methanol (50:50 ma ọ bụ 70:30), ma e wezụga n'ihi na ụfọdụ samples iji 70:30 ihe mgbaze usoro (pụtara dị ka kpakpando nọmba) na eruba ọnụego nke 1.5 mL / min. The kọlụm na-4 n'igosi 2.5 mL / min.
A na-agbakọ mpaghara % kacha elu nke ihe nlele ahụ site na mpaghara kacha elu nke alkyne fọdụrụnụ, naanị ngwaahịa triazole, yana ntụtụ nke ihe mmalite nyere ohere ka amata ọnụ ọgụgụ dị mkpa.
A na-enyocha ihe nlele niile site na iji Thermo iCAP 6000 ICP-OES. A na-akwado ụkpụrụ nhazi niile site na iji 1000 ppm Cu ọkọlọtọ ngwọta na 2% nitric acid (SPEX Certi Prep) .A na-akwado ụkpụrụ niile na 5% DMF na 2% HNO3 ngwọta, na ihe nlele niile na-agbaze 200.
UAM na-eji ultrasonic metal ịgbado ọkụ dị ka a bonding Usoro maka metal foil ihe eji wuo ikpeazụ mgbakọ.Ultrasonic metal ịgbado ọkụ utilizes a vibrating metal ngwá ọrụ (a na-akpọ mpi ma ọ bụ ultrasonic mpi) itinye nrụgide na foil oyi akwa / mbụ consolidated oyi akwa na-boiled mgbe ịma jijiji material.N'ihi na-aga n'ihu na-arụ ọrụ, na sonotrode vibring elu na cylin n'elu ihe na-etinyere bonding n'elu. , oxides dị n'elu ihe nwere ike ịgbawa. Ịga n'ihu na nrụgide na ịma jijiji nwere ike ime ka asperities nke ihe ahụ daa 36. Mmekọrịta mmekọrịta chiri anya na okpomọkụ na nrụgide nke mpaghara na-eduga mgbe ahụ na-eduga n'inwe njikọ siri ike na steeti ihe;ọ nwekwara ike inye aka adhesion site mgbanwe na elu energy48.The ọdịdị nke bonding usoro merie ọtụtụ n'ime nsogbu ndị metụtara na agbanwe agbaze okpomọkụ na elu okpomọkụ mgbe-mmetụta kwuru na ndị ọzọ mmako n'ichepụta techniques.This na-enye ohere maka kpọmkwem bonding (ie, na-enweghị elu mgbanwe, fillers ma ọ bụ adhesives) nke otutu n'ígwé nke dị iche iche ihe n'ime otu consolidated Ọdịdị.
A abụọ mma ihe maka UAM bụ elu ogo nke plastic eruba hụrụ na dara ihe, ọbụna na ala okpomọkụ, ie ọma n'okpuru agbaze ebe nke dara material.The Nchikota ultrasonic oscillation na nrụgide induces elu etoju nke obodo ọka ókè Mbugharị na recrystallization na-enweghị nnukwu okpomọkụ na-abawanye omenala jikọtara na nnukwu material.N'oge na-ewu nke ikpeazụ mgbakọ, nke a na-arụsi ọrụ ike oyi akwa nwere ike gafere n'etiti nke ikpeazụ nzukọ, nke a nwere ike na-arụ ọrụ oyi akwa n'etiti phenomenon. Site Layer.Elements dị ka ngwa anya emep uta eri 49, reinforcements 46, electronics 50, na thermocouples (ọrụ a) niile e ọma agbakwunyere n'ime UAM Ọdịdị ike na-arụsi ọrụ ike na-agafe agafe composite mgbakọ.
N'ime ọrụ a, ejirila ma ihe jikọrọ ihe dị iche iche yana ohere ịmekọrịta nke UAM iji mepụta microreactor na-ahụ maka ọnọdụ okpomọkụ kacha mma.
E jiri ya tụnyere palladium (Pd) na ihe ndị ọzọ na-emepụta ígwè na-ejikarị eme ihe, Cu catalysis nwere ọtụtụ uru: (i) N'ụzọ akụ na ụba, Cu dị ọnụ ala karịa ọtụtụ ọla ndị ọzọ a na-eji na-eme ihe na-eme ka ọ bụrụ ihe na-adọrọ adọrọ maka ụlọ ọrụ nhazi kemịkalụ (ii) The nso nke Cu-catalyzed cross-coupling reactions na-abawanye ma na-egosi na ọ bụ ihe na-akwado Pd53-based. nke ọma na enweghị njikọ ndị ọzọ, Njikọ ndị a na-adịkarị mfe ma dị ọnụ ala ma ọ bụrụ na achọrọ ya, ebe ndị a na-eji na Pd chemistry na-emekarị mgbagwoju anya, dị oke ọnụ, na ikuku-sensitive (iv) Cu, karịsịa mara maka ikike ya iji jikọta alkynes na nhazi, Dịka ọmụmaatụ, Sonogashira bimetallic-catalyzed Sonogashira njikọ na amistryuclidition nwekwara ike na-akwalite na chemistry. nke ọtụtụ nucleophiles na mmeghachi omume ụdị Ullmann.
Ihe atụ nke heterogenization nke mmeghachi omume ndị a niile ka egosipụtara n'oge na-adịbeghị anya n'ihu Cu (0) .Nke a bụ n'ụzọ dị ukwuu n'ihi ụlọ ọrụ na-emepụta ọgwụ na mmụba na-elekwasị anya na mgbake metal catalyst mgbake na reuse55,56.
Onye ọsụ ụzọ Huisgen na 1960s57, mmeghachi omume 1,3-dipolar cycloaddition dị n'etiti acetylene na azide na 1,2,3-triazole a na-ewere ya dị ka mmeghachi omume synergistic.
Mmeghachi omume a bịara na-elekwasị anya ọzọ mgbe Sharpless na ndị ọzọ webatara echiche nke "click chemistry" 59. A na-eji okwu ahụ bụ "click chemistry" mee ihe iji kọwaa ihe siri ike, nke a pụrụ ịdabere na ya na nhọrọ nke mmeghachi omume maka ngwa ngwa ngwa ngwa nke ogige ọhụrụ na ụlọ akwụkwọ combinatorial site na heteroatom linkage (CXC) 60 The synthetic mkpesa nke ndị a mmeghachi omume dị mfe na-emepụta oxygen, mmeghachi omume dị elu nke ọnọdụ ndị a na-eme ka ikuku oxygen na-esi na ya pụta. 1.
The oge gboo Huisgen 1,3-dipole cycloaddition esoghị na udi nke "click chemistry" Otú ọ dị, Medal na Sharpless gosiri na nke a azide-alkyne njikọ ihe omume na-enweta 107 ka 108 na ọnụnọ nke Cu (I) tụnyere uncatalyzed 1,3-dipolar 6 usoro mmeghachi omume cycloadle3 adịghị mkpa. ma ọ bụ ọnọdụ mmeghachi omume siri ike ma na-amịpụta nso ntughari zuru oke na nhọrọ na 1,4-mgbanwe 1,2,3-triazoles (anti- 1,2,3-triazole) n'ogo oge (Nyocha 3).
Nsonaazụ nke isometric nke omenala na ọla kọpa-catalyzed Huisgen cycloadditions.Cu (I) -catalyzed Huisgen cycloadditions na-enye naanị 1,4-disubstituted 1,2,3-triazoles, ebe Huisgen cycloadditions na-ekpo ọkụ na-emepụta 1,4- na 1,5-triazoles 1,5-triazoles.
Ọtụtụ usoro iwu gụnyere mbelata isi mmalite Cu (II), dị ka mbelata CuSO4 ma ọ bụ Cu (II)/Cu(0) ụdị njikọ na sodium salts. Tụnyere mmeghachi omume metal-catalyzed ndị ọzọ, ojiji nke Cu (I) nwere uru bụ isi nke ịbụ ọnụ ala ma dị mfe ijikwa.
Kinetic na isotopic labeling ọmụmụ nke Worrell et al.65 gosiri na, n'ihe banyere ọnụ alkynes, abụọ nhata ọla kọpa na-etinye aka na ịgbalite reactivity nke molekul ọ bụla kwupụta azide. Usoro a tụrụ aro na-enweta site na mgbanaka ọla kọpa nke nwere isii nke kpụrụ site na nhazi nke azide na σ-bonded ọla kọpa acetylide na π-bonded ọla kọpa dị ka a kwụsiri ike Donor ligazom. proton ire ere iji nye ngwaahịa triazole ma mechie okirikiri catalytic.
Ezie na uru nke eruba kemịkalụ ngwaọrụ na-ọma akwụkwọ, e nwere a ọchịchọ iwekota analytical ngwaọrụ n'ime ndị a usoro maka in-line, na-n'ọnọdụ, usoro monitoring66,67.UAM gosiri na-a dabara adaba usoro maka emebe na-amị ukwuu mgbagwoju 3D eruba reactors mere nke catalytically arụ ọrụ, thermally conductive ihe na ozugbo agbakwunyere sensing ọcha 4 (Fig).
Aluminom-ọla kọpa eruba reactor ekepụtara site ultrasonic mgbakwunye n'ichepụta (UAM) na mgbagwoju esịtidem ọwa Ọdịdị, agbakwunyere thermocouples na catalytic mmeghachi omume chamber.Iji anya n'ime ime mmiri ụzọ ụzọ, a transperent prototype ekepụtara site na iji stereolithography na-egosikwa.
Iji hụ na a na-emepụta reactors maka mmeghachi omume organic n'ọdịnihu, ihe mgbaze kwesịrị ikpo ọkụ n'enweghị ihe ọ bụla n'elu ebe esi mmiri;ha bụ nrụgide na okpomọkụ a nwalere. Nnwale nrụgide ahụ gosipụtara na usoro ahụ na-ejigide nrụgide siri ike ma na-adịgide adịgide ọbụna na-eme ka usoro nrụgide na-arịwanye elu (1.7 MPa) . A na-eme nyocha nke hydrostatic na ụlọ okpomọkụ na-eji H2O dị ka mmiri mmiri.
Ijikọ agbakwunyere (Figure 1) thermocouple na data data okpomọkụ gosiri na thermocouple bụ 6 Celsius C (± 1 Celsius C) jụrụ oyi karịa mmemme okpomọkụ na usoro FlowSyn. A na-ahụkarị, mmụba nke 10 Celsius C na-arụpụta okpukpu abụọ nke mmeghachi omume mmeghachi omume, ya mere, ọdịiche okpomọkụ dị iche iche nke dị ole na ole degrees nwere ike ime mgbanwe dị iche iche nke mmeghachi omume na-eme ka okpomọkụ dị elu na-agbanwe n'oge okpomọkụ. usivity nke ihe eji eme ihe na mmepụta usoro.This thermal drift bụ na-agbanwe agbanwe na ike ya mere a ga-aza maka na ngwá setup iji hụ na ezi okpomọkụ na-ruru na tụrụ n'oge reaction.Ya mere, nke a online nlekota ngwá ọrụ mmemmem uko akara nke mmeghachi omume okpomọkụ ma na-eme ka ndị ọzọ ziri ezi usoro njikarịcha na mmepe nke ezigbo ọnọdụ.These sensọ nwekwara ike-eji na-amata mmeghachi omume exotherms na-egbochi usoro runaway.
The reactor ewepụtara na ọrụ a bụ ihe atụ mbụ nke ngwa nke UAM technology na-emepụta nke chemical reactors na adreesị ọtụtụ isi adịghị ike ugbu a jikọtara AM / 3D mbipụta nke ndị a ngwaọrụ, dị ka: (i) imeri kọrọ nsogbu metụtara ọla kọpa ma ọ bụ aluminum alloy nhazi (ii) mma esịtidem ọwa mkpebi tụnyere ntụ ntụ bed fusion (PBF) usoro dị ka nhọrọ nke laser agbaze (PBF) 6 usoro dị ka nhọrọ nke laser agbaze5 (PBF) 6. duduced nhazi okpomọkụ, nke mmemmem kpọmkwem bonding nke sensọ, nke na-agaghị ekwe omume na powder bed technology, (v) merie ogbenye n'ibu Njirimara na uche nke polymer dabeere components ka a dịgasị iche iche nke nkịtị organic solvents17,19.
Usoro mmeghachi omume nke ihe omume nke Alkyned na-eme ka a na-arụ ọrụ na-aga n'ihu site na usoro na-aga n'ihu na-aga n'ihu na usoro nke 1,2,4 yl dị iche iche na sodium chloride (ọgụgụ 3) ENE NA Iodotatante) (Lee eserese 5).
(N'elu aka ekpe) Atụmatụ nhazi nke ejiri tinye 3DP reactor n'ime usoro eruba (n'elu aka nri) enwetara na atụmatụ kachasị (ala) nke atụmatụ Huisgen cycloaddition 57 n'etiti phenylacetylene na iodoethane maka njikarịcha na igosi ọnụọgụ ntụgharị nzaghachi kachasị mma.
Site n'ịchịkwa oge obibi nke reagents na catalytic akụkụ nke reactor na anya nlekota nke mmeghachi omume okpomọkụ na ozugbo Integrated thermocouple nyocha, mmeghachi omume ọnọdụ nwere ike kachasị ngwa ngwa na n'ụzọ ziri ezi na obere oge na ihe oriri.It e ngwa ngwa kpebisiri ike na ndị kasị elu ntọghata enwetara mgbe a obibi oge nke 15 nkeji na a mmeghachi omume okpomọkụ nke 150 Celsius C na-eji ma software ebe a na-ahụ ihe dị mkpa na ọnọdụ okpomọkụ. .Na-agba ọsọ na-arụ ọrụ n'ime ngwa ngwa site na iji okwu ndị a ahọpụtara na-emepụta usoro mmeghachi omume nke e mere iji mee ka ebe kachasị elu nke ngwaahịa na-ebelata ebe mmalite nke ihe onwunwe. Nkwalite a na-eme ka 53% ntụgharị nke ngwaahịa triazole, nke kwekọrọ na amụma nlereanya nke 54%.
Dabere na akwụkwọ ndị na-egosi na ọla kọpa (I) oxide (Cu2O) nwere ike na-eme dị ka ihe dị irè catalytic ụdị on efu-valent ọla kọpa na-ebupụta na ndị a mmeghachi omume, ikike nke pre-oxidize na reactor elu tupu arụpụta mmeghachi omume na eruba e nyochara70,71. The mmeghachi omume n'etiti phenylacetylene na iodoethane e wee rụrụ ọzọ n'okpuru ezigbo ọnọdụ na-mkpụrụ na-esi na-amalite na-mkpụrụ na-mkpụrụ na-atụnyere nke a na-amụba nke ọma ọnọdụ. ihe onwunwe, nke e gbakọọ na-> 99% . Otú ọ dị, nlekota nke HPLC gosiri na nke a ntughari budata belata oké ogologo mmeghachi omume oge ruo ihe dị ka 90 nkeji, ebe ọrụ pụtara larịị anya na iru a "otu ebe" .Nke a chọpụtara na-egosi na isi iyi nke catalytic ọrụ na-enweta site n'elu ọla kọpa oxide kama efu-valent ọla kọpa substrate na-Cuprotective metal n'ụzọ dị mfe oxide oyi oyi n'ime ụlọ. .Nke a na-ewepụ mkpa ịgbakwunye ihe enyemaka ọla kọpa (II) maka co-composition71.