I-Hielscher Ultrasound Technology

I-Ultrasonically Induced and Enhanced Phase Transfer Catalysis

Amandla amakhulu e-ultrasound ayaziwa kakhulu ngegalelo lazo ekusebenzeni okuhlukahlukene kwamakhemikhali. Yilokho okuthiwa Sonochemistry. Ukusabela okungajwayelekile - kanye nokusabela kwesigaba se-phase - yizinsizakalo ezinamandla zokusebenzisa amandla we-ultrasound. Ngenxa yamandla kagesi nama-sonochemical asetshenziselwa ama-reagents, ukusabela kungase kuqalwe, ijubane lokuphendula lingakhuthukiswa kakhulu, kanye namazinga aphezulu okuguqulwa, isivuno esiphezulu, nemikhiqizo engcono ingafinyelelwa. Ukusabalalisa okulinganayo kwe-ultrasound nokutholakala kwe-ultrasonic ethembekile Izimboni imishini yenza le nqubo ibe yisisombululo esithakazelisayo sokukhiqizwa kwamakhemikhali
Glass reactor for targeted and reliable sonication processes

I-Ultrasonic Glass Cell Flow

isigaba sokudluliswa kwesigaba

Isigaba sokudlulisa i-Catalysis (i-PTC) ifomu elikhethekile le-catalysis engavamile futhi eyaziwa njengendlela yokwenza okusebenzayo yokwenziwa kwe-organic. Ngokusebenzisa i-catalyst yokudluliselwa kwesigaba, kuba lula ukuxazulula ama-reactants e-ionic, okuvame ukuqubutheka kwisigaba esineqhwa kodwa kungenasisindo kwisigaba sezinto eziphilayo. Lokhu kusho ukuthi i-PTC iyisisombululo esithile sokunqoba inkinga ye-heterogeneity ekuphenduleni lapho ukuxhumana phakathi kwezinto ezimbili ezisezigaba ezahlukene zenhlanganisela kuvinjelwe ngenxa yokungakwazi kwamagagagasi ukuhlangana ndawonye. (Esen et al., 2010) Izinzuzo ezijwayelekile zokudluliswa kwesigaba sezinyathelo ziyizinyathelo zokulungiselela, izinqubo ezilula zokuhlola, izimo zokuphendula kahle, izinga eliphezulu lokuphendula, ukukhetha okuphezulu, nokusetshenziswa kwama-reagents angabizi futhi anemvelo, njenge-quaternary ammonium usawoti, kanye nezixazululo, futhi kungenzeka ukuthi kwenziwe amalungiselelo amakhulu (Ooi et al. 2007).
Izimo ezihlukahlukene zamanzi-liquid and liquid-reaction ziye zaqina futhi zenziwe ngokukhetha ngokusebenzisa izigaba ezilula zokudlulisa (PT) ezifana nezindleko, i-polyethylene glycol-400, njll, okuvumela izinhlobo ze-ionic ukuba zinywe kusuka kwesigaba se-aqueous to isigaba eziphilayo. Ngakho-ke, izinkinga ezihlotshaniswa ne-solubility ephansi kakhulu ye-reactants eziphilayo ezingxenyeni ze-aqueous zinganqotshwa. Kulezi zimboni zezinambuzane nezidakamizwa, i-PTC isetshenziselwa kakhulu futhi ishintshe izinto eziyisisekelo zebhizinisi. (Sharma 2002)

I-Power ultrasound

Ukusetshenziswa kwamandla ultrasound kuyithuluzi eyaziwa kakhulu ukudala kahle kakhulu Emulsions. Emakhemikhali anjalo ama-emulsions amancane ajwayelekile kakhulu asetshenziselwa ukuthuthukisa ukuphendula kwamakhemikhali. Lokhu kusho ukuthi indawo yokuxhumana ephakathi kokuphakathi kwamanzi amabili noma ngaphezulu okungenakuqhathaniswa nokuphuza ikhula ngendlela ephawulekayo futhi inikeza ngaleyo ndlela inkambo engcono, ephelele futhi / noma esheshayo yokusabela.
Ukuze ukudluliselwa kwesigaba se-catalysis – okufana nokunye ukuphendula kwamakhemikhali - okwanele kinetic energy kuyadingeka ukuqala ukusabela.
Lokhu kunemiphumela emihle ephathelene nokuphendula kwamakhemikhali:

  • Ukusabela kwamakhemikhali okungavamile ukuba kwenzeke ngenxa yamandla ayo aphansi kinetic angakwazi ukuqala nge-ultrasonication.
  • Ukusabela kwamakhemikhali kungasheshiswa nge-ultrasonic-assisted PTC.
  • Qedela ukugwema ukudluliswa kwesigaba sokudlulisa.
  • Izinto eziwusizo zingasetshenziswa ngokuphumelelayo.
  • Ama-by-products angancishiswa.
  • Ukushintshwa kwesisekelo esiqinile esinobungozi obuqinile esinesizinda esingabizi esincane.

Ngezimpikiswano, i-PTC iyindlela ephawulekayo yamakhemikhali yokuhlanganisa okuphilayo okuvela ezimpikisini ezimbili nangaphezulu ezingabonakali: Ukudluliswa kwesigaba se-catalysis (i-PTC) kwenza ukuba kusetshenziswe izinto ezibonakalayo ezinqubo zamakhemikhali ngendlela ephumelelayo futhi ukukhiqiza izindleko ezingaphezulu. Ukuthuthukiswa kokusebenza kwamakhemikhali yi-PTC kuyithuluzi elibalulekile lokukhiqiza kwamakhemikhali elingathuthukiswa ngokusetshenziswa kwe-ultrasound ngokuphawulekayo.

Ultrasonic cavitation in a glass column

I-cavitation in liquid

Izibonelo zokuphendula kwe-PTC nge-ultrasonically

  • Ukuhlanganiswa kwezinto ezintsha ze-N '- (4,6-disubstituted-pyrimidin-2-yl) -N- (5-aryl-2-furoyl) izithwala ze-thiourea esebenzisa i-PEG-400 ngaphansi kwe-ultrasonication. (Ken et al. 2005)
  • Ukwenziwa kwe-ultrasonically kwe-mandelic acid nge-PTC ku-liquid ionic kubonisa ukuthuthukiswa okuphawulekayo ekuphenduleni izivuno ngaphansi kwezimo ezinzulu. (Hua et al. 2011)
  • Kubo et al. (2008) kubika ukuthi i-C-alkylation eyasiza kakhulu i-phenylacetonitrile endaweni engenawo amandla. Umphumela we-ultrasound ukugqugquzela ukusabela kuye kubangelwa indawo enkulu kakhulu yokuxhumana phakathi kwezigaba zombili zamanzi. Ukukhishwa kwe-Ultrasonication kubangela ukuphendula okusheshayo okukhulu kunokuxubana kwemishini.
  • I-Sonication ngenkathi kusabela kwe-carbon tetrachloride nge-magnesium ekwakheni i-dichlorocarbene imiphumela emvunweni ophezulu we-gem-dichlorocyclopropane phambi kwama-olefins. (Lin et al. 2003)
  • I-Ultrasound inikeza ukusheshisa kokuphendula kwe-Cannizzaro P-chlorobenzaldehyde ngaphansi kwezimo zokudluliswa kwesigaba. Ezingxenye ezintathu zezinto zokudlulisa izigaba – i-benzyltriethylammonium chloride (TEBA), i-Aliquat ne-18-crown-6 -, ehlolwe ngu-Polácková et al. (1996) TEBA itholakala ukuthi iyasebenza kakhulu. Ferrocenecarbaldehyde futhi P-dimethylaminobenzaldehyde yanikeza, ngaphansi kwezimo ezifanayo, i-1,5-diaryl-1,4-pentadien-3-eyodwa njengomkhiqizo oyinhloko.
  • Lin-Xiao et al. (1987) baye babonisa ukuthi inhlanganisela ye-ultrasonication ne-PTC ikhuthaza ngokuphumelelayo isizukulwane se-dichlorocarbene esivela ku-chloroform ngesikhathi esifushane nesitshalo esingcono kanye nesilinganiso esincane sokubamba iqhaza.
  • Yang et al. (2012) baphenyisisa ukutshala okuluhlaza okwenziwe i-benzyl 4-hydroxybenzoate e-green, ultrasonically-assisted nge-4,4'-bis (tributylammoniomethyl) -1,1'-biphenyl dichloride (i-QCl2) njenge-catalyst. Ngokusetshenziswa kwe-QCl2, baye bahlakulela i-novel-site catalysis-transfer catalytic. Le-solid-liquid phase-transfer catalysis (SLPTC) yenziwe njengenqubo ye-batch nge-ultrasonication. Ngaphansi kwe-sonication enamandla, i-33% ye-Q2 + eyengeziwe ene-45.2% we-Q (Ph (OH) COO)2 uye wadluliselwa kwisigaba esiyingozi ukuze asabele nge-benzyl bromide, ngakho-ke izinga lokuphendula ngokubanzi lenziwa ngcono. Lokhu kufinyelela izinga lokuphendula kwatholakala ku-0.106 iminithi-1 ngaphansi kwe-300W ye-ultrasonic irradiation, ngenkathi ngaphandle kokwazisa ngesilinganiso se-0.0563 iminithi-1 kwaqashelwa. Ngenxa yalokho, umphumela we-synergistic we-double-site phase-transfer catalyst ne-ultrasound ku-phase transfer catalysis uye waboniswa.
The ultrasonic lab device UP200Ht provides powerful sonication in laboratories.

Isithombe 1: I-UP200Ht i-homogenizer enamandla ye-watts engu-200

Ukuthuthukiswa kwe-ultrasonic ye-Asymmetric Phase Transfer Reaction

Ngenhloso yokwenza indlela ewusizo yokuhlanganiswa kwe-amino acids kanye ne-derivatives yabo i-Maruoka no-Ooi (2007), baphenya ngokuthi "ngabe ukusebenza kabusha kwe-N-spiro chiral quaternary ammonium usawoti kungathuthukiswa futhi izakhiwo zabo zilula. Njengoba i-ultrasonic irradiation ikhiqiza i-homogenization, okungukuthi, kuhle kakhulu Emulsions, liyakwandisa kakhulu indawo yokuxhumana lapho kungenziwa khona, okungaholela ekunciphiseni izinga lokushisa ekwenziweni kwe-liquide-liquid phase-transfer. Ngempela, ukunikezwa kwe-reaction ye-2, i-methyl iodide, kanye ne-S (S, S) -naphtyl subunit (1 mol%) ku-toluene / 50% i-KOH e-aqueous ku-0 degC yehora eli-1 yenze umkhiqizo ohambelanayo we-alkylation ngo-63% ukukhiqiza nge 88% ee; ukukhiqizwa kwamakhemikhali kanye ne-enantioselectivity kwakufaniswa nalabo abasabela ekusebenzeni okulula kokuhlanganiswa kwamahora angu-8 (0 degC, 64%, 90% ee). "(Maruoka et al. 2007;

Improved phase transfer reactions by sonication

I-Scheme 1: I-Ultrasonication ithuthukisa izinga lokuphendula ngesikhathi sokulinganisa kwe-α-amino acids [Maruoka et al. 2007]

Olunye uhlobo lokuphendulela lwe-catalysis asymmetric yi-reaction kaMichael. Ukwengeza kukaMichael we-diethyl n-acetyl-aminomalonate ukuze i-chalcone ithonywe kahle yi-ultrasonication eholela ekunyuseni kwe-12% yemvuno (kusukela ku-72% etholakalayo ngesikhathi isenzo sokuthula singena ku-82% ngaphansi kwe-ultrasonication). Isikhathi sokuphendula sikhulu ngokushesha izikhathi eziyisithupha ngaphansi kwamandla ultrasound uma kuqhathaniswa nokuphendula ngaphandle kwe-ultrasound. Ukudlulela kwe-enantiomeric (ee) akukashintshi futhi kwaba kokubili kokuphendula - ngaphandle nangaphandle kwe-ultrasound - ku-40% ee. (Mirza-Aghayan et al. 1995)
Li et al. (2003) yabonisa ukuthi ukuphendula kukaMichael ngama-chalcones njengabalamukeli abane-methylene ehlanganisiwe efana ne-diethyl malonate, i-nitromethane, i-cyclohexanone, i-ethyl acetoacetate kanye ne-acetylacetone njengabaxhasi abanjwe yi-KF / i-alumina eyisisekelo emakhulwini athengisa isivuno esikhulu ngesikhathi esifushane ngaphansi kwe-ultrasound i-irradiation. Kwesinye isifundo, Li et al. (2002) baye babonisa ukuphumelela okuhlangenwe nakho kwe-ultrasonically-okusizwa ngama-chalcones okwenziwe yi-KF-Al2O3.
Lezi zimpendulo ze-PTC ngenhla kubonisa kuphela ububanzi obuncane bokuthi kungenzeka yini kanye namathuba we-ultrasonic irradiation.
Ukuhlolwa nokuhlolwa kwe-ultrasound mayelana nokuthuthukiswa okungenzeka ku-PTC kulula kakhulu. Amadivaysi webhu ultrasonic afana ne-Hielscher UP200Ht (Ama-watts angu-200) nezinhlelo zebheke-top ezifana ne-Hielscher's I-UIP1000hd (1000 watts) vumela ukuhlolwa kokuqala. (bheka isithombe 1 no-2)
I-Ultrasonic ithuthukise ukulinganisa okungaphezulu kukaMichael (Chofoza ukuze ukhulise!)

I-Scheme 2: I-ultrasonically isiza ukulinganisa kukaMichael okungukuthi uMichael N-acetyl-aminomalonate kuya ku-chalcone [Török et al. 2001]

Ukukhiqiza okuphumelelayo kwi-Chemical Market

Ukusebenzisa ultrasonic isigaba ukudlulisa catalysis uzothola inzuzo eyodwa noma ngaphezulu izinzuzo ezihlukahlukene:

  • ukuqaliswa kokuphendula okungenakwenzeka
  • ukwanda komkhiqizo
  • ukunciphisa ama-solvents abizayo, anhydrous, aprotic
  • ukunciphisa isikhathi sokuphendula
  • ukuphendula okuphansi okushisa
  • ukulungiswa okulula
  • ukusetshenziswa kwensimbi yama-alkali enamafutha esikhundleni se-alkali metal alkoxides, i-amide sodium, i-hydride ye-sodium noma i-sodium metallic
  • ukusetshenziswa kwezinsimbi ezibizayo, ikakhulukazi izakhi
  • ukushintsha kokukhetha
  • ukuguqulwa kwezivumelwano zomkhiqizo (isb. i-alkylation ye-O- / C)
  • ukuhlukaniswa lula nokuhlanzwa
  • ukwanda komkhiqizo ngokucindezela ukuphendula okuhlangene
  • elula, elinganiselwe-kuze kufike ezingeni lokukhiqiza ezimbonini, ngisho ne-highput
UIP1000hd Bench-Top Ultrasonic Homogenizer

Ukusetha nge-1000W iprosesa ye-ultrasonic, ukugeleza kweseli, ithangi kanye nepompo

Ukuhlolwa okulula futhi okungenangcupheni ye-Ultrasonic Effects eKhemistry

Ukuze ubone ukuthi ithonya le-ultrasound lithinta kanjani izinto kanye nokuphendula, ukuhlolwa kokuqala kokufezeka kungenziwa ngezinga elincane. Amadivayisi we-laboratory abanjwe ngesandla noma amisiwe angama-watts angu-50 kuya ku-400 avumela ukunikezwa kwamasampuli amancane namaphakathi nendawo phakathi kwe-beaker. Uma imiphumela yokuqala ibonisa ukufezeka okungenzeka, inqubo ingathuthukiswa futhi ihlelwe ebhentshini phezulu ngenqubo ye-industrial ultrasonic, isib. I-UIP1000hd (1000W, 20kHz). Amasistimu we-ultrasonic bench-top systems 500 i-watts kuya 2000 ama-watts amadivayisi afaneleka ku-R&D nokusebenza kahle. Lezi zinhlelo ze-ultrasonic - zenzelwe i-beaker kanye ne-sonication encane – unike amandla ngokugcwele phezu kwepharamitha yenqubo ebaluleke kunazo zonke: Ukulinganisa, Ukucindezela, Ukushisa, Ukungazi lutho, nokuxhaswa.
Ukulawulwa okunembile phezu kwemingcele kuvumela ukuzala okuqondile kanye nokusabalalisa okulinganayo yemiphumela etholakalayo. Ngemuva kokuthi uhlole amasu ahlukahlukene, ukucushwa okutholakele ukuthi kungcono kungasetshenziswa ukuqhubeka ngokuqhubekayo (24h / 7d) ngaphansi kwezimo zokukhiqiza. I-PC-Control yokuzikhethela (isikhombimsebenzisi se-software) iphinde ihlinzekele ukurekhodwa kokuhlolwa okulindelekile. Ukuze i-sonication yeziphuzo ezivuthayo noma izixazululo ezindaweni eziyingozi (ATEX, FM) the I-UIP1000hd itholakala kwinguqulo eqinisekisiwe ye-ATEX: I-UIP1000-Exd.

Okujwayelekile ukuzuza nge-ultrasonication ekhemistry:

  • Ukusabela kungase kuphuthumise noma kunzima ukuphoqelela izimo kungadingeka uma kusetshenziswa i-sonication.
  • Izinkathi zokuxoshwa ngokuvamile ziyancishiswa kakhulu njengoba ziyizifo ezivame ukuhambisana nokuphendula okunjalo.
  • Ukuphendula kwe-sonochemical kuvame ukuqaliswa yi-ultrasound ngaphandle kwesidingo sezingxube.
  • Inani lezinyathelo ezivame ukudingwa emgwaqweni wokwenza izinto ngezinye izikhathi zingancishiswa.
  • Kwezinye izimo ukusabela kungaqondiswa kwenye indlela.

Xhumana Nathi / Cela Ukwaziswa Olwengeziwe

Khuluma nathi mayelana nezidingo zakho zokucubungula. Sizosikisela ukusetha nokulungiswa kwemingcele efanele yephrojekthi yakho.





Sicela uqaphele wethu Inqubomgomo yobumfihlo.


Izincwadi / Izinkomba

  1. Esen, Ilker et al. (2010): Ukuguqulwa Kwesigaba Esikude Sokudluliswa Kwama-Catalysts Ekuphenduleni Kwemigodi Yama-Aldehydes Aromatic Emanzini Ngaphansi Kwe-Ultrasonic Effect. I-Bulletin yaseKorea Chemical Society 31/8, 2010; iphe. 2289-2292.
  2. Hua, Q. et al. (2011): I-ultrasonically-yakhuthazwa nge-mandelic acid nge-phase transfer catalysis ku-liquid ionic. Ku: Ultrasonics Sonochemistry Vol. 18/5, 2011; iphe. 1035-1037.
  3. ULi, J.-T. et al. (2003): Ukuphendula kukaMichael kuthathwe i-KF / i-alumina eyisisekelo ngaphansi kwe-ultrasound irradiation. I-Ultrasonics Sonochemistry 10, 2003. iphe. 115-118.
  4. Lin, Haixa et al. (2003): Indlela Elula Yokukhiqiza I-Dichlorocarbene kusukela ekusebenzeni kwe-Carbon Tetrachloride ne-Magnesium esebenzisa i-Ultrasonic Irradiation. Ku: Ama-Molecule 8, 2003; iphe. 608 -613.
  5. Lin-Xiao, Xu et al. (1987): Indlela engokoqobo yenqubo yokukhiqiza i-dichlorocebene nge-ultrasonic irradiation kanye nesigaba sokudlulisa i-catalysis. Ku: Acta Chimica Sinica, Umq. 5/4, 1987; iphe. 294-298.
  6. Ken, Shao-Yong et al. (2005): Ukudluliselwa kwesigaba kuhlanganiswe ukuvuselelwa kwe-ultrasonic irradiation kanye nokusetshenziswa kwemvelo ye-N '- (4,6-disubstituted-pyrimidin-2-yl) -N- (5-aryl-2-furoyl) izidakamizwa ze-thiourea. Ku: Indian Journal of Chemistry Vol. 44B, 2005; k. 1957-1960.
  7. Kubo, Masaki et al. (2008): I-Kinetics ye-Solvent-Free C-Alkylation ye-Phenylacetonitrile esebenzisa i-Ultrasonic Irradiation. I-Chemical Engineering Journal eJapane, Umq. 41, 2008; amakhasi 1031-1036.
  8. Maruoka, Keiji et al. (2007): Izinzuzo zamuva ku-Phase-Transfer Catalysis. Ku: Angew. I-Chem. Int. Ed., Umq. 46, Wiley-VCH, Weinheim, 2007; iphe. 4222-4266.
  9. UMason, uThimothewu no-al. (2002): Ukusetshenziswa kwe-sonochemistry: ukusetshenziswa kwamandla ultrasound ekhemistry nokucutshungulwa. Wiley-VCH, Weinheim, 2002.
  10. UMirza-Aghayan, M. et al (1995): I-Ultrasound Irradiation Effects kwi-Asymmetric Michael Reaction. I-tetrahedron: i-Asymmetry 6/11, 1995; iphe. 2643-2646.
  11. Polácková, Viera et al. (1996): Ukusabela kwe-Cannizzaro okukhuthazwa yi-ultrasound ngaphansi kwezimo zokudlulisa isigaba. Ku: Ultrasonics Sonochemistry Vol. 3/1, 1996; k. 15-17.
  12. Sharma, MM (2002): Amasu okuqhuba ukuphendula ngesilinganiso esincane. Ubunjiniyela bokukhetha kanye nenqubo yokuqinisa. Ku: Ama-Chemistry ahlanzekile futhi asebenzisekile, Umq. 74/12, 2002; iphe. 2265-2269.
  13. Török, B. et al. (2001): Ukusabela okulinganiselwe ku-sonochemistry. Ultrasonics Sonochemistry 8, 2001; k. 191-200.
  14. Wang, Maw-Ling et al. (2007): Ukuxoshwa kwesigaba sokudluliswa kwesigaba se-Ultrasound esiyinkimbinkimbi ye-1,7-octadiene - Ucwaningo lwekinetic. Ku: Ultrasonics Sonochemistry Vol. 14/1, 2007; k. 46-54.
  15. I-Yang, H.-M .; Chu, W.-M. (2012): I-Ultrasound-Assisted Phase-Transfer Catalysis: i-Green Synthesis ye-Benzoate esakhiwe nge-Novel Dual-Site Phase-Transfer Catalyst ku-System-Solid-Liquid System. Ku: Ukuqhubela phambili kokungu-14th I-Asia Pacific Confederation of Chemical Engineering Congress APCChE 2012.


Amaqiniso Okufanele Ukwazi

I-ultrasonic izicubu ze-homogenizers ngokuvamile ibizwa ngokuthi i-sonicator yesondlo, i-lyser ye-sonic, i-ultrasound ephazamisayo, i-grinder ye-ultrasonic, i-sono-ruptor, i-sonifier, i-sonic dismembrator, i-cell disrupter, i-ultrasonic disperser noma i-dissolver. Amagama ahlukene avela ezinhlobonhlobo zokusebenza ezingagcwaliseka nge-sonication.