TRI-N-OCTYLPHOSPHINE (txuas:https://www.bloomtechz.com/synthetic-chemical/organic-intermediates/tri-n-octylphosphine-cas-4731-53-7.html) yog ib qho organophosphorus compound nrog ntau yam kev siv. Ob peb txoj hauv kev rau kev sib xyaw TRI-N-OCTYLPHOSPHINE yuav qhia.
1. Phosphorus trichloride txoj kev:
Tshuaj tiv thaiv formula:
3 C8H17Nr + PCl3 → [(C8H17)3P] + 3 HCl
Cov kauj ruam tshuaj tiv thaiv:
Kauj Ruam 1: Qhuav Bromide
- Qhuav n-octyl bromide (C8H17Br) nyob rau hauv lub tshuab nqus tsev los ntawm lub tshuab ziab khaub ncaws los yog qhov cub kom tshem tawm cov dej noo.
Kauj Ruam 2: Inert huab cua tiv thaiv
- Thaum lub sij hawm cov txheej txheem tshuaj tiv thaiv, ib qho chaw inert tas li yuav tsum tau tswj kom tsis txhob muaj huab cua thiab noo noo nkag mus rau hauv cov tshuaj tiv thaiv.
- Txuas cov roj inert (xws li nitrogen) muab cov khoom siv los qhia cov roj inert rau hauv cov tshuaj tiv thaiv.
Kauj Ruam 3: Cov khoom siv tshuaj tiv thaiv kev npaj
- Npaj cov tshuaj tiv thaiv qhuav vial (xws li lub khob ntim hauv qab) thiab tso lub vial rau hauv lub tshuab ua kom sov. Xyuas kom lub hauv qab ntawm lub raj mis yog nruab nrog ib tug sib nqus do bar.
Kauj Ruam 4: Ntxiv Phosphorus Trichloride
- Ntxiv qhov tsim nyog ntawm phosphorus trichloride (PCl3) mus rau cov tshuaj tiv thaiv lub raj mis thaum tuav ib qho chaw inert los tiv thaiv cov ingress ntawm ya raws thiab oxygen.
Kauj Ruam 5: Ntxiv n-octyl bromide
- Maj mam los yog tsis tu ncua tso n-octyl bromide (C8H17Br) rau hauv cov tshuaj tiv thaiv lub khob.
- Txhawm rau tswj cov tshuaj tiv thaiv tus nqi thiab qhov kub thiab txias, bromide yuav tsum tau ntxiv maj mam.
Kauj Ruam 6: Kev tswj qhov kub thiab txias
- Thaum lub sij hawm cov tshuaj tiv thaiv, tswj qhov ntsuas kub kom tsim nyog, feem ntau yog nyob rau hauv thaj tsam ntawm 30-60 degrees Celsius.
- Siv lub da dej kub tas li los yog lub rhaub dej kub kom tswj tau qhov kub thiab txias.
Kauj Ruam 7: Nucleophilic hloov cov tshuaj tiv thaiv
- Lub bromine atom yog hloov los ntawm ib tug phosphine atom los ntawm ib tug nucleophilic hloov cov tshuaj tiv thaiv.
- Ib qho kev xaiv nucleophile xws li thiourea lossis thiouracil tuaj yeem siv los ua kom tiav cov kauj ruam no.
Kauj Ruam 8: Ntxiv cov Nucleophile
- Ntxiv cov nucleophile rau cov tshuaj tiv thaiv lub raj mis thiab txuas ntxiv do cov tshuaj tiv thaiv ntawm qhov kub siab, feem ntau yog nyob rau thaj tsam ntawm 80-100 degrees Celsius.
Kauj Ruam 9: Sib tov sib xyaw ua ke
- Tom qab lub sij hawm tsim nyog, TRI-N-OCTYLPHOSPHINE yuav raug tsim nyob rau hauv cov tshuaj tiv thaiv sib tov.
- Extract thiab purify cov khoom uas xav tau los ntawm kev sib cais thiab purification cov kauj ruam (xws li hnyav extraction, crystallization, distillation, thiab lwm yam).
2. Direct phosphating txoj kev:
Tshuaj tiv thaiv formula:
3 C8H18 + P4 → 3 (C8H17)3P
Cov kauj ruam tshuaj tiv thaiv:
Kauj Ruam 1: Raw khoom kom qhuav
- Qhuav n-octane (C8H18) thiab dawb phosphorus (P4) nyob rau hauv lub tshuab nqus tsev los ntawm lub tshuab ziab khaub ncaws los yog qhov cub kom tshem tawm cov dej noo thiab impurities.
Kauj Ruam 2: Inert huab cua tiv thaiv
- Thaum lub sij hawm cov txheej txheem tshuaj tiv thaiv, ib qho chaw inert tas li yuav tsum tau tswj kom tsis txhob muaj huab cua thiab noo noo nkag mus rau hauv cov tshuaj tiv thaiv.
- Txuas cov roj inert (xws li nitrogen) muab cov khoom siv los qhia cov roj inert rau hauv cov tshuaj tiv thaiv.
Kauj Ruam 3: Kev Npaj Reactor
- Npaj cov tshuaj tiv thaiv qhuav vial (xws li lub khob ntim hauv qab) thiab tso lub vial rau hauv lub tshuab ua kom sov. Xyuas kom lub hauv qab ntawm lub raj mis yog nruab nrog ib tug sib nqus do bar.
Kauj Ruam 4: Cua sov cov tshuaj tiv thaiv vial
- Tshav kub cov tshuaj tiv thaiv vial rau qhov tsim nyog kub. Feem ntau, cov tshuaj tiv thaiv kub yog nyob rau hauv thaj tsam ntawm 150-200 degrees Celsius.
Kauj Ruam 5: Ntxiv Phosphorus Dawb
- Maj mam ntxiv ua ntej qhuav dawb phosphorus hmoov rau lub rhaub dej kub.
- Batch ntxiv yog pom zoo los tswj cov tshuaj tiv thaiv tus nqi thiab kub.
Kauj Ruam 6: Ntxiv n-octane
- Maj mam ntxiv n-octane dropwise rau cov tshuaj tiv thaiv lub khob.
- n-octane yuav ua raws li hnyav thiab txo tus neeg sawv cev hauv cov tshuaj tiv thaiv phosphating.
Kauj Ruam 7: Cov tshuaj tiv thaiv stirring thiab kub tswj
- Txuas ntxiv mus do cov tshuaj tiv thaiv sib tov thiab tswj cov tshuaj tiv thaiv kom zoo.
- Kev tswj qhov kub thiab txias yog qhov tseem ceeb los xyuas kom meej txaus thiab xaiv cov tshuaj tiv thaiv.
Kauj Ruam 8: Cov khoom rho tawm thiab purification
- Tom qab lub sij hawm tsim nyog, TRI-N-OCTYLPHOSPHINE yuav raug tsim nyob rau hauv cov tshuaj tiv thaiv sib tov.
- Raws li qhov xav tau, cov khoom xav tau tuaj yeem muab rho tawm thiab ua kom huv los ntawm kev sib cais thiab kev ua kom huv (xws li hnyav rho tawm, crystallization, distillation, thiab lwm yam).
3. Phosphine hydride txoj kev:
Txoj kev phosphine hydride yog ib txoj hauv kev tshiab rau kev npaj TRI-N-OCTYLPHOSPHINE, uas muaj kev xaiv ntau dua thiab cov txheej txheem sib dua. Tshuaj tiv thaiv formula:
(C8H17)3P + H2 → (C8H17)3PH
Cov kauj ruam tshuaj tiv thaiv:
Kauj Ruam 1: Inert huab cua tiv thaiv
- Thaum lub sij hawm cov txheej txheem tshuaj tiv thaiv, ib qho chaw inert tas li yuav tsum tau tswj kom tsis txhob muaj huab cua thiab noo noo nkag mus rau hauv cov tshuaj tiv thaiv.
- Txuas cov roj inert (xws li nitrogen) muab cov khoom siv los qhia cov roj inert rau hauv cov tshuaj tiv thaiv.
Kauj Ruam 2: Kev Npaj Reactor
- Npaj cov tshuaj tiv thaiv qhuav los yog lub raj mis tshuaj tiv thaiv, thiab muab lub raj mis los yog lub raj mis tso rau hauv lub tshuab ua kom sov. Xyuas kom tseeb tias hauv qab ntawm lub raj mis los yog lub raj mis yog nruab nrog lub tshuab nqus hlau nplaum.
Kauj Ruam 3: Ntxiv tri-n-octylphosphine
- Maj mam ntxiv cov pre-npaj tri-n-octylphosphine rau hauv cov tshuaj tiv thaiv kettle los yog lub raj mis.
- Tri-n-octylphosphine yuav ua cov khoom pib rau cov tshuaj tiv thaiv phosphating.
Kauj Ruam 4: Ntxiv Acid Catalyst
- Ntxiv cov kua qaub uas tsim nyog (xws li hydrochloric acid lossis sulfuric acid). Acid catalysts tuaj yeem pab txhawb cov tshuaj tiv thaiv.
Kauj Ruam 5: Qhia Txog Hydrogen
- Qhib cov khoom siv hydrogen thiab cia hydrogen ntws maj mam mus rau hauv lub reactor lossis lub raj mis.
- Hydrogen yuav ua raws li tus neeg sawv cev txo qis rau cov tshuaj tiv thaiv.
Kauj Ruam 6: Cov tshuaj tiv thaiv stirring thiab kub tswj
- Pib lub thermostatic stirrer kom sib tov cov tshuaj tiv thaiv kom zoo.
- Tswj cov tshuaj tiv thaiv kub kom ntseeg tau tias cov tshuaj tiv thaiv tshwm sim.
Kauj Ruam 7: Kev Tiv Thaiv Lub Sijhawm Tswjhwm
- Raws li qhov xav tau, tswj qhov ntev ntawm cov tshuaj tiv thaiv lub sijhawm. Cov tshuaj tiv thaiv ntev dua tuaj yeem ua rau muaj txiaj ntsig thiab purity.
Kauj Ruam 8: Cov khoom rho tawm thiab purification
- Tom qab lub sij hawm tsim nyog, TRI-N-OCTYLPHOSPHINE yuav raug tsim nyob rau hauv cov tshuaj tiv thaiv sib tov.
- Raws li qhov xav tau, cov khoom xav tau tuaj yeem muab rho tawm thiab ua kom huv los ntawm kev sib cais thiab kev ua kom huv (xws li hnyav rho tawm, crystallization, distillation, thiab lwm yam).
Nws yuav tsum raug sau tseg tias thaum lub sij hawm synthesis ntawm TRI-N-OCTYLPHOSPHINE, cov ntsiab lus hauv qab no yuav tsum raug sau tseg:
1) Xyuas kom tseeb tias cov reactor thiab reagents qhuav ua ntej cov tshuaj tiv thaiv kom tsis txhob muaj cov dej noo ntawm cov catalyst lossis reactants.
2) Txij li qee cov tshuaj lom neeg siv rau hauv cov txheej txheem synthesis, thov ua raws li cov txheej txheem kev nyab xeeb thiab siv cov kev tiv thaiv tsim nyog.
3) Thaum lub sij hawm cov txheej txheem tshuaj tiv thaiv, cov tshuaj tiv thaiv kub, cov tshuaj tiv thaiv lub sij hawm thiab feem ntawm cov reactants yuav tsum tau tswj kom ntseeg tau siab yield thiab purity.
4) Thaum kawg, cov synthesized TRI-N-OCTYLPHOSPHINE tuaj yeem dhau los ua cov kauj ruam ua kom huv, xws li recrystallization, distillation, thiab lwm yam, kom tau txais cov khoom purer.