Ethyl caprylate(txuas:https://www.bloomtechz.com/synthetic-chemical/additive/ethyl-caprylate-cas-106-32-1.html) yog ib yam tshuaj uas muaj ntxhiab thiab fruity saj, uas yog dav siv nyob rau hauv cov zaub mov, txuj lom, flavors, tshuaj thiab lwm yam teb. Ntxiv rau alkyd esterification, transesterification thiab esterification txo, muaj lwm txoj hauv kev los ua ke Ethyl caprylate.
1. Sulfate esterification txoj kev:
Txoj kev sulfate esterification yog ib txoj kev siv tshuaj tiv thaiv feem ntau rau kev npaj sulfate ester tebchaw. Nws tuaj yeem hnov mob cawv nrog sulfuric acid los tsim cov sulfate ester sib xws. Cov tshuaj tiv thaiv kab zauv sib npaug ntawm txoj kev sulfate esterification tuaj yeem qhia tau tias:
ROH + HOSO₃H → RSO₃H + H₂O
Ntawm lawv, ROH sawv cev rau cawv thiab RSO₃H sawv cev rau sulfate ester. Hauv cov tshuaj tiv thaiv tshwj xeeb, cawv thiab cov ethanol kiag li sib xyaw hauv qhov sib piv ntawm 1: 1, tom qab ntawd ntxiv sulfuric acid thiab sulfur trioxide, thiab qhov kub thiab txias yog tswj ntawm 0-5 degree rau cov tshuaj tiv thaiv. Tom qab cov tshuaj tiv thaiv tiav, ntxiv dej los kho cov pH rau nruab nrab, tom qab ntawd rho tawm cov theem ntawm cov organic nrog diethyl ether, thiab thaum kawg siv cov evaporator rotary kom evaporate cov diethyl ether nyob rau hauv cov organic theem kom tau cov khoom nyoos. Cov khoom nyoos yog ua kom zoo kom tau txais cov khoom lag luam siab purity sulfate ester.
Kev sim cov kauj ruam:
Kauj Ruam 1: Sib tov Ethyl caprylate (ethyl acetate) thiab ethanol kiag li hauv qhov sib piv ntawm 1: 1, ntxiv rau lub khob, thiab do sib npaug.
Kauj Ruam 2: Sib tov cov concentrated sulfuric acid thiab sulfur trioxide ntawm qhov sib piv ntawm 1: 1, maj mam poob rau hauv lub hwj, thiab tswj cov tshuaj tiv thaiv kub ntawm 0-5 degree .
Kauj Ruam 3: Khaws qhov kub ntawm 0-5 degree thiab do rau 30 feeb kom muaj kev sib haum xeeb ntawm ethyl acetate thiab ethanol.
Kauj Ruam 4: Cov cua kub ntau yuav raug tsim thaum lub sij hawm cov tshuaj tiv thaiv, thiab cov tshuaj tiv thaiv kub tuaj yeem tswj tau los ntawm kev siv cov dej khov da dej.
Kauj Ruam 5: Tom qab cov tshuaj tiv thaiv tiav lawm, ntxiv cov dej tsim nyog los ua kom cov tshuaj tiv thaiv acidic, thiab tom qab ntawd ntxiv cov tshuaj sodium hydroxide los kho cov pH rau nruab nrab.
Kauj Ruam 6: Extract cov tshuaj tiv thaiv nrog diethyl ether, thiab sau cov organic theem los ntawm kev sib cais kua.
Kauj Ruam 7: Siv cov evaporator teb kom evaporate cov diethyl ether nyob rau hauv cov organic theem kom tau cov khoom nyoos.
Kauj Ruam 8: Kev kho cov khoom nyoos, koj tuaj yeem siv txoj hauv kev xws li distillation lossis recrystallization kom tau txais Ethyl caprylate sulfate nrog purity siab dua.
Sulfuric acid esterification yog esterification cov tshuaj tiv thaiv siv sulfuric acid ua ib qho catalyst. Cov tshuaj tiv thaiv no feem ntau ua tiav ntawm qhov kub thiab txias, thiab cov kua qaub catalyst ntxiv los txhawb cov tshuaj tiv thaiv. Tsis tas li ntawd, vim tias yuav tsum tau siv ntau cov kua qaub catalysts, ntau cov kua qaub kua qaub yuav raug tsim tawm, uas ua rau muaj teeb meem loj rau ib puag ncig.
2. Nyob rau hauv-situ tiam ntawm acetic acid txoj kev:
Txoj kev tsim cov acetic acid nyob rau hauv qhov chaw yog sib tov n-octanol, sodium acetate thiab dej me me, ntxiv ib qho tsim nyog ntawm sulfuric acid rau qhov sib tov, thiab ua kom sov qhov sib xyaw kom txog 90 degrees Celsius. Tom qab ntawd, ethanol tau maj mam ntxiv rau cov tshuaj tiv thaiv sib xyaw, thiab cov tshuaj tiv thaiv kub thiab lub sijhawm raug tswj los txhawb kev tsim ntawm Ethyl caprylate. Thaum kawg, cov txheej txheem xws li rho tawm thiab distillation tuaj yeem siv los cais thiab ntxuav cov khoom siv tshuaj tiv thaiv.
Kev sib npaug tshuaj tiv thaiv kab mob:
CH₃CH₂OH + NH₃ → CH₃CH₂ONH₃⁺ + OH⁻
CH₃CH₂OH + CO₂ → CH₃CH₂CO₂H + H₂O NH₃ + H₂O + CO₂= NH₄HCO₃
NH₄HCO₃ + H₂SO₄= NH₄HSO₄+ CO₂+ H₂O NH₄HSO₄+ CH₃CH₂OH= CH₃CH₂O⁺ + NH₄₂OH² + SO
Cov kauj ruam tshwj xeeb yog raws li hauv qab no:
(1) Ntxiv ethanol thiab ammonia dej rau lub reactor, do sib npaug, thiab tswj cov tshuaj tiv thaiv kub ntawm 25-30 degree .
(2) Muab cov pa roj carbon dioxide rau hauv lub reactor, ua kom lub siab ntawm 2-3 cua, thiab lub sij hawm tshuaj tiv thaiv yog 2-3 teev.
(3) Tom qab cov tshuaj tiv thaiv tiav, lim cov tshuaj tiv thaiv kom tshem tawm cov dej nag.
(4) Ntxiv sulfuric acid rau filtrate kom cov concentration ntawm sulfuric acid nyob rau hauv cov tshuaj yog 80%, ces kub mus rau 70-80 degree thiab tswj qhov kub ntawm no rau 2-3 teev.
(5) Tom qab cov tshuaj tiv thaiv, ntxiv cov dej tsim nyog los ua kom cov tshuaj tiv thaiv acidic, thiab tom qab ntawd ntxiv ether los rho tawm cov tshuaj tiv thaiv.
(6) Distilled lub aqueous theem muab rho tawm nrog diethyl ether siv ib tug teb evaporator kom tau crude ethyl acetate khoom.
(7) Txhawm rau txhim kho cov khoom siv raw, distillation lossis recrystallization tuaj yeem siv tau kom tau txais ethyl acetate nrog ntau dua purity.
Txoj kev no yog cov tshuaj tiv thaiv esterification uas tsim cov acetic acid hauv qhov chaw. Reactants muaj xws li n-octanol, sodium acetate, thiab sulfuric acid. Txoj kev no yuav tsum muaj cov cuab yeej tshwj xeeb thiab kev ua haujlwm, thiab muaj kev nkag siab zoo rau cov ntsiab lus ntawm sulfuric acid thiab dej cov ntsiab lus, yog li nws nyuaj rau kev khiav lag luam. Tsis tas li ntawd, kev siv cov catalyst sulfuric acid kuj yuav ua rau cov kua qaub ntau ntau, ua rau muaj kuab paug ib puag ncig.
3. Kev kub siab oxidation txoj kev:
Cov txheej txheem oxidation siab yog sib tov n-octanol thiab acetic acid ntawm molar piv ntawm 1: 1, thiab ntxiv cov sib tov rau cov khoom siv tshuaj tiv thaiv nrog oxygen thiab catalyst. Cov khoom siv yuav tsum muaj tej yam kev mob xws li kub, siab thiab oxygen input rate. Los ntawm kev tswj cov tshuaj tiv thaiv lub sijhawm thiab cov xwm txheej, Ethyl caprylate yog tsim tau zoo. Thaum kawg, kev sib cais thiab kev ua kom huv yog siv los cais thiab ntxuav cov Ethyl caprylate los ntawm cov tshuaj tiv thaiv sib tov.
Ethyl acetate tau txais cov tshuaj tiv thaiv oxidation nyob rau hauv qhov kev txiav txim ntawm hydrogen peroxide thiab concentrated sulfuric acid los tsim acetic acid thiab dej. Cov tshuaj tiv thaiv kab mob sib npaug yog: CH₃CH₂OOC₂H₅+ H₂O₂+ H₂SO₄= CH₃CH₂OH+ CH₃COOH+ H₂O
Cov kauj ruam ntxaws yog raws li nram no:
(1) Ntxiv ethyl acetate, hydrogen peroxide thiab concentrated sulfuric acid rau lub siab-siab reactor, do sib npaug, thiab tswj cov tshuaj tiv thaiv kub ntawm 80-100 degree .
(1) Kaw lub siab-siab reactor, nce qhov kub thiab txias mus rau 100-150 degree, thiab tswj qhov kub ntawm no rau 3-5 teev.
(1) Tom qab cov tshuaj tiv thaiv tiav, txias cov tshuaj tiv thaiv kua rau hauv chav tsev kub, thiab rho tawm cov tshuaj tiv thaiv kua nrog toluene.
(1) Distilled lub aqueous theem muab rho tawm nrog toluene siv ib tug teb evaporator kom tau crude ethyl acetate khoom.
(1) Txhawm rau kho cov khoom lag luam tsis zoo, distillation lossis recrystallization tuaj yeem siv tau kom tau txais ethyl acetate nrog purity siab dua.
Raws li lub npe qhia, high-pressure oxidation yog hais txog cov tshuaj tiv thaiv oxidation ua nyob rau hauv high-pressure oxygen cua. Txoj kev no yuav tsum muaj cov khoom siv tshuaj tiv thaiv tshwj xeeb thiab cov xwm txheej thiab tsuas yog tsim nyog rau qee yam tshuaj tshwj xeeb. Nyob rau tib lub sijhawm, vim qhov xav tau siv cov pa oxygen ntau, cov nqi khiav haujlwm ntawm txoj kev no yog qhov siab. Tsis tas li ntawd, muaj qee yam teeb meem kev nyab xeeb thaum hnov mob nyob rau hauv qhov kub thiab txias, siab siab, thiab siab concentration oxygen cua.
4. Alkyl tooj liab-mediated dawb radical cov tshuaj tiv thaiv:
Alkyl tooj liab-mediated dawb radical cov tshuaj tiv thaiv yog ib txoj hauv kev zoo rau kev tsim cov ntaub ntawv polymer. Sib tov n-octanol thiab acetic acid ntawm molar piv ntawm 1: 1, tom qab ntawd ntxiv qhov tsim nyog ntawm alkyl tooj liab reagent, thiab kho qhov kub thiab txias sijhawm. ua raws li cov xwm txheej. Ethyl caprylate yog purified los ntawm kev sib cais thiab purification cov txheej txheem.
Copper alkyl-mediated dawb radical tshua feem ntau cuam tshuam nrog kev hloov pauv ntawm ntau pawg ua haujlwm. Ntawm no yog ib qho piv txwv ntawm cov tshuaj tiv thaiv kab mob sib npaug:
Ethyl caprylate thiab alkyl tooj liab ntsev tau txais kev sib txuas cov tshuaj tiv thaiv nyob rau hauv qhov kev txiav txim ntawm dawb radical pib los tsim ib lub siab molecular polymer. Cov txheej txheem no tuaj yeem qhia tau tias:
nC6H5CH2CH2CuBr + (C6H5CH2CH2) mBr → (C6H5CH2CH2n + mCuBr2+ mHBr
qhov twg n sawv cev rau qib ntawm polymerization thiab m sawv cev rau tus naj npawb ntawm cov saw txuas. Qhov sib npaug tshuaj tiv thaiv kab mob no sawv cev rau cov qauv ntawm kev sib txuas ntau Ethyl caprylate molecules los ntawm cov tshuaj tiv thaiv dawb radical mediated los ntawm alkyl tooj liab los tsim cov kab txuas polymer.
Kev sim cov kauj ruam:
(1) Ntxiv Ethyl caprylate thiab tooj liab ntsev rau lub reactor, do tusyees, thiab tswj cov tshuaj tiv thaiv kub ntawm chav tsev kub thiab 80 degree.
(2) Ntxiv cov dawb radical pib poob los ntawm kev poob, ua kom cov tshuaj tiv thaiv kub tas li kom pib cov tshuaj tiv thaiv dawb radical.
(3) Thaum lub sij hawm cov txheej txheem tshuaj tiv thaiv, qib ntawm cov tshuaj tiv thaiv dawb radical tuaj yeem hloov kho los ntawm kev tswj lub sij hawm thiab qhov kub thiab txias.
(4) Tom qab cov tshuaj tiv thaiv tiav lawm, siv qhov sib cais los cais cov tshuaj tiv thaiv rau hauv cov theem organic thiab theem aqueous.
(5) Rotary evaporate cov organic theem kom tau cov khoom nyoos.
(6) Txhawm rau txhim kho cov khoom lag luam tsis zoo, distillation lossis recrystallization tuaj yeem siv tau kom tau txais cov khoom lag luam nrog ntau dua purity.
Alkyl tooj liab-mediated dawb radical cov tshuaj tiv thaiv yog cov tshuaj tiv thaiv dawb radical catalyzed siv alkyl tooj liab reagents. Cov tshuaj tiv thaiv no siv cov qauv tshwj xeeb thiab cov khoom ntawm alkyl tooj liab los txhawb oxidation los yog hloov cov tshuaj tiv thaiv ntawm atoms lossis molecules. Nyob rau hauv cov tshuaj tiv thaiv no, alkyl tooj liab plays ob lub luag hauj lwm ntawm catalyst thiab active hom, txhim kho cov tshuaj tiv thaiv tus nqi thiab xaiv.
Hauv cov ntsiab lus, ntxiv rau alkyd esterification cov tshuaj tiv thaiv, cov tshuaj tiv thaiv transesterification thiab esterification txo cov tshuaj tiv thaiv, muaj lwm txoj hauv kev uas tuaj yeem siv los ua ke Ethyl caprylate. Txawm li cas los xij, txhua txoj kev muaj nws qhov tshwj xeeb zoo, qhov tsis zoo thiab qhov kev thov, thiab cov qauv tsim nyog yuav tsum tau xaiv raws li qhov xwm txheej tiag tiag. Nyob rau tib lub sijhawm, cov kev ua haujlwm thiab cov nqi lag luam kuj yuav tsum tau tswj xyuas nruj me ntsis thaum lub sijhawm ua haujlwm kom ntseeg tau tias kev ua haujlwm zoo thiab kev nyab xeeb ntawm cov tshuaj tiv thaiv.