Hydrazine sulfate, tseem hu ua hydrazine sulfate , yog ib tug liab scaly siv lead ua los yog rhombic siv lead ua. Tus txheeb ze ntom ntom yog 1.37, lub melting point yog 254 degree, thiab decomposition tshwm sim thaum cua sov txuas ntxiv. Nws yog me ntsis soluble hauv dej txias thiab yooj yim soluble hauv dej kub. Cov tshuaj aqueous yog acidic thiab insoluble hauv ethanol thiab ether. Nws yog ruaj khov heev nyob rau hauv cov huab cua thiab susceptible alkali thiab oxidant. Nws muaj zog reducibility. Hydrazine ua los ntawm oxidizing ammonia nrog sodium hypochlorite yog npaj los ntawm reacting nrog sulfuric acid, los yog ncaj qha los ntawm reacting hydrazine nrog sulfuric acid. Nws yog siv rau kev txiav txim siab gravimetric ntawm npib tsib xee, cobalt thiab cadmium, kev ua kom huv ntawm cov hlau tsawg thiab kev sib cais ntawm polonium thiab tellurium, nrog rau nag lossis daus ntawm chlorate, hypochlorite thiab carboxyl compounds. Nws kuj yog siv rau kev npaj ntawm isoniazid, furacilin, parahydrazine, anhydrous hydrazine, thiab lwm yam. nws kuj yog siv los ua ib tug txo tus neeg sawv cev, tshuaj tua kab thiab kom tsis muaj menyuam.
Kev npaj ntawm hydrazine sulfate:
Txoj Kev 1: sodium hypochlorite tau npaj los ntawm cov tshuaj tiv thaiv chlorine thiab sodium hydroxide, tom qab ntawd hnov mob nrog ammonia los npaj hydrazine hydrate, thaum kawg lub cev qhuav dej los npaj hydrazine, thiab tom qab ntawd ua rau cov tshuaj sulfuric acid los npaj hydrazine sulfate.
Txoj Kev 2: hydrazine sulfate tau tsim los ntawm hydrazine hydrate los ntawm kev tso cov concentrated sulfuric acid. Cov kauj ruam tshwj xeeb yog raws li nram no:
1) Dilute ib qho nyiaj ntawm hydrazine hydrate (80 feem pua) thiab tom qab ntawd ntxiv rau hauv plaub lub caj dab, thiab maj mam txias hauv da dej kub.
2) Ntxiv 98 feem pua ntawm cov tshuaj sulfuric acid nyob rau hauv qhov tso tawm thiab maj mam muab tso rau hauv plaub lub caj dab lub raj mis, ua kom qhov kub thiab txias hauv lub hwj ntawm li 0-10 degree , thiab ntsuas nws pH nrog pH daim ntawv xeem. Kev poob tuaj yeem nres thaum tus nqi pH yog 5-7.
3) Txias cov tshuaj maj mam, do maj mam, thiab muab cia rau 2 teev. cov khoom dawb tuaj yeem kho tau.
4) Ntxiv cov tshuaj methanol kom raug rau hauv cov tshuaj tov, precipitate thiab lim kom tau hydrazine sulfate khoom.
Txoj kev 3: ib txoj kev npaj ntawm hydrazine sulfate, muaj cov hauv qab no cov kauj ruam:
S1. Siv butanone thiab ammonia ua raw cov ntaub ntawv, huab cua li oxidant, PdCl2 thiab CuCl2 ua catalysts, formamide thiab sodium bromide ua cocatalysts los ua ke butanone thiab nitrogen;
S2. Sib cais cov roj theem siab uas muaj butanone thiab nitrogen thiab theem aqueous uas muaj cov catalyst;
S3. Tus nqi pH ntawm cov roj sib cais yog hloov kho rau 1-4 nrog cov kua qaub, thiab butanone thiab nitrogen yog acid hydrolyzed rau hauv hydrazine ntsev thiab butanone;
S4. Kho tus nqi pH ntawm cov tshuaj uas muaj hydrazine ntsev rau 9-12, neutralize hydrazine ntsev nrog alkali los tsim hydrazine hydrate, evaporate tag nrho cov hydrazine hydrate thiab dej hauv cov tshuaj, thiab distilled cov condensate rau hauv hydrazine hydrate tov;
S5. Hydrazine sulfate yog npaj los ntawm kev ntxiv concentrated sulfuric acid rau hydrazine hydrate, thiab cov khoom hydrazine sulfate yog tau los ntawm txias crystallization, nqus pom, ntxuav thiab ziab.
Txoj Kev 4: ib txoj kev npaj ntawm qib siab ntshiab hydrazine sulfate. Cov txheej txheem npaj tshwj xeeb yog raws li hauv qab no: (1) ntxiv dej ntshiab rau hauv cov iav lined reactor, maj mam ntxiv 98 feem pua sulfuric acid nyob rau hauv nplawm thiab txias, ntxiv 80 feem pua hydrazine hydrate ntawm 70-80 degree tom qab ntxiv, thiab lim thaum kub. nyob rau hauv qhov sib piv loj ntawm cov dej ntshiab, 98 feem pua sulfuric acid thiab 80 feem pua hydrazine hydrate yog 10:10:4; (2) Cov lim dej tau hloov kho rau pH=4-5 nrog sulfuric acid lossis hydrazine hydrate, thiab nplawm rau 20-60min. Thaum lub pH tsis hloov, nws yog txias thiab crystallized rau 25 degree, centrifuged thiab crystallized, ntxuav nrog kiag li ethanol, thiab cua qhuav nyob rau hauv chav tsev kub kom tau cov khoom tiav; Txoj kev npaj yog yooj yim nyob rau hauv tus txheej txheem. Raws li cov txheej txheem kev lag luam, kev npaj tshuaj reagent hydrazine sulfate tau tsim. Cov khoom lag luam tau nce mus txog qib siab purity tus qauv thiab tsim nyog rau cov kev xav tau ntawm kev lag luam loj.
Hydrazine sulfate feem ntau yog siv los ua raw khoom rau kev tsim tshuaj thiab qib qib azodiisobutyronitrile. Nws kuj tseem tuaj yeem siv los ua tus neeg saib xyuas kev txo qis, feem ntau yog siv los ua cov tshuaj reagent rau kev kho cov hlau saum npoo thiab tshuaj xyuas, thiab tseem siv rau kev ua kom huv ntawm cov hlau tsis tshua muaj. Hauv kev ua liaj ua teb, nws yog siv los ua tshuaj tua kab thiab tshuaj tua kab mob. Nws daim ntawv thov piv txwv yog raws li nram no:
1. Kev txiav txim siab ntawm Trace Selenium los ntawm hydrazine sulfate Turbidimetry
Selenium yog ib qho tseem ceeb ntawm cov kab mob rau ntau yam kab mob, suav nrog tib neeg. Nws muaj ntau yam kev ua haujlwm ntawm lub cev xws li tiv thaiv qog noj ntshav, tiv thaiv oxidation thiab tiv thaiv cov hlau hnyav hnyav. Cov kev tshawb fawb tau pom tias muaj ntau yam kab mob phem muaj feem cuam tshuam nrog selenium deficiency, xws li qog nqaij hlav qog noj ntshav, mob qog noj ntshav, mob ntsws, mob ntsws, mob ntsws ntsws, kab mob Keshan, kab mob Kashin Beck, kab mob hauv lub cev xeeb tub thiab lwm yam. Vim tias feem ntau ntawm peb lub teb chaws nyob rau hauv cov khoom siv selenium tsawg thiab cov ntsiab lus ntawm selenium hauv av yog tsawg, tib neeg tau them nyiaj ntau thiab ntau dua rau kev noj cov selenium los ntawm cov khoom noj thiab tshuaj. Txawm li cas los xij, ntau npaum li cas ntawm selenium tshuaj lom yog nqaim heev, yog li nws muaj qhov tseem ceeb hauv kev txiav txim siab cov ntsiab lus ntawm selenium hauv cov zaub mov thiab tshuaj.
2. Rau kev npaj 4-methylpyrazole
Methylpyrazole yog ib qho cawv dehydrogenase inhibitor pom zoo los ntawm US FDA thiab tsim los ntawm kev kho mob menyuam ntsuag thaum ntxov 1998. Nws yog siv los cawm cov cawv xws li ethylene glycol, ethanol thiab methanol. Ua ntej, cov concentrated sulfuric acid thiab hydrazine hydrate yog siv los ua raw khoom los tsim hydrazine sulfate los ntawm cua sov thiab refluxing; Tom qab ntawd, sulfuric acid, hydrazine sulfate thiab poov tshuaj iodide yog ntxiv rau lub reactor, isobutyraldehyde ntxiv nyob rau hauv cov xwm txheej ntawm nruam stirring rau cua sov thiab refluxing cov tshuaj tiv thaiv. Tom qab cov tshuaj tiv thaiv, pH ntawm cov tshuaj tiv thaiv yog kho rau 7, thiab tom qab ntawd cov kuab tshuaj yog muab rho tawm, qhuav thiab evaporated thiaj li yuav tau txais cov crude 4-methylpyrazole; Subjecting tau cov khoom crude rau thawj lub tshuab nqus tsev distillation rau purification; Tom qab thawj zaug purification, cov khoom tau ntxiv rau cov kua sib tov ntawm ethyl acetate thiab roj av ether rau recrystallization, thiab thaum kawg, nws tau distilled dua nyob rau hauv txo siab kom tau 4-methylpyrazole refined khoom. Lub 4-methylpyrazole npaj los ntawm invention yuav ua tau nyob rau hauv ib txwm siab, txoj kev npaj yog yooj yim, thiab yog conducive rau industrial ntau lawm; Qhov purity ntawm 4-methylpyrazole yog siab, thiab cov ntsiab lus ntawm ib qho impurity tsawg dua 0.1 feem pua, uas ua tau raws li qhov yuav tsum tau ua.