Cov ntsiab lus tseem ceeb ntawmDBDMH (txuas:https://www.bloomtechz.com/basic-chemicals/raw-materials/dbdmh-cas-77-48-5.html) yog dibromohydrin, ib tug derivative ntawm hydantoin thiab dawb los yog lub teeb daj crystalline hmoov. Nws yog ib yam tshiab ntawm cov tshuaj tua kab mob uas muaj txiaj ntsig zoo nrog cov kab mob dav dav, cov kab mob bactericidal muaj zog, kev ua haujlwm me me, thiab tuaj yeem decomposed rau hauv carbon dioxide, nitrogen thiab dej. Lub downside yog tias nws dissolves qeeb heev hauv dej. Raws li cov kab mob bactericidal thiab algicide, nws tuaj yeem tua ntau yam kab mob, fungi, kab mob, algae, kab mob siab kab mob siab, Escherichia coli, Staphylococcus aureus, gonorrhea, kab mob cholera, Salmonella typhimurium, thiab lwm yam. Nws tuaj yeem siv dav hauv kev tua kab mob ntawm pej xeem chaw, tshuaj tua kab mob. ntawm cov khoom ib puag ncig, tshuaj tua kab mob ntawm cov khoom siv huv, thiab kev txuag zaub mov: hauv aquaculture, nws tuaj yeem tiv thaiv thiab tswj tau ntau yam kab mob thiab cov kab mob fungal xws li ntses, vaub kib, crabs, cws, qav, thiab shellfish. Kab mob; Disinfect thiab sterilize cov dej ua lag luam, kais dej, dej phwj hauv tsev, thiab cov pas dej da dej.
Vim nws txoj kev siv ntau yam, ntau tus kws tshawb fawb tau kawm txog cov khoom. Txhawm rau nce cov txiaj ntsig ntawm cov khoom, cov kws tshawb fawb tau ua ntau yam kev sim los txhim kho qhov purity ntawm cov khoom. Ntawm no peb sau plaub txoj kev siv hluavtaws rau 1,3-Dibromo-5,5-dimethylhydantoin (DBDMH):
1. Hydrobrominated urea txoj kev:
Txoj kev no yog ib txoj hauv kev rau kev sib txuas DBDMH. Cov kauj ruam yog raws li nram no:
1.1. Npaj anhydrous acetic acid los yog methyl chloride tov:
Hauv cov tshuaj tiv thaiv qhuav, ntxiv qhov tsim nyog ntawm anhydrous acetic acid lossis methyl chloride. Nco ntsoov tias kev xaiv ntawm cov kuab tshuaj anhydrous nyob ntawm qhov kev sim thiab kev ua haujlwm ntawm cov tshuaj tiv thaiv.
1.2. Dissolving urea:
Ntxiv urea maj mam mus rau anhydrous acetic acid los yog methyl chloride kom txog thaum saturation. Kev tawg ntawm urea tuaj yeem ua kom nrawm nrawm los ntawm kev nplawm thiab tswj qhov kev sib cais ntawm qhov kub ntawm 0-5 degrees Celsius.
1.3. Ntxiv kua bromine:
Maj mam thiab tsis tu ncua ntxiv bromine dropwise rau anhydrous acetic acid los yog methyl chloride yaj hauv urea. Qhov zoo tshaj plaws ntxiv tus nqi yog ntxiv bromine rau cov tshuaj tiv thaiv kab mob nyob rau hauv daim ntawv ntawm trickle flow. Nyob rau tib lub sijhawm, khaws qhov ntsuas kub ntawm cov tshuaj tiv thaiv hauv qhov ntau ntawm 0-5 degrees Celsius.
1.4. stirring thiab tuav lub sij hawm ntawm cov tshuaj tiv thaiv sib tov:
Thaum lub sij hawm maj mam ntxiv ntawm bromine rau cov tshuaj tiv thaiv kab mob, qhov sib tov tau maj mam stirred siv ib tug stirrer. Kev sib xyaw ntawm cov tshuaj tiv thaiv sib xyaw tau txuas ntxiv rau 2-4 teev kom paub meej cov tshuaj tiv thaiv txaus.
1.5. Collection ntawm sediment:
Thaum kawg ntawm cov tshuaj tiv thaiv, koj yuav soj ntsuam qhov tsim ntawm cov khoom dawb precipitate hauv cov tshuaj tiv thaiv sib tov, uas yog 1,3-Dibromo-5,5-dimethylhydantoin khoom.
Cov tshuaj tiv thaiv sib tov tau lim siv lub lim dej kom cais cov khoom precipitate.
1.6. Ntxuav cov khoom lag luam:
Cov khoom tsim tau raug ntxuav nrog ethanol txias. Cov kauj ruam no yog tshem tawm cov seem bromine thiab lwm yam impurities.
Txias ethanol tau ntxiv rau cov khoom lag luam, nplawm thiab lim.
Cov kauj ruam ntxuav no tuaj yeem rov ua dua ob peb zaug kom ntseeg tau tias cov khoom siv purity.
1.7. Qhuav thiab purification:
Muab cov khoom ntxuav rau hauv lub tshuab nqus tsev desiccator thiab ziab nws ntawm qhov kub thiab txias. Qhov no tuaj yeem pab tshem tawm cov khoom seem ethanol thiab noo noo, thiab tau txais cov ntshiab 1, 3-Dibromo-5, 5-dimethylhydantoin crystals.
Thaum kawg, koj yuav tau txais cov ntshiab DBDMH crystals.
2. Tetrabromocyclospendine txoj kev:
Txoj kev siv tetrabromocycloclidinone ua raw khoom los ua ke DBDMH. Cov kauj ruam yog raws li nram no:
2.1. Kev npaj Bromocyclopentadienylacetone (DMDHPA):
- Hauv cov tshuaj tiv thaiv kab mob, ntxiv qhov tsim nyog ntawm cyclopentadiene thiab acetone, ntxiv cov catalyst (xws li borane, thiab lwm yam), thiab tau txais DMDHPA los ntawm cua sov thiab reacting. Cov kauj ruam no tuaj yeem ua tau los ntawm txoj kev paub.
2.2. Cov tshuaj tiv thaiv nrog bromine:
- Hauv cov hlab ntsha qhuav, ntxiv DMDHPA thiab bromine.
- Ua kom sov cov tshuaj tiv thaiv rau qhov kub thiab txias (feem ntau yog nyob rau hauv thaj tsam ntawm 60-100 degrees Celsius), thiab do cov tshuaj tiv thaiv sib tov los txhawb cov tshuaj tiv thaiv.
- Thaum lub sij hawm cov tshuaj tiv thaiv, nws tau pom tias bromine reacted nrog DMDHPA los tsim 1, 3-Dibromo-5, 5-dimethylhydantoin.
2.3. cais cov khoom:
- Tom qab cov tshuaj tiv thaiv dhau lawm, cov tshuaj tiv thaiv sib tov yog txias thiab diluted nrog ib qho dej txaus.
- Cov khoom lag luam 1,3-Dibromo-5,5-dimethylhydantoin yuav ua kom nag lossis daus.
- Sib cais thiab sau cov khoom lag luam siv lub tshuab lim.
2.4. Purification thiab ziab:
- Cov khoom ntim khoom tuaj yeem muaj cov impurities uas yuav tsum tau ua kom huv.
- Recrystallization tuaj yeem ua tau siv cov kuab tshuaj xws li diethyl ether lossis chloroform kom tshem tawm cov impurities.
- Lub tshuab nqus tsev kom qhuav cov khoom ntshiab kom tshem tawm cov kuab tshuaj seem thiab cov dej noo kom tau txais cov ntshiab 1, 3-Dibromo-5, 5-dimethylhydantoin.
3. p-toluenesulfonic acid txoj kev:
Txoj kev npaj DBDMH los ntawm reacting p-toluenesulfonic acid thiab hydrobromic acid. Cov kauj ruam yog raws li nram no:
3.1. Kev npaj ntawm 5, 5-dimethylcyclopentadienylacetone (DMDHPA):
- Hauv cov tshuaj tiv thaiv kab mob, ntxiv cov nqi tsim nyog ntawm cyclopentadiene thiab acetone, thiab ntxiv cov catalyst (xws li borane, thiab lwm yam) tib lub sijhawm.
- Cov tshuaj tiv thaiv cyclization yog ua los ntawm cua sov cov tshuaj tiv thaiv los tsim 5, 5-dimethylcyclopentadienylacetone (DMDHPA).
- Cov kauj ruam no tuaj yeem ua tau los ntawm kev paub txog.
3.2. Cov tshuaj tiv thaiv nrog bromine:
- Dissolve p-toluenesulfonic acid nyob rau hauv ib tug txaus npaum li cas ntawm acetonitrile.
- Ntxiv DMDHPA rau cov tshuaj tiv thaiv kab mob thiab maj mam ntxiv bromine dropwise.
- Nws raug nquahu kom ua cov tshuaj tiv thaiv nyob rau hauv kev tswj qhov kub thiab txias, feem ntau nyob rau hauv thaj tsam ntawm 0-10 degrees Celsius.
- Raws li cov tshuaj tiv thaiv tshwm sim, bromine tau pom tias muaj kev cuam tshuam nrog DMDHPA rau daim ntawv 1, 3-Dibromo-5, 5-dimethylhydantoin.
3.3. Kev cais ntawm cov khoom:
- Tom qab cov tshuaj tiv thaiv tiav lawm, dilute cov tshuaj tiv thaiv sib tov, thiab qhov tsim nyog ntawm acetonitrile lossis deionized dej tuaj yeem siv.
- Cov khoom lag luam 1,3-Dibromo-5,5-dimethylhydantoin yuav ua kom nag lossis daus.
- Sib cais thiab sau cov khoom lag luam siv lub tshuab lim.
3.4. Purification thiab ziab:
- Cov khoom ntim khoom tuaj yeem muaj cov impurities uas yuav tsum tau ua kom huv.
- Recrystallization tuaj yeem ua tau siv cov kuab tshuaj xws li diethyl ether lossis chloroform kom tshem tawm cov impurities.
- Lub tshuab nqus tsev kom qhuav cov khoom ntshiab kom tshem tawm cov kuab tshuaj seem thiab cov dej noo kom tau txais cov ntshiab 1, 3-Dibromo-5, 5-dimethylhydantoin.
4. Pyridine txoj kev:
Txoj kev siv pyridine ua raw khoom los ua ke DBDMH. Cov kauj ruam yog raws li nram no:
4.1. Kev npaj ntawm pyridine -2, 4-dicarboxylic acid:
- Hauv cov tshuaj tiv thaiv kab mob, sib tov pyridine thiab formic acid thiab ntxiv catalyst (xws li pyrophosphate triester).
- Cov tshuaj tiv thaiv feem ntau yog nqa tawm ntawm qhov kub siab dua, xws li cov tshuaj tiv thaiv kub.
- Tom qab cov tshuaj tiv thaiv tiav, pyridine -2, 4- dicarboxylic acid tau txais.
4.2. Cov tshuaj tiv thaiv nrog sodium nitrite:
- Dissolve pyridine-2, 4-dicarboxylic acid nyob rau hauv cov kuab tshuaj txaus xws li chloroform.
- Ntxiv qhov tsim nyog ntawm sodium nitrite los kho tus nqi pH.
- Do cov reactants ntawm qhov kub thiab txias.
- Raws li cov tshuaj tiv thaiv tshwm sim, kev tsim cov tshuaj nitrosopyridine tau pom.
4.3. Cov tshuaj tiv thaiv bromination:
- Hloov cov reactants mus rau lwm lub thawv.
- Ntxiv qhov tsim nyog ntawm cuprous bromide (CuBr2) ua catalyst.
- Raws li cov tshuaj tiv thaiv tshwm sim, kev hloov pauv tshuaj tiv thaiv ntawm nitrosopyridine nrog bromine raug pom los tsim cov tshuaj bromopyridine.
4.4. Kev cais ntawm cov khoom:
- Tom qab cov tshuaj tiv thaiv tiav lawm, dilute cov tshuaj tiv thaiv sib tov, thiab qhov tsim nyog ntawm ethyl acetate tuaj yeem siv.
- Kho cov pH, feem ntau nrog sodium bicarbonate (NaHCO3) tov.
- Sib cais cov organic thiab aqueous theem thiab sau cov organic theem.
4.5. Purification thiab ziab:
- Tshem tawm cov kuab tshuaj los ntawm cov txheej txheem organic siv lub evaporator rotary kom tau cov bromopyridine compound.
- Rau kev ua kom huv ntawm bromopyridine, txoj kev xws li recrystallization lossis kem chromatography tuaj yeem siv.
- Lub tshuab nqus tsev kom qhuav cov khoom ntshiab kom tshem tawm cov kuab tshuaj seem thiab cov dej noo kom tau txais cov ntshiab 1, 3-Dibromo-5, 5-dimethylhydantoin.
Cov no yog cov lus piav qhia luv luv ntawm plaub txoj kev siv hluavtaws rau 1,3-Dibromo-5,5-dimethylhydantoin (DBDMH). Thov nco ntsoov tias thaum ua cov tshuaj synthesis cov tshuaj tiv thaiv hauv chav kuaj, koj yuav tsum ua raws li cov txheej txheem kev nyab xeeb ntawm kev sim tshuaj thiab xyuas kom meej tias lawv tau ua raws li qhov tsim nyog. Yog tias koj xav tau cov ntaub ntawv qhia ntxaws ntxaws thiab tshwj xeeb, thov xa mus rau cov ntaub ntawv tshuaj lom neeg thiab cov ntaub ntawv tshaj lij.