Acephate(txuas:https://www.bloomtechz.com/synthetic-chemical/api-researching-only/acephate-powder-cas-30560-19-1.html) yog cov tshuaj tua kab uas muaj keeb kwm ntev ntawm kev siv tshuaj tua kab organic phosphorus. Nws tus yam ntxwv yog hais tias nws yog ib tug endothermic insecticide nrog gastric toxicity thiab tiv tauj tua cov teebmeem, thiab tuaj yeem tua cov qe. Nws muaj cov nyhuv fumigation thiab yog cov tshuaj tua kab qeeb. Nws lub hauv paus ntsiab lus ntawm cov tshuaj tua kab yog inhibiting kab acetylcholine acetate enzyme. Haum rau zaub, haus luam yeeb, txiv hmab txiv ntoo, paj rwb, citrus, mov, thiab nplej, los tiv thaiv thiab tswj ntau yam zom thiab nqus qhov ncauj kab tsuag thiab pythons. Yog tias sib xyaw nrog cov tshuaj tua kab xws li carbaryl thiab dimethoate, nws muaj kev sib koom ua ke thiab tuaj yeem txuas lub txee lub neej.
Txoj Kev 1: Ib txoj hauv kev yooj yim, muaj txiaj ntsig siab, tus nqi qis, thiab kev ua siab dawb huv rau kev npaj acephate; Nws tuaj yeem kov yeej cov txheej txheem neutralization uas yuav tsum tau sib cais ntawm acetic acid, txo qhov kev puas tsuaj ntawm acetylmethylamine los ntawm kev ua kom tsis zoo, thiab tsis tas yuav tsum muaj cov txheej txheem loj ntawm cov organic solvent extraction thiab tsim cov dej khib nyiab ntau. Cov kev daws teeb meem suav nrog cov txheej txheem synthesis hauv qab no:
(1) Siv ethylene ketone thiab O, O-dimethylthiophosphoramide ua raw cov ntaub ntawv, nyob rau hauv cov kev mob ntawm acylation catalyst thiab organic hnyav, ethylene ketone undergoes acetylation cov tshuaj tiv thaiv nrog O, O-dimethylthiophosphoramide kom tau acetylated O, O-dimethylthiophosphoramide; Ntawm lawv, qhov sib piv loj ntawm ethylene ketone rau O, O-dimethylthiophosphoramide yog (015-0.40): 1;
(2) React acetylated O, O-dimethylthiophosphoramide nyob rau hauv isomerization catalyst tej yam kev mob los npaj acetomethamidophos tov;
(3) Acetylmethamidophos tov yog crystallized, solid-kua sib cais, thiab qhuav los npaj Acetylmethamidophos nyoos hmoov.
Cov tshuaj tiv thaiv kab mob sib npaug yog raws li hauv qab no:
Txoj Kev 2:
Cov khoom siv raw rau kev tsim acephate muaj xws li methyl chloride, ammonia, dichloroethane, ethylene glycol, thiab dimethyl sulfate vinegar. Tau los ntawm cov kauj ruam tshuaj tiv thaiv xws li amination, acylation, thiab isomerization.
1. Amination:
Ntxiv methyl chloride thiab sib piv tus nqi ntawm dichloroethane horizontally mus rau hauv lub amination kettle los ntawm qib siab metering, thiab pib lub stirring thiab khov brine. Thaum qhov kub hauv lub lauj kaub poob mus rau 15C, maj mam muab cov dej nitrogen tso rau hauv lub lauj kaub los ntawm qib siab ntsuas lub tank ntawm ammonia dej, thiab tswj qhov kub hauv lub lauj kaub ntawm 35-40 feem pua C rau 35.40 min . Tom qab ntxiv dej ammonia, kho cov brine khov kom txo qhov kub hauv lub lauj kaub rau 20-23C. Khaws qhov kub thiab txias rau 30-35 feeb, tom qab ntawd ntxiv 6L dej. Tom qab stirring rau 2-3 feeb, nres stirring thiab tso cov khoom mus rau hauv lub amination separator rau stratification. Tom qab 30 feeb, tso cov theem ntawm cov organic rau hauv lub tank txais kev ntsuas. Qhov no organic theem yog amine compound nrog hnyav (0.0 dimethyl thiophosphoramide).
2. Acylation:
(1) acetic anhydride txoj kev: Muab cov amine nrog hnyav rau hauv acylation kettle los ntawm qib siab ntsuas tank, pib stirring, ces ntxiv acetic anhydride rau hauv acylation kettle los ntawm qib siab ntsuas tank ntawm acetic anhydride, thiab ces tig rau khov brine. . Thaum qhov kub hauv lub lauj kaub poob rau 10 degree C, maj mam ntxiv cov tshuaj sulfuric acid los ntawm qib siab ntsuas lub tank rau hauv cov tshuaj tiv thaiv hluav taws xob. Tom qab ntxiv sulfuric acid, tig rau cua siab, tso cov brine khov los ntawm lub tsho, thiab maj mam ua kom sov nws nrog chav kom nce qhov kub hauv lub lauj kaub rau 55-60 degree C, tuav cov tshuaj tiv thaiv rau 50 feeb, ua kom tiav cov tshuaj tiv thaiv. , thiab tom qab ntawd txo qhov kub hauv lub lauj kaub rau 10C. Ntxiv chlorine dej dropwise los ntawm cov qib siab tank ntawm ammonia dej kom neutralize cov kua qaub generated los ntawm cov tshuaj tiv thaiv, thiab neutralize nws mus rau tus nqi pH ntawm 7-8. Thaum lub sij hawm neutralization txheej txheem, qhov kub thiab txias yuav tsum tau tswj hauv qab 30 degree C. Tom qab neutralization, cov khoom yuav tsum tau pumped rau hauv ib tug separator rau static sib cais, thiab cov organic theem yuav tsum tau muab cais rau crude acylate cia tank. Tom qab ntawd, nws yuav tsum tau muab tso rau hauv lub tshuab hluav taws xob distillation rau lub tshuab nqus tsev distillation thiab desorption (nqus degree 86.kPa, 70C, 15-20} feeb), Lub acylated compound (0,0-dimethyl-N -yl thiophosphoramide) tau txais.
(2) Acetyl chloride txoj kev: Muab cov amine compound nrog hnyav rau hauv acylation kettle los ntawm qib siab ntsuas tank, pib nplawm, thiab ntxiv acetyl chloride los ntawm qib siab ntsuas tank ntawm ethyl chloride. Tom qab ntawd maj mam nce qhov kub ntawm lub reactor mus rau 50 ° C, tswj qhov kub thiab txias rau 2 teev, thiab hnov mob ntau dua. Txo qhov kub ntawm lub reactor mus rau 10 ° C, thiab tom qab ntawd maj mam ntxiv cov dej nitrogen los ntawm cov dej ammonia qib siab ntsuas lub tank kom tshem tawm cov kua qaub uas tsim los ntawm cov tshuaj tiv thaiv. Neutralize nws mus rau pH tus nqi ntawm 7. Thaum lub sij hawm neutralization txheej txheem, qhov kub thiab txias nyob rau hauv lub reactor yuav tsum tau tswj hauv qab no 30 degree C. Tom qab neutralization, ntxiv ib tug tsim nyog cov dej. Dissolve lub plating ntsev generated thaum lub sij hawm neutralization txheej txheem, do rau 2-3 feeb, thiab rho tawm cov khoom mus rau lub separator rau static sib cais. Cais cov theem qis ntawm cov organic thiab muab rho tawm mus rau hauv lub tshuab hluav taws xob distillation rau lub tshuab nqus tsev desorption (nqus degree 86.7kPa, 70C, 15-20min) kom tau txais cov khoom sib xyaw. Cov tshuaj tiv thaiv acylation siv acetic anhydride lossis acetyl chloride raws li tus neeg sawv cev acylating tuaj yeem ua tiav cov txiaj ntsig zoo.
3. Isomerization:
Muab ntau npaum li cas ntawm cov tshuaj acylated rau hauv isomerization kettle los ntawm qib high-theem metering tank ntawm acylated tshuaj, pib stirring, thiab ces ntxiv dimethyl sulfate vinegar proportionally rau lub isomerization kettle los ntawm high-level metering tank ntawm dimethyl sulfate vinegar. Maj mam nce qhov ntsuas kub mus rau 65-70 degree C, tswj qhov kub thiab txias rau 2 teev, thiab tso tawm kom tau txais acephate crude roj. Rau txhua qhov kev tsim khoom ntawm 1 tuj ntawm 50 feem pua ntawm cov roj crude, cov khoom siv hauv qab no tau noj: 1953 kg ntawm methanol (98 feem pua), 1660 kg ntawm triple phosphate phosphorus (98%), 120 kg ntawm caustic soda (30%), 3220 kg ntawm dimethyl sulfate (98%), 2450 kg ntawm ammonia (18%), 315 kg ntawm sulfur (98 feem pua), 295 kg ntawm acetic acid (98%), 1700 kg ntawm aminated KO (40%), 490 kg ethylene (69%), thiab 250 kg ntawm sulfurized (kev lag luam) dichlorane (98 feem pua).
Txoj Kev 3:
Siv dimethyl thiophosphate chloride ua raw khoom, nyob rau hauv nplawm, amination yog nqa tawm nrog dej ammonia, ua raws li acetylation nrog acetic anhydride. Acetylation yog ua nyob rau hauv lub xub ntiag ntawm sulfuric acid. Thaum lub sij hawm acetylation txheej txheem, ib feem ntawm acetic anhydride yog hloov mus rau hauv acetic acid, uas yog neutralized nrog ammonia. Acetyl chloride tuaj yeem siv los ua tus neeg sawv cev acylating. Tom qab acylation, cov tshuaj yog sab laug kom sawv thiab organically tov nyob rau hauv qis txheej. Tom qab kev sib cais, dimethyl sulfate yog siv rau isomerization, ua raws li lub tshuab nqus tsev distillation los ntxuav cov khoom, lub tshuab nqus tsev concentration, thiab crystallization kom tau acephate.
[1] : Acephate
Txoj Kev 4:
1. Thawj isomerization ua raws li acylation. Ua ntej, nyob rau hauv lub xub ntiag ntawm ib tug me me ntawm dimethyl sulfate, 0, 0-dimethylthiotenamide yog rhuab rau isomerization los tsim O, S-dimethylthiotenamide, uas ces reacts nrog ethylene los yog acetyl chloride los tsim acephate.
2. Ua ntej, acylation ua raws li isomerization cuam tshuam nrog cov tshuaj tiv thaiv ntawm 0, 0-dimethylthioacetamide nrog tus neeg ua haujlwm txias hauv cov kuab tshuaj ntawm di-ethane lossis benzene. Feem ntau siv acylating agents muaj xws li acetic acid ntxiv rau zinc trichloride, vinegar paste, acetyl chloride, vinyl ketone, thiab lwm yam. Cov tshuaj tiv thaiv cua txias generates O, 0-dimethyl-N-ethylthiotenamide, uas yog ces rhuab thiab isomerized rau ethyl methamidophos nyob rau hauv lub muaj ib qho me me ntawm dimethyl sulfate.
3. By using new catalysts and special crystalline solvents, high-purity raw materials can be prepared. The process involves adding 200g of methamidophos crude oil to a reaction flask, stirring and heating to the reaction temperature. Under the action of the catalyst, acylating agent acetic acid is added dropwise, and the reaction temperature is controlled. After dropwise addition, the crude crude oil of methamidophos is incubated for several hours, and then neutralized and extracted to separate the organic and aqueous phases, Organic phase purification of acephate refined crude oil is carried out by adding solvent A and crystal forming additives, slowly stirring, cooling, crystallization, filtration, and rinsing to obtain the finished product. After processing the mother liquor, qualified finished products can be recovered, with a total product yield of>78 feem pua thiab cov ntsiab lus ntawm 298.0 feem pua .