N,N-Dimethylaniline

Eyaziwa nangokuthi i-dimethyl tiphenylamine, uketshezi olunamafutha angenambala kuya kokuphuzi okhanyayo, olunephunga elimnandi, ukufakwa kalula emoyeni emoyeni noma ngaphansi kwelanga nokusebenzisa okuthi ze mnyama. Ukuminyana okuhlobene (20 ℃ / 4 ℃) 0.9555, iphoyinti eliqandayo 2.0 ℃, iphoyinti abilayo 193 ℃, iphoyinti elikhanyayo (ukuvulwa) 77 ℃, iphoyinti elikhanyayo 317 ℃, i-viscosity (25 ℃) 1.sn528mpa inkomba 4,528mpa . Incibilika ku-ethanol, ether, chloroform, benzene nezinye izinyibilikisi eziphilayo. I-Soluble kuma-organic compounds ahlukahlukene. Incibilika kancane emanzini. Iyasha futhi izosha uma kuba nelangabi elivulekile. Umhwamuko nomoya kuzokwakha ingxube eqhumayo enomkhawulo wokuqhuma ongu-1.2%~7.0% (vol). Inobuthi obukhulu, futhi igesi ye-aniline enobuthi ikhishwa ukubola kwamandla okushisa aphezulu. Ingamuncwa esikhumbeni futhi ibangele ubuthi, LD501410mg/kg, ukugxila okuphezulu okuvunyelwe emoyeni ngu-5mg/m3.
Indlela yokugcina
1.Izinyathelo Zokuqaphela Isitoreji[25] Gcina endaweni yokugcina impahla epholile, enomoya omuhle. Gcina kude nomlilo nemithombo yokushisa. Gcina isitsha sivaliwe. Kufanele igcinwe ngokuhlukana nama-acids, ama-halogen, namakhemikhali adliwayo, futhi ingalokothi ixutshwe. Ifakwe izinhlobo ezihambisanayo kanye nenani lemishini yokucisha umlilo. Indawo yokugcina kufanele ifakwe izinto zokwelashwa eziphuthumayo zokuvuza nezinto zokukhosela ezifanele.

2. Faka isigubhu sensimbi esivaliwe, 180kg isigubhu ngasinye, bese usigcina endaweni epholile nengena umoya. Gcina futhi uthuthe ngokuvumelana nemithethonqubo yezinto ezivuthayo nezinobuthi.
indlela yokuhlanganisa
1. Itholakala ngokusabela phakathi kwe-aniline ne-methanol phambi kwe-sulfuric acid ekushiseni okuphezulu nokucindezela okukhulu. Ukugeleza kwenqubo:1. I-790kg ye-aniline, i-625kg ye-methanol, i-85kg ye-sulfuric acid (i-ammonium 100%) yengezwa kugedlela lokusabela, izinga lokushisa lokulawula 210-215 ℃, ingcindezi engu-3.1MPa, isabela i-4h, bese ikhulula ingcindezi, impahla ikhishwa ku- isihlukanisi, esincishiswe ngo-30% i-sodium hydroxide, i-static, kanye nosawoti ophansi we-quaternary ammonium uhlukaniswa. Bese kuthi ku-160 ℃, 0.7-0.9MPa hydrolysis reaction for 3h, imikhiqizo ye-hydrolysis kanye nongqimba olungaphezulu lwezinto ezinamafutha kuhlanganiswe ngokuwashwa ngemuva kokukhishwa kwe-vacuum distillation yomkhiqizo oqediwe.

2. Ukusebenzisa i-methanol ne-aniline njengezinto zokusetshenziswa, ihlanganiswa yi-alumina catalyst ngaphansi kwesimo esingu-200-250℃ nge-methanol eyeqile kanye nokucindezela komkhathi. I-quota yokusetshenziswa kwempahla eluhlaza: i-aniline 790kg/t, i-methanol 625kg/t, i-sulfuric acid 85kg/t. Amalungiselelo aselabhorethri angasabela i-aniline ne-trimethyl phosphate.

3, i-aniline ne-methanol kuxutshwe (n aniline: n methanol ≈ 1:3), futhi ngokusebenzisa iphampu yemitha ye-non-pulse ephindaphindayo ejovwe ngesivinini somoya esingu-0.5h-1 kureactor efakwe i-catalyst, ukuphuma kokusabela kuqala engilazini. isihlukanisi esiwuketshezi lwegesi, isihlukanisi esingaphansi koketshezi oluqoqwe ngezikhathi ezithile sikhishiwe ukuze kuhlaziywe i-chromatographic.

Ngo-2001, i-Nankai University kanye ne-Tianjin Ruikai Technology Development Co., Ltd. ngokuhlanganyela bakha i-aniline methylation catalyst esebenza kahle kakhulu, futhi baqaphela ukuhlanganiswa kwesigaba segesi se-N,N-dimethyl aniline. Inqubo imi kanje: I-aniline ewuketshezi ixutshwa ne-methanol, ifakwe umhwamuko embhoshongweni wokuhwamuka, bese ingena esikhunjeni esineshubhu esinesivinini somoya esingu-0.5-1.0h-1 (umbhede ongashintshi we-reactor ye-tubular ifakwe nano elayishiwe. -i-solid catalyst), futhi ikhiqizwa ngokuqhubekayo ku-250-300℃ ngaphansi kwengcindezi yasemkhathini, ngesivuno se-DMA esingaphezu kuka-96%.

Indlela yokucwenga: Ivamise ukuqukatha ukungcola okufana ne-aniline ne-N-methyl aniline. I-N,N-dimethylaniline incibilika ku-40% we-sulfuric acid futhi igaywe ngumhwamuko wamanzi. I-sodium hydroxide yengezwa ukuze ibe ne-alkaline. I-distillation iqhutshwa ngomhwamuko wamanzi. I-distillate ihlukaniswa ibe yizingqimba ezinamanzi futhi yomiswe nge-potassium hydroxide. I-distillation yengcindezi evamile yenziwa phambi kwe-acetic anhydride. I-distillate igezwa ngamanzi ukuze isuse iminonjana ye-acetic anhydride, yomiswe nge-potassium hydroxide, ilandelwe yi-barium oxide, futhi ihlanjululwe ngaphansi kwengcindezi encishisiwe phambi komfudlana we-nitrogen. Ezinye izindlela zokucwenga i-distillate zihlanganisa ukungeza i-acetic anhydride engu-10% kanye ne-refluxing amahora ambalwa ukuze kukhishwe ama-amine ayisisekelo nesesibili. Ngemuva kokupholisa, i-hydrochloric acid engaphezu kuka-20% yengezwa futhi ikhishwe nge-ether. Ungqimba lwe-hydrochloric acid luyi-alkaline ne-alkali bese lukhishwa nge-ether, futhi ungqimba lwe-ether lomiswa nge-potassium hydroxide futhi luhlakazwe ngaphansi kwengcindezi encishisiwe ngaphansi komfudlana we-nitrogen. I-N,N-dimethylaniline ingabuye iguqulelwe kusawoti we-picric acid, iphinde ikhiqizwe endaweni encibilikayo engashintshi bese iboliswa ngesixazululo esinamanzi esingu-10% se-sodium hydroxide. Khona-ke ikhishwa nge-ether, igezwe futhi yomiswe, futhi ihlanjululwe ngaphansi kwengcindezi encishisiwe.

5. I-Aniline, i-methanol ne-sulfuric acid exutshwe ngokulingana, ukusabela kwe-condensation ku-autoclave, imikhiqizo yokusabela ngokubuyiswa kwengcindezi ye-methanol, engeza ukungathathi hlangothi kwe-alkali, ukuhlukanisa bese u-distillation ngokunciphisa ingcindezi yokuthola umkhiqizo.

6. I-N,N-dimethylaniline ingakhiqizwa ukusabela kwe-methylation ye-aniline ne-trimethyl phosphate, bese ikhishwa nge-ether, yomisiwe futhi i-distilled.

7. I-N,N-dimethylaniline ingahlanganiswa kumbhede we-catalytic we-Ziegler catalyst ohlelweni lwe-copper-manganese noma isistimu ye-copper-zinc-chromium engu-280℃ ngengxube ye-aniline ne-methanol ngesilinganiso esingu-1:3.5. I-N,N-dimethylaniline etholiwe yaqoqwa ku-193-195℃ emshinini wokucwilisa ikholomu wamathebhu angama-54 futhi yapakishwa emabhodleleni engilazi ansundu. Ukuze kulungiswe i-N,N-dimethylaniline emsulwa, i-N,N-dimethylaniline ingajovwa ngegesi ye-nitrogen njengegesi yokuthwala ku-chromatograph yegesi yokulungisa enekholomu ye-phosphate yensimbi.