I-N,N-Dimethylaniline

Yaziwa nangokuthi i-dimethyl tiphenylamine, uketshezi olunamafutha olungenambala kuya koluphuzi olukhanyayo, olunephunga elimnandi, okulula ukuluxuba emoyeni noma ngaphansi kwelanga futhi lusebenzise i-ze darkned. Ubuningi obuhlobene (20 ℃ / 4 ℃) 0.9555, iphuzu lokuqandisa 2.0 ℃, iphuzu lokubila 193 ℃, iphuzu lokugqama (ukuvula) 77 ℃, iphuzu lokugqama 317 ℃, i-viscosity (25 ℃) 1.528mpa-s, i-refractive index (n20D) 1.5584. Incibilika ku-ethanol, i-ether, i-chloroform, i-benzene kanye nezinye izinyibilikisi eziphilayo. Incibilika ezinhlobonhlobo zamakhemikhali e-organic. Incibilika kancane emanzini. Iyasha futhi izosha uma ilangabi livulekile. Umhwamuko nomoya kuzokwakha ingxube eqhumayo enomkhawulo wokuqhuma ongu-1.2% ~ 7.0% (vol). Inobuthi obukhulu, futhi igesi ye-aniline enobuthi ikhishwa ngokubola kwamandla okushisa aphezulu. Ingamuncwa ngesikhumba futhi ibangele ubuthi, i-LD501410mg/kg, izinga eliphezulu elivunyelwe emoyeni lingu-5mg/m3.
Indlela yokugcina
1. Izinyathelo Zokuqapha[25] Gcina endaweni yokugcina epholile, enomoya omuhle. Gcina kude nomlilo kanye nemithombo yokushisa. Gcina isitsha sivaliwe. Kufanele sigcinwe ngokwehlukana nama-acid, ama-halogen, namakhemikhali adliwayo, futhi singalokothi sixutshwe. Sihlonyiswe ngezinhlobo ezifanele kanye nenani lemishini yokulwa nomlilo. Indawo yokugcina kufanele ifakwe imishini yokwelapha ephuthumayo yokuvuza kanye nezinto zokukhosela ezifanele.

2. Sebenzisa ukupakisha okuvalwe nge-iron drum, okungama-180kg nge-drum ngayinye, bese ugcina endaweni epholile nengena umoya. Gcina futhi uthuthe ngokwemithetho yezinto ezivuthayo nezinobuthi.
indlela yokuhlanganisa
1. Itholakala ngokusabela phakathi kwe-aniline ne-methanol lapho kukhona i-sulfuric acid ekushiseni okuphezulu kanye nokucindezela okuphezulu. Ukugeleza kwenqubo: 1. Ama-790kg e-aniline, ama-625kg e-methanol, ama-85kg e-sulfuric acid (i-ammonium 100%) afakwa eketheni lokusabela, izinga lokushisa lokulawula lingu-210-215℃, ingcindezi ingu-3.1MPa, isabela amahora ama-4, bese ikhulula ingcindezi, izinto zikhishwa ziye kusihlukanisi, zisuswe yi-30% ye-sodium hydroxide, i-static, bese kuhlukaniswa usawoti we-ammonium ophansi we-quaternary. Bese kuthi ku-160 ℃, i-0.7-0.9MPa isabela nge-hydrolysis amahora ama-3, imikhiqizo ye-hydrolysis kanye nongqimba olungaphezulu lwezinto ezinamafutha kuhlanganiswe ngokugeza ngemva kokucwiliswa kwe-vacuum komkhiqizo oqediwe.

2. Ukusebenzisa i-methanol ne-aniline njengezinto zokusetshenziswa, kuhlanganiswa yi-alumina catalyst ngaphansi kwesimo esingu-200-250℃ nge-methanol eyengeziwe kanye nomfutho womoya. Isilinganiso sokusetshenziswa kwezinto zokusetshenziswa: i-aniline 790kg/t, i-methanol 625kg/t, i-sulfuric acid 85kg/t. Ukulungiswa kwelabhorethri kungasabela ku-aniline nge-trimethyl phosphate.

3, i-aniline ne-methanol kuxutshwe (i-aniline: n methanol ≈ 1:3), futhi ngephampu yokulinganisa engashayi i-pulse ephindaphindayo ifakwa ngesivinini somoya esingu-0.5h-1 ku-reactor efakwe i-catalyst, ukuphuma kokusabela kuqala ku-glass gas-liquid separator, i-separator ngaphansi koketshezi oluqoqwe ngezikhathi ezijwayelekile isuswe ukuze kuhlaziywe i-chromatographic.

Ngo-2001, iNankai University kanye neTianjin Ruikai Technology Development Co., Ltd. bakha ngokubambisana i-aniline methylation catalyst esebenza kahle kakhulu, futhi baqaphela ukwakheka kwe-gas-phase ye-N,N-dimethyl aniline. Inqubo imi kanje: I-aniline ewuketshezi ixutshwa ne-methanol, ifuthwe embhoshongweni wokufutha, bese ifakwa kwi-tubular reactor enejubane lomoya elingu-0.5-1.0h-1 (umbhede oqinile we-tubular reactor ifakwe i-nano-solid catalyst elayishiwe), futhi ikhiqizwa njalo ku-250-300℃ ngaphansi kwengcindezi yomoya, nge-DMA ephumayo engaphezu kuka-96%.

Indlela yokucwenga: Ivame ukuqukethe ukungcola okufana ne-aniline kanye ne-N-methyl aniline. I-N,N-dimethylaniline incibilikiswa ku-40% sulfuric acid bese ihluzwa ngumhwamuko wamanzi. I-sodium hydroxide iyengezwa ukuze ibe yi-alkaline. Ukuhluzwa kuyaqhubeka nomhwamuko wamanzi. I-distillate ihlukaniswa ibe yizingqimba zamanzi bese yomiswa nge-potassium hydroxide. Ukuhluzwa okuvamile kwengcindezi kwenziwa lapho kukhona i-acetic anhydride. I-distillate igezwa ngamanzi ukuze kususwe iminonjana ye-acetic anhydride, yomiswe nge-potassium hydroxide, kulandelwe yi-barium oxide, bese ihluzwa ngaphansi kwengcindezi encishisiwe lapho kukhona umsinga we-nitrogen. Ezinye izindlela zokuhluza i-distillate zifaka phakathi ukwengeza i-acetic anhydride engu-10% kanye nokuhluzwa amahora ambalwa ukuze kususwe ama-amine ayinhloko nawesibili. Ngemva kokupholisa, kufakwe i-hydrochloric acid engaphezu kuka-20% bese kukhishwa nge-ether. Ingqimba ye-hydrochloric acid iyi-alkaline ene-alkali bese ikhishwa nge-ether, bese ungqimba lwe-ether lomiswa nge-potassium hydroxide bese luhluzwa ngaphansi kwengcindezi encishisiwe ngaphansi komsinga we-nitrogen. I-N,N-dimethylaniline ingaguqulwa ibe usawoti we-picric acid, iphinde isetshenziswe endaweni yokuncibilika engaguquki bese ibola ngesisombululo samanzi esifudumele esingu-10% se-sodium hydroxide. Bese ikhishwa nge-ether, igezwe futhi yomiswe, bese ihluzwa ngaphansi kwengcindezi encishisiwe.

5. I-Aniline, i-methanol kanye ne-sulfuric acid kuxutshwe ngokulingana, ukusabela kokujiya ku-autoclave, imikhiqizo yokusabela ngokukhululwa kwengcindezi ye-methanol, engeza ukungathathi hlangothi kwe-alkali, ukuhlukaniswa bese kuba ukuhluzwa ngokucindezela okuncishisiwe ukuze kutholakale umkhiqizo.

6. I-N,N-dimethylaniline ingadalwa ukusabela kwe-methylation kwe-aniline ne-trimethyl phosphate, bese ikhishwa yi-ether, yomiswe futhi ihluzwe.

7. I-N,N-dimethylaniline ingakhiwa embhedeni we-catalytic we-Ziegler catalyst ohlelweni lwe-copper-manganese noma uhlelo lwe-copper-zinc-chromium ku-280℃ ngengxube ye-aniline ne-methanol ngesilinganiso esingu-1:3.5. I-N,N-dimethylaniline etholiwe yaqoqwa ku-193-195℃ kudivayisi yokucwilisa ikholomu enamathebhu angu-54 futhi yafakwa emabhodleleni engilazi ansundu. Ukuze kulungiselelwe i-N,N-dimethylaniline emsulwa, i-N,N-dimethylaniline ingafakwa ngegesi ye-nitrogen njengegesi yokuthwala ku-chromatograph yegesi yokulungiselela enekholomu ye-phosphate yensimbi.