N, N-Dimethylaniline

Ikwaziwa ngokuba yi-dimethyl tiphenylamine, engenambala ukuya kulwelo oluneoyile olukhanyayo, olunevumba elinukayo, kulula ukufakwa kwi-oxidize emoyeni okanye phantsi kwelanga kwaye usebenzise i-ze mnyama. Relative density (20 ℃ / 4 ℃) 0.9555, freezing point 2.0 ℃, boiling point 193 ℃, flash point (opening) 77 ℃, flash point 317 ℃, viscosity (25 ℃) 1.528mpa-4,528 index refractive. . Inyibilika kwi ethanol, ether, chloroform, benzene kunye nezinye izinyibilikisi eziphilayo. Inyibilika kwiintlobo ngeentlobo zeekhompawundi eziphilayo. Inyibilika kancinane emanzini. Iyatsha kwaye iya kutsha xa kuthe kwabakho ilangatye elivulekileyo. Umphunga kunye nomoya uya kwenza umxube oqhumayo kunye nomda oqhumayo we-1.2% ~ 7.0% (vol). Inetyhefu kakhulu, kwaye igesi yeaniline eyityhefu ikhutshwa kukubola kwamandla obushushu aphezulu. Inokuthi ifakwe esikhumbeni kwaye ibangele ubuthi, i-LD501410mg / kg, i-concentration ephezulu evumelekileyo emoyeni yi-5mg / m3.
Indlela yokugcina
1.ImiQathango yokuGcina[25] Gcina kwindawo yokugcina epholileyo, nengena umoya. Zigcine kude nomlilo kunye nemithombo yobushushu. Gcina isitya sivaliwe. Kufuneka igcinwe ngokwahlukileyo kwi-asidi, i-halogens, kunye neekhemikhali ezidliwayo, kwaye ingaxutywanga. Ukuxhotyiswa ngeentlobo ezihambelanayo kunye nobuninzi bezixhobo zokucima umlilo. Indawo yokugcina kufuneka ixhotyiswe ngezixhobo zonyango olungxamisekileyo lokuvuza kunye nezixhobo ezifanelekileyo zokukhusela.

2. Yamkela igubu lentsimbi elitywiniweyo elipakishiweyo, i-180kg ngegubu ngalinye, kwaye uligcine kwindawo epholileyo nengena umoya. Gcina kwaye uhambise ngokwemigaqo yezinto ezinokutsha kunye netyhefu.
indlela yokuhlanganisa
1. Ifunyenwe ngokusabela phakathi kwe-aniline kunye ne-methanol phambi kwe-sulfuric acid kwiqondo lokushisa eliphezulu kunye noxinzelelo oluphezulu. Ukuhamba kwenkqubo:1. I-790kg ye-aniline, i-625kg ye-methanol, i-85kg ye-sulfuric acid (i-ammonium 100%) yongezwa kwi-kettle yokusabela, ubushushu bokulawula i-210-215 ℃, uxinzelelo lwe-3.1MPa, i-react for 4h, emva koko ikhulule uxinzelelo, izinto zikhutshwe i-separator, ingathathi hlangothi nge-30% ye-sodium hydroxide, i-static, kunye ne-quaternary ammonium ityuwa ephantsi iyahlukana. Emva koko kwi-160 ℃, i-0.7-0.9MPa i-hydrolysis reaction ye-3h, iimveliso ze-hydrolysis kunye nomgangatho ophezulu wezinto ezinamafutha ezidityaniswe ngokuhlamba emva kwe-vacuum distillation yemveliso egqityiweyo.

2. Ukusebenzisa i-methanol kunye ne-aniline njengezinto eziluhlaza, zenziwe nge-alumina catalyst phantsi kwemeko ye-200-250 ℃ kunye ne-methanol engaphezulu kunye noxinzelelo lwe-atmospheric. I-quota yokusetyenziswa kwezinto ekrwada: i-aniline 790kg / t, i-methanol 625kg / t, i-sulfuric acid 85kg / t. Amalungiselelo aselebhu anokusabela i-aniline nge-trimethyl phosphate.

I-3, i-aniline kunye ne-methanol ixutywe (n aniline: n methanol ≈ 1: 3), kunye nepompo yokulinganisa i-non-pulse metering efakwe kwi-0.5h-1 yesantya somoya kwi-reactor exhotywe nge-catalyst, ukuphuma kwe-reaction kuqala kwiglasi. isahluli segesi-ulwelo, isahluli phantsi kolwelo oluqokelelwe ngamaxesha aqhelekileyo asuswe kuhlalutyo lwechromatographic.

Kwi-2001, iYunivesithi yaseNankai kunye ne-Tianjin Ruikai Technology Development Co., Ltd. ngokudibeneyo baphuhlise i-aniline methylation catalyst esebenzayo kakhulu, kwaye baqaphela i-gas-phase synthesis ye-N, N-dimethyl aniline. Inkqubo imi ngolu hlobo lulandelayo: I-aniline yolwelo ixutywe kunye ne-methanol, i-vaporized tower to vaporization, ize ingene kwi-reactor ye-tubular enesantya somoya se-0.5-1.0h-1 (ibhedi esisigxina ye-reactor tubular ixhotyiswe nge-nano elayishiwe. -i-catalyst eqinile), kwaye iveliswe ngokuqhubekayo kwi-250-300 ℃ phantsi koxinzelelo lwe-atmospheric, kunye nesivuno se-DMA esingaphezu kwe-96%.

Indlela yokucoca: Ihlala iqulethe ukungcola okufana ne-aniline kunye ne-N-methyl aniline. I-N, i-N-dimethylaniline ichithwa kwi-40% ye-asidi ye-sulfuric kwaye idilizwe ngumphunga wamanzi. I-sodium hydroxide yongezwa ukuyenza i-alkaline. Idistillation iqhutyelwe ngomphunga wamanzi. I-distillate iyahlukana ibe ngamanqanaba amanzi kwaye yomiswe nge-potassium hydroxide. Uxinzelelo oluqhelekileyo lwe-distillation lwenziwa phambi kwe-acetic anhydride. I-distillate ihlanjwe ngamanzi ukuze isuse i-acetic anhydride, yomiswe nge-potassium hydroxide, ilandelwa yi-barium oxide, kwaye ihlanjwe phantsi koxinzelelo oluncitshisiweyo phambi komlambo we-nitrogen. Ezinye iindlela zokucoca i-distillate ziquka ukongeza i-10% ye-acetic anhydride kunye ne-refluxing kwiiyure ezimbalwa ukususa ii-amine eziphambili kunye nesekondari. Emva kokupholisa, ukugqithisa kwe-20% ye-hydrochloric acid yongezwa kwaye ikhutshwe nge-ether. I-hydrochloric acid layer i-alkaline kunye ne-alkali kwaye ikhutshwe nge-ether, kwaye i-ether layer yomiswa nge-potassium hydroxide kwaye idilizwe phantsi koxinzelelo oluncitshisiweyo phantsi komlambo we-nitrogen. I-N, i-N-dimethylaniline ingaphinda iguqulwe ibe yi-picric acid salts, iphinde ihlaziywe kwindawo yokunyibilika rhoqo kwaye idibaniswe nesisombululo esifudumeleyo se-10% se-sodium hydroxide. Emva koko ikhutshwe nge-ether, ihlanjwe kwaye yomiswe, kwaye ikhutshwe phantsi koxinzelelo oluncitshisiweyo.

5. I-Aniline, i-methanol kunye ne-asidi ye-sulfuric exutywe ngokulinganayo, ukuphendulwa kwe-condensation kwi-autoclave, iimveliso zokusabela ngokubuyiswa koxinzelelo lwe-methanol, yongeza i-alkali neutralization, ukuhlukana kunye nokuchithwa kwe-distillation ngokunciphisa uxinzelelo lokufumana imveliso.

6. I-N, i-N-dimethylaniline inokuveliswa ngokuphendula kwe-methylation ye-aniline kunye ne-trimethyl phosphate, kwaye ikhutshwe nge-ether, yomisiwe kwaye idilizwe.

7. I-N, N-dimethylaniline inokwenziwa kwi-catalytic bed ye-Ziegler catalyst kwi-copper-manganese system okanye i-copper-zinc-chromium system kwi-280℃ kunye nomxube we-aniline kunye ne-methanol kwi-1: 3.5. I-N, N-dimethylaniline efunyenweyo yaqokelelwa kwi-193-195 ℃ kwisixhobo se-54-tab ye-distillation kwaye ifakwe kwiibhotile zeglasi ezimdaka. Ukulungiselela i-N, i-N-dimethylaniline ecocekileyo, i-N, i-N-dimethylaniline inokutofwa ngegesi ye-nitrogen njenge-carrier gesi kwi-chromatograph yegesi yokulungisa enekholomu ye-metal phosphate.