N,N-Dimethylaniline

Iyo inozivikanwawo se dimethyl tiphenylamine, isina ruvara kune yakavheneka yero ine mafuta emvura, ine hwema hunonhuhwirira, nyore kuisa oxidize mumhepo kana pasi pezuva uye kushandisa ze yakasvibiswa. Relative density (20 ℃ / 4 ℃) 0.9555, freezing point 2.0 ℃, boiling point 193 ℃, flash point (opening) 77 ℃, flash point 317 ℃, viscosity (25 ℃) 1.528mpa-4,528D index. . Soluble mu ethanol, ether, chloroform, benzene uye zvimwe organic solvents. Soluble mumhando dzakasiyana-siyana dzeorganic compounds. Kunyungudika zvishoma mumvura. Inobvira uye ichapisa kana moto wakazaruka. Iyo mhute nemhepo zvinogadzira musanganiswa unoputika une muganho unoputika we1.2% ~ 7.0% (vol). Iyo ine muchetura zvakanyanya, uye ine muchetura aniline gasi inoburitswa nekupisa kukuru kwesimba rekuora. Inogona kutorwa kuburikidza neganda uye inokonzera chepfu, LD501410mg/kg, iyo yakanyanya kubvumidzwa yekuisa mumhepo ndeye 5mg/m3.
Kuchengeta nzira
1.Kuchengetedza Kuchengetedza[25] Chengeta muimba yekuchengetera inotonhorera, ine mhepo yakanaka. Ramba kure nemoto nekupisa. Chengetedza mudziyo wakavharwa. Inofanira kuchengetwa zvakasiyana kubva kune acids, halogens, uye makemikari anodyiwa, uye haana kumbosanganiswa. Yakashongedzerwa nemhando dzinoenderana uye huwandu hwemidziyo yekudzimisa moto. Nzvimbo yekuchengetera inofanirwa kuve nemidziyo yekukurumidzira yekurapa inodonha uye yakakodzera pekugara.

2. Gamuchira dhiramu resimbi rakavharwa kurongedza, 180kg padhiramu, uye chengeta munzvimbo inotonhorera uye ine mhepo. Chengetedza uye kutakura maererano nemirairo yezvinhu zvinopisa uye zvine chepfu.
synthesis nzira
1. Inowanikwa nekuita pakati peaniline uye methanol muhupo hwe sulfuric acid pakupisa kwepamusoro uye kudzvinyirira kukuru. Maitiro ekuyerera:1. 790kg ye aniline, 625kg ye methanol, 85kg ye sulfuric acid (ammonium 100%) inowedzerwa mu kettle yekupindura, kudzora tembiricha 210-215 ℃, kumanikidza 3.1MPa, kuita kwe4h, wozosunungura kumanikidza, izvo zvinoiswa kune iyo separator, yakaderedzwa ne30% sodium hydroxide, static, uye yakaderera quaternary ammonium munyu inoparadzaniswa. Zvino pa160 ℃, 0.7-0.9MPa hydrolysis reaction ye3h, zvigadzirwa zvehydrolysis uye yepamusoro peya yemafuta zvinhu zvakasanganiswa nekugezwa mushure mekutsvaira kwechigadzirwa chakapedzwa.

2. Kushandisa methanol uye aniline semidziyo, inogadzirwa nealumina catalyst pasi pemamiriro e200-250 ℃ ine methanol yakawandisa uye kumanikidzwa kwemhepo. The raw material kushandiswa quota: aniline 790kg/t, methanol 625kg/t, sulfuric acid 85kg/t. Kugadzirira murabhoritari kunogona kuita aniline ine trimethyl phosphate.

3, aniline uye methanol yakasanganiswa (n aniline: n methanol ≈ 1: 3), uye kuburikidza neinodzokorora isiri-pulse metering pombi inobaiwa pa 0.5h-1 mhepo yekumhanya mu reactor yakashongedzerwa necatalyst, iyo reaction inobuda kutanga mugirazi. gasi-mvura yekuparadzanisa, inoparadzanisa pasi pemvura inounganidzwa panguva dzenguva dzose inobviswa kuti iongorore chromatographic.

Muna 2001, Nankai University neTianjin Ruikai Technology Development Co., Ltd. vakabatana vakagadzira aniline methylation catalyst inoshanda zvakanyanya, uye vakaziva kuumbwa kwegasi-chikamu cheN, N-dimethyl aniline. Maitiro acho ndeaya anotevera: Liquid aniline inosanganiswa ne methanol, yakanyungudutswa mu vaporization tower, yobva yapinda mune tubular reactor ine air velocity ye 0.5-1.0h-1 (mubhedha wakagadziriswa we tubular reactor wakashongedzerwa nano yakatakura. -solid catalyst), uye inoramba ichigadzirwa pa250-300 ℃ pasi pemhepo yemhepo, ine DMA goho rinopfuura 96%.

Nzira yekunatsa: Inowanzo ine tsvina yakadai seaniline uye N-methyl aniline. N,N-dimethylaniline inonyungudutswa mu40% sulfuric acid uye yakanyungudutswa nemhute yemvura. Sodium hydroxide inowedzerwa kuti iite alkaline. Iyo distillation inoenderera mberi nemhute yemvura. Iyo distillate inoparadzaniswa kuita aqueous layers uye yakaomeswa ne potassium hydroxide. Normal pressure distillation inoitwa pamberi peacetic anhydride. Iyo distillate inoshambidzwa nemvura kuti ibvise acetic anhydride, yakaomeswa ne potassium hydroxide, inoteverwa nebarium oxide, uye inonyungudutswa pasi pekumanikidzwa kwakaderedzwa pamberi perukova rwenitrogen. Dzimwe nzira dzekuchenesa distillate dzinosanganisira kuwedzera 10% acetic anhydride uye refluxing kwemaawa mashomanana kubvisa maamine ekutanga uye echipiri. Mushure mekutonhora, yakawandisa ye20% hydrochloric acid inowedzerwa uye inotorwa ne ether. Iyo hydrochloric acid layer ine alkaline ine alkali uye yobva yatorwa ne ether, uye iyo ether layer inoomeswa ne potassium hydroxide uye inonyungudutswa pasi pekumanikidzwa kwakaderedzwa pasi perukova rwenitrogen. N, N-dimethylaniline inogonawo kushandurwa kuita picric acid munyu, yakadzokororwa kusvika painonyungudika inogara ichinyunguduka yobva yaora nekudziya 10% aqueous solution ye sodium hydroxide. Inobva yabviswa ne ether, yosukwa uye yoomeswa, uye inonyungudutswa pasi pekumanikidzwa kwakaderedzwa.

5. Aniline, methanol uye sulfuric acid yakavhenganiswa muchikamu, condensation reaction mu autoclave, maitiro ekugadzirisa nekudzvinyirira kudzorerwa kwemethanol, kuwedzera alkali neutralization, kuparadzanisa uye ipapo distillation nekuderedza kudzvinyirira kuwana chigadzirwa.

6. N, N-dimethylaniline inogona kugadzirwa nemethylation reaction yeaniline uye trimethyl phosphate, uye inobva yabudiswa ne ether, yakaomeswa uye yakasvibiswa.

7. N,N-dimethylaniline inogona kugadzirwa pamubhedha unobatsira weZiegler catalyst mumhangura-manganese system kana mhangura-zinc-chromium system pa280 ℃ nemusanganiswa weaniline uye methanol pachiyero che1: 3.5. Iyo yakawanikwa N, N-dimethylaniline yakaunganidzwa pa193-195 ℃ pane 54-tab column distillation mudziyo uye yakaiswa mumabhodhoro egirazi rebrown. Kugadzira yakachena N,N-dimethylaniline, iyo N,N-dimethylaniline inogona kubaiwa nenitrogen gasi semutakuri gasi mugadziriro gasi chromatograph iyo ine metal phosphate column.