N,N-Dimethylaniline

Kuj hu ua dimethyl tiphenylamine, tsis muaj xim rau lub teeb daj oily kua, nrog ib tug pungent tsw, yooj yim rau oxidize nyob rau hauv huab cua los yog nyob rau hauv lub hnub thiab siv lub ze darkened. Qhov sib piv ntawm qhov ceev (20 ℃ / 4 ℃) 0.9555, freezing point 2.0 ℃, boiling point 193 ℃, flash point (qhib) 77 ℃, flash point 317 ℃, viscosity (25 ℃) 1.528mpa-s, refractive index (n20D) 1.5584. Yaj nyob rau hauv ethanol, ether, chloroform, benzene thiab lwm yam organic solvents. Yaj nyob rau hauv ntau yam organic compounds. Me ntsis soluble nyob rau hauv dej. Nws yog combustible thiab yuav hlawv nyob rau hauv cov ntaub ntawv ntawm qhib nplaim taws. Lub pa thiab huab cua yuav tsim ib tug tawg sib tov nrog ib tug tawg txwv ntawm 1.2% ~ 7.0% (vol). Nws yog heev lom, thiab lom aniline roj yog tso tawm los ntawm high kub zog decomposition. Nws tuaj yeem nqus tau los ntawm daim tawv nqaij thiab ua rau lom, LD501410mg / kg, qhov siab tshaj plaws tso cai concentration hauv huab cua yog 5mg / m3.
Txoj kev khaws cia
1. Kev Ceev Faj Txog Kev Khaws Cia [25] Khaws cia rau hauv qhov chaw txias thiab muaj cua nkag zoo. Khaws cia kom deb ntawm cov hluav taws thiab cov cua sov. Khaws lub thawv kom kaw. Nws yuav tsum khaws cia cais ntawm cov kua qaub, halogens, thiab cov tshuaj noj tau, thiab tsis txhob sib xyaw. Nruab nrog cov khoom siv tua hluav taws sib xws thiab ntau npaum li cas. Thaj chaw khaws cia yuav tsum tau nruab nrog cov khoom siv kho mob thaum muaj xwm txheej ceev rau cov xau thiab cov ntaub ntawv tiv thaiv tsim nyog.

2. Siv lub thoob hlau ntim khoom kaw, 180kg ib lub thoob, thiab khaws cia rau qhov chaw txias thiab muaj cua nkag. Khaws cia thiab thauj mus los raws li cov cai ntawm cov khoom siv hluav taws xob thiab tshuaj lom.
txoj kev sib xyaw ua ke
1. Nws tau txais los ntawm kev sib xyaw ntawm aniline thiab methanol nyob rau hauv qhov muaj sulfuric acid ntawm qhov kub thiab siab. Cov txheej txheem ntws: 1. 790kg ntawm aniline, 625kg ntawm methanol, 85kg ntawm sulfuric acid (ammonium 100%) raug ntxiv rau hauv lub lauj kaub sib xyaw, tswj qhov kub thiab txias 210-215 ℃, siab 3.1MPa, sib xyaw rau 4 teev, tom qab ntawd tso qhov siab, cov khoom raug tso tawm mus rau lub tshuab cais, neutralized los ntawm 30% sodium hydroxide, static, thiab qis dua quaternary ammonium ntsev raug sib cais. Tom qab ntawd ntawm 160 ℃, 0.7-0.9MPa hydrolysis sib xyaw rau 3 teev, cov khoom hydrolysis thiab cov txheej sab saud ntawm cov khoom siv roj sib xyaw ua ke los ntawm kev ntxuav tom qab nqus tsev distillation ntawm cov khoom tiav.

2. Siv methanol thiab aniline ua cov khoom siv raw, nws yog synthesized los ntawm alumina catalyst nyob rau hauv lub xeev ntawm 200-250 ℃ nrog ntau dhau methanol thiab atmospheric siab. Cov khoom siv raw quota noj: aniline 790kg / t, methanol 625kg / t, sulfuric acid 85kg / t. Kev npaj hauv chav kuaj tuaj yeem cuam tshuam aniline nrog trimethyl phosphate.

3, aniline thiab methanol sib xyaw (n aniline: n methanol ≈ 1: 3), thiab los ntawm lub twj tso kua mis reciprocating non-pulse metering txhaj tshuaj ntawm 0.5h-1 cua ceev rau hauv lub reactor nruab nrog lub catalyst, cov tshuaj tiv thaiv tawm ua ntej mus rau hauv lub iav roj-kua separator, lub separator nyob rau hauv cov kua sau ntawm cov sijhawm tsis tu ncua tshem tawm rau chromatographic kev tshuaj ntsuam.

Xyoo 2001, Nankai University thiab Tianjin Ruikai Technology Development Co., Ltd. tau koom ua ke tsim cov tshuaj catalyst aniline methylation zoo heev, thiab tau pom cov roj-theem synthesis ntawm N, N-dimethyl aniline. Cov txheej txheem yog raws li nram no: Cov kua aniline yog sib xyaw nrog methanol, vaporized hauv lub vaporization tower, thiab tom qab ntawd nkag mus rau hauv lub tubular reactor nrog lub cua ceev ntawm 0.5-1.0h-1 (lub txaj ruaj khov ntawm lub tubular reactor yog nruab nrog cov khoom siv nano-khoom catalyst), thiab tsim tawm tas li ntawm 250-300 ℃ nyob rau hauv atmospheric siab, nrog DMA yield ntawm ntau dua 96%.

Txoj kev ua kom zoo: Nws feem ntau muaj cov khoom tsis huv xws li aniline thiab N-methyl aniline. N,N-dimethylaniline yog yaj rau hauv 40% sulfuric acid thiab distilled los ntawm cov pa dej. Sodium hydroxide yog ntxiv rau kom nws alkaline. Lub distillation yog txuas ntxiv nrog cov pa dej. Lub distillate yog sib cais ua cov txheej aqueous thiab ziab nrog potassium hydroxide. Lub siab ib txwm distillation yog nqa tawm nyob rau hauv lub xub ntiag ntawm acetic anhydride. Lub distillate yog ntxuav nrog dej kom tshem tawm cov cim ntawm acetic anhydride, ziab nrog potassium hydroxide, ua raws li barium oxide, thiab distilled nyob rau hauv lub siab txo qis nyob rau hauv lub xub ntiag ntawm cov kwj deg ntawm nitrogen. Lwm txoj hauv kev ntawm kev ua kom zoo lub distillate suav nrog ntxiv 10% acetic anhydride thiab refluxing rau ob peb teev kom tshem tawm cov thawj thiab theem nrab amines. Tom qab txias, ntau tshaj 20% hydrochloric acid yog ntxiv thiab rho tawm nrog ether. Lub hydrochloric acid txheej yog alkaline nrog alkali thiab tom qab ntawd rho tawm nrog ether, thiab lub ether txheej yog qhuav nrog potassium hydroxide thiab distilled nyob rau hauv lub siab txo qis nyob rau hauv lub kwj deg ntawm nitrogen. N,N-dimethylaniline kuj tseem tuaj yeem hloov mus ua cov ntsev picric acid, recrystallized mus rau qhov chaw yaj tas li thiab tom qab ntawd decomposed nrog cov kua dej sov 10% ntawm sodium hydroxide. Tom qab ntawd nws raug rho tawm nrog ether, ntxuav thiab ziab, thiab distilled nyob rau hauv kev txo qis siab.

5. Aniline, methanol thiab sulfuric acid sib xyaw ua ke, cov tshuaj tiv thaiv condensation hauv autoclave, cov khoom tshuaj tiv thaiv los ntawm kev rov qab los ntawm kev nyem siab ntawm methanol, ntxiv alkali neutralization, kev sib cais thiab tom qab ntawd distillation los ntawm kev txo qis kom tau txais cov khoom.

6. N, N-dimethylaniline tuaj yeem tsim los ntawm cov tshuaj methylation ntawm aniline thiab trimethyl phosphate, thiab tom qab ntawd rho tawm los ntawm ether, ziab thiab distilled.

7. N,N-dimethylaniline tuaj yeem tsim tau rau ntawm lub txaj catalytic ntawm Ziegler catalyst hauv lub cev tooj liab-manganese lossis lub cev tooj liab-zinc-chromium ntawm 280 ℃ nrog rau qhov sib xyaw ntawm aniline thiab methanol ntawm qhov sib piv ntawm 1: 3.5. N,N-dimethylaniline tau txais tau sau ntawm 193-195 ℃ ntawm lub tshuab distillation 54-tab thiab ntim rau hauv lub raj mis iav xim av. Rau kev npaj N,N-dimethylaniline ntshiab, N,N-dimethylaniline tuaj yeem txhaj nrog cov roj nitrogen ua cov roj nqa mus rau hauv cov roj chromatograph uas muaj cov hlau phosphate kem.