The Synthesis Of Aromatics And Diethyl Malonate By Catalytic Method And The Gas Chromatography Analysis Of The Products

Gas Chromatograph analysis is one of the most important branches and it plays an important role in organic analytical method. The paper studys chromatograph analy of product in two organic catalytic reactions, it has definite utilitarian value in chromatograph analy of organic product.In the catalytic conversion of methanol to aromatics(MTA), the selectivity of aromatics and BTX (benzene, toluene, and xylene) reached 64.0% and 56.6%, respectively, using La/Zn/HZSM-5 at 437℃, 0.1 MPa and methanol WHSV (weight hourly space velocity=0.8 h^-1). Catalytic results showed that the La species increased selectivity of aromatics, and prolonged the catalyst lifetime on stream. We searched a right analytical method because the kinds of reaction product of MTA were various and analyzing product was diffiduct. The gas phase product was analyzed on-line by a gas chromatograph equipped with a Porapak-Q packed column and a TCD detector, was qualified by standard samples and was quantified by area normalization. The oil phase product and the water phase product were analyzed off-line by a gas chromatograph equipped with a HP-5 capillary column and an Agilent FID detector, were qualified by standard samples and were quantified by internal standard method which heptane and isopropanol were internal standard.In the reaction of synthetize diethyl malonate(DEM), Na[Co(CO)₄] of high catalytic activity was synthetized at 55℃and CO partial pressure of 1.5 MPa, which CoCl₂, Zn, Na₂SO₃ with the determinate molar ratio in the ethanol solvent. The percent conversion of ClCH₂COOC₂H₅ was 96%, the selectivity and yield were 95%, 93% respectively after 2 h in C₂H₅OH solvent at 85℃and CO partial pressure of 2.0 MPa, which ClCH₂COOC₂H₅ was used a substrate, Na₂CO₃ as a alkali, Na[Co(CO)₄] as a catalyst. Chromatograph analytical method of product in carbonylation reaction was studied. The product was analyzed off-line by a gas chromatograph equipped with a HP-5 capillary column and an FID detector, was qualified by standard samples and was quantified by internal standard method which o-xylene was internal standard. The analytical method is simple, analysis time is short and quantitative is accurate.