改性钨酸铵上歧化松香腈的制备与鉴定  

Preparation and identification of the disproportionated rosin nitrile on modified ammonium tungstate

作　　者：陈芳[1] 韦小杰[1] 陈小鹏[1] 罗雪霞[1] 

机构地区：[1]广西大学化学化工学院,广西南宁530004

出　　处：《广西大学学报（自然科学版）》2010年第3期405-409,共5页Journal of Guangxi University（Natural Science Edition）

基　　金：国家自然科学基金项目(20976031);广西自然科学基金项目(0991030;064001);广西教育厅科研基金项目(20070ZL014;20070ZL015);广西大学科研基金项目(X081020)

摘　　要：以自制改性钨酸铵为催化剂、歧化松香和氨气为原料,在高压釜内经氨化脱水制备歧化松香腈。以反应产物的酸值和折光率为指标,判断反应是否完全;采用气相色谱-质谱联用技术(GC-MS)和傅立叶红外光谱(FT-IR)对反应产物进行了分析鉴定。结果表明,改性钨酸铵上歧化松香氨化反应产物的酸值为1.05 mg KOH.g-1,折射率为1.533 7(ND20),说明氨化反应完全;GC-MS分析共分离出9个峰,鉴定出9种化合物,其中主要产物为脱氢枞腈和8-二氢枞腈,其质量分数分别为63.17%和13.39%;质谱分析证明存在有分子量为281的歧化松香腈的碎片;FT-IR分析显示,在2 230 cm-1处有腈的特征峰—C≡N。Disproportionated rosin nitrile was prepared in autoclave with disproportionated rosin and ammonia as raw material and modified ammonium tungstate as catalyst.The acid value and refractive index of reaction products were used as indicators to determine the reaction extent. Products were analyzed by chromatography and gas chromatography-mass spectrometry system（GC-MS） and fourier infrared spectrophotometry（FT-IR）.The results showed that the acid value of the product was 1.05 mg KOH·g-1,the refractive index of product was 1.533 7（ND20）,indicating that the amination reaction were completely.Nine peaks were separated and 9 compounds were tentatively identified by GC-MS.The main products were dehydroabietic nitrile and 8-dihydro-abietic nitrile,with the mass fraction of 63.17% and 13.39%.Debris of disproportionated rosin nitrile with molecular weight of 281 was idantified by MS analysis.As a result of FT-IR,A characteristic peak（—C≡N） of nitrile in 2 230 cm-1 was idantified by FT-IR.

关 键 词：改性钨酸铵 歧化松香 歧化松香腈 氨化 

分 类 号：TQ351.47[化学工程]