2,6-二异丙基萘液相氧化制2,6-萘二甲酸催化条件的研究

<title>udy on Liquid Phase Catalytic Oxidation of 2,6-Diisopropylnaphthalene to 2,6- Naphthalenedicarboxylic Acid

在半连续搅拌釜中,以乙酸钴、乙酸锰、溴化钾和乙酸钾为催化剂,研究了2,6-二异丙基萘(2,6-DIPN)液相空气氧化制2,6-萘二甲酸的过程。通过红外光谱、测酸值和高效液相色谱法对所得固体产物进行定性分析,确认产物为2,6-萘二甲酸。采用反相高效液相色谱法分析不同催化条件下2,6-萘二甲酸的收率和纯度,确定了n(Co+Mn)／n(HAc),n(Co)／n(Co+Mn),n(Br)／n(Co+Mn),n(Co+Mn)／n(2,6-DIPN)和n(K+)／n(Co+Mn)对反应的影响,从而得到了反应适合的催化条件。在此催化条件下,当反应压力3.0 MPa、温度170℃、体系水含量(质量分数)7％和n(O2)／n(2,6-DIPN)=53.6时,2,6-萘二甲酸的收率和纯度分别为73.3％和98.3％。

<abstract>quid phase oxidation of 2,6-diisopropylnaphthalene(DIPN) with air in presence of cobalt acetate, manganese acetate,potassium bromide and potassium acetate to prepare 2,6-naphthalenedicarboxylic acid (2,6 -NDCA) was studied in a semi-continuous stirred tank reactor. The solid product was determined to be 2,6-NDCA by acid value titration.IR spectrometric,and liquid chromatographyic analysis. Yield and purity of 2,6-NDCA were analyzed by using high performance liquid chromatography to investigate the effects of n (Co + Mn)/n(HAc),n(Co)/n(Co+Mn),n(Br)/n(Co+Mn),n(Co+Mn)/n(2,6-DIPN) and n(K+)/n(Co + Mn) on reaction,and settled optimum catalytic conditions. When reaction proceeded at 3.0 MPa,170 ℃ with a ratio of n(O2)/n(DIPN) being 53.6 and 7% water in the system,the yield and purity of 2,6-NDCA were 73. 3% and 98.3% ,respectively.