Synthesis And Analysis Of 2-tert-amyl Anthraquinone

2–tert-amylanthraquinone as a carrier in the process of hydrogen peroxide production plays an important role and broad application prospects.This article is mainly for synthesis of 2–tert-amylanthraquinone,and create a new synthetic route. Research work is mainly around the following three aspects:The synthesis of tert-amyl benzene: tert-amyl alcohol and benzene by the molar ratio of 1:9 join reaction system, and then under the catalysis of aluminium trichloride proceed Friedel- Crafts alkylation reaction, after the reaction finished, extract with benzene, after vacuum distillation get tertiary amyl benzene.The experimental results show that: when n(AlCl3) : n(C6H6) = 1:9, reaction temperature 6-8℃, reaction time is 4 to 5 h, n(AlCl3) : n(tert-amyl alcohol) = 1:0. 8, the average yield of tert-amyl benzene can reach 79.61%(with benzene).The synthesis of 2-(4’-tert-amyl benzoyl) benzoic acid: phthalic anhydride, aluminium chloride, triethylamine and chlorobenzene was added in the reaction system in turn, and mixed evenly, then add to the system of tertiary amyl benzene, control temperature 15 ℃,under 5 h reaction product 2-(4’–tert-amyl benzoyl) benzoic acid.The experimental results show that: when n(AlCl3) : n(tert-amyl alcohol) = 1:0. 9, n(phthalic anhydride) : n(C6H5Cl) =1:13,T= 15℃, reaction time was 5 h, the yield of 2-(4’-tert amyl benzoyl) benzoic acid can reach 80.36%(with tert-amyl benzene).The synthesis of 2-tert-amylanthraquinone: First, 2-(4’-tert-amyl benzene formyl) benzoic acid dissolved in chloroform was added to the reaction system, and then at a constant temperature,concentrated sulfuric acid was added dropwise to the reaction system, then the reaction temperature was raised to 110°C.After 2h stopped the reaction and got 2-tert-amylanthraxquinone. The results show that: when n(H2SO4): n(ABB acid)=50:1,reaction temperature 110℃,reaction time 2h, 2-tert-amylanthraquinone yield up to 82.5% on average.Qualitative and Quantitative analysis of 2-tert-amylanthraquinone and tert-amyl benzene: 2-tert-amylanthraquinone has strong UV absorption, and therefore high performance liquid chromatography was used to the qualitative and quantitative analysis of 2-tert-amylanthraquinone. Experiment to determine the chromatographic conditions: Agilent1200 high performance liquid chromatography, HC-C18 column(250nm × 4.6mm, 5μm), UV detector(255nm), the mobile phase(V(CH3OH): V(H2O) = 80: 20) rate of 1.0 m L/min, the column temperature was 35 ℃, the injection volume 5μL.Gas chromatography was used to the qualitative and quantitative analysis of tert-amyl benzene. Experiment to determine the chromatographic conditions: Agilent7890 A GC, HT-5 column(30m×0.32nm×0.25μm), two temperature programmed(initial temperature: 40 ℃, 10 ℃ / min to 100 ℃, constant temperature 4min; 20 ℃ / min to 200 ℃, constant temperature 10min), carrier gas flow rate 60 m L / min, FID detector(380 ℃), the injection volume 1.0μL.