To expedite the development of industrial technology for producing 2-alkylanthraquinone,a novel pilot test of alkylation-oxidation technology was conducted.The process mainly included anthracene alkylation,separation ...To expedite the development of industrial technology for producing 2-alkylanthraquinone,a novel pilot test of alkylation-oxidation technology was conducted.The process mainly included anthracene alkylation,separation of anthracene and 2-alkylanthracene,oxidation of 2-alkylanthracene,and product purification.Optimal alkylation conditions yielded a 91.1%conversion of anthracene and a 71.73%selectivity for 2-alkylanthracene.To address the separation problem of anthracene and 2-alkylanthracene,solvent-assisted distillation technology was developed,resulting in a 98.9%purity of 2-alkylanthracene and a 91.82%separation yield.When the molar ratio of H2O_(2) to 2-alkylanthracene was 7:1,a 98.96%conversion of 2-alkylanthracene and a 99.94%selectivity for 2-alkylanthraquinone were achieved.A novel composition of 2-alkylanthraquinone,including 2-tert-butylanthraquinone,2-tert-amylanthraquinone,and 2-hexylanthraquinone,was developed.This composition could be effectively separated and purified through a combination of crystallization and washing processes.The elemental composition of the product met the existing standards,and its hydrogenation performance closely matched that of commercially available 2-tert-amylanthraquinone products.展开更多
基金supported by a grant from the National Natural Science Foundation of China(NSFC 22378437)the SINOPEC Excellent Youth Funds(ST22174).
文摘To expedite the development of industrial technology for producing 2-alkylanthraquinone,a novel pilot test of alkylation-oxidation technology was conducted.The process mainly included anthracene alkylation,separation of anthracene and 2-alkylanthracene,oxidation of 2-alkylanthracene,and product purification.Optimal alkylation conditions yielded a 91.1%conversion of anthracene and a 71.73%selectivity for 2-alkylanthracene.To address the separation problem of anthracene and 2-alkylanthracene,solvent-assisted distillation technology was developed,resulting in a 98.9%purity of 2-alkylanthracene and a 91.82%separation yield.When the molar ratio of H2O_(2) to 2-alkylanthracene was 7:1,a 98.96%conversion of 2-alkylanthracene and a 99.94%selectivity for 2-alkylanthraquinone were achieved.A novel composition of 2-alkylanthraquinone,including 2-tert-butylanthraquinone,2-tert-amylanthraquinone,and 2-hexylanthraquinone,was developed.This composition could be effectively separated and purified through a combination of crystallization and washing processes.The elemental composition of the product met the existing standards,and its hydrogenation performance closely matched that of commercially available 2-tert-amylanthraquinone products.
文摘为解决2-烷基蒽醌传统生产工艺——苯酐法的污染问题,开发了2-烷基蒽(R-AN)氧化生产2-烷基蒽醌的技术路线。采用过氧化氢盐酸(H_(2)O_(2) /HCl)体系进行R-AN的氧化,通过质谱与核磁共振分析确定主产物为2-烷基蒽醌,副产物为R-AN的一氯和二氯取代物;对氧化反应机理进行研究,明确了氧化反应活性物种为HClO和^(1)O_(2)。系统考察了溶剂种类、反应时间、H_(2)O_(2)及HCl与R-AN的物质的量之比、反应初始液相中的水质量分数[w(H_(2)O)]和R-AN质量浓度[ρ(R-AN)]对氧化反应效果的影响,并基于支持向量回归(SVR)理论建立了收率预测模型。通过模拟优化,确定最佳工艺条件为:常压、70℃、n(H_(2)O_(2))/n(R-AN)=5、n(HCl)n(R-AN)=5、w(H_(2)O)=8%、ρ(R-AN)=0.04 g mL、反应时间8 h。此条件下,所得2-烷基蒽醌的收率大于98%。模型的预测效果好,相对误差大部分在1.5%以内。
基金This research was supported by the National Science Foundation of China (20572015, 20672028)Program for NewCentury Ex-cellent Talents in University (NCET-05-0610)+3 种基金the Scientific Research Foundation for the Returned Overseas Chinese Scholars, State Education Min-istry (SRF for ROCS, SEM)Program for Young Excellent Talents in Henan UniversitiesFoundation of Education Department of Henan Province(2006150004)Program for Extraordinary Professors of Henan University and the Key Foundation of Henan University (04ZDZR013)
