偏三甲苯溶剂法2,4′-二羟基二苯砜的合成  

SYNTHESIS OF 2,4'- DIHYDROXYDIPHENYL SULFONE WITH unsym-TRIMETHYL BENZENE AS SOLVENT

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作  者:吴永红[1] 张兵[1] 朱静[1] 孙明珠[1] 

机构地区:[1]沈阳工业大学石油化工学院,辽宁辽阳111003

出  处:《精细石油化工》2011年第3期73-76,共4页Speciality Petrochemicals

基  金:辽宁省教育厅科研计划项目(2008498);沈阳工业大学青年学术骨干教师项目(200923)部分资助

摘  要:以苯酚和硫酸为原料,偏三甲苯为溶剂合成了新型显色剂2,4′-二羟基二苯砜(2,4′-BPS),并通过两步甲醇-邻二氯苯混合溶剂法精制,得到高质量分数试样。在粗品合成中,考察了原料摩尔比、催化剂用量等因素对收率和质量分数影响;在精制过程中,考察了甲醇质量分数、溶剂用量等对产品收率和质量分数的影响。结果表明采用廉价偏三甲苯效果优于传统均三甲苯,在苯酚/硫酸摩尔比2.3/1,催化剂用量4g时,粗品中2,4′-BPS质量分数达37.8%,收率为91.17%;通过对粗品两步连续精制,2,4′-BPS质量分数达95.0%以上。Novel color developer, 2,4'-dihydroxydiphenyl sulfone (2,4'-BPS), was synthesized by u- sing phenol and sulfuric acid as raw materials and unsyrn-trimethyl benzene as solvent. The as-ob- tained product was further purified by mixing solvent method to reach high content. The effects of some factors in the synthetic process of the crude product, such as feed composition, catalyst dosage, etc. , on the yield and purity were investigated. The effects of methanol content and solvent mass on the product during purification were also studied. It demonstrated that the relative inexpensive solvent unsyrn-trimethyl benzene is a promising substitute for conventional sym-trimethylbenzene (mesity- lene) to synthesize 2,4'-BPS with high yield and purity. The yield of 91.17% and purity of 37.8% for 2,4'-BPS were reached under the condition of phenol/sulfic acid equaling 2.3 : 1 and catalytic dosage of 4 g. Furthermore, 2,4'-BPS above 95.0% can be obtained from methanol-o-dichlorobenzene mixing solvent through two successive purification steps, with the advantages of easy recovery and recycle.

关 键 词:偏三甲苯 二羟基二苯砜 合成 精制 

分 类 号:TQ247.3[化学工程—有机化工]

 

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