摘要
分别以酸碱法2-巯基苯并噻唑(简称M)和溶剂法M为原料,采用过氧化氢/次氯酸钠混合氧化法合成了促进剂N-环己基-2-苯并噻唑次磺酰胺(CBS),考察了氧化剂、环己胺及次氯酸钠用量,过氧化氢含量,氧化反应温度及时间对产物质量的影响,确定了最适宜工艺条件。结果表明,以酸碱法M为原料时,在M/环己胺/过氧化氢/次氯酸钠/水(摩尔比)为1/2.0/0.7/0.40/33.3、过氧化氢质量分数为30%、过氧化氢氧化温度为35℃及氧化时间为2.0 h、次氯酸钠氧化温度为35℃及氧化时间为1.5~2.0 h的条件下可制得促进剂CBS,其纯度超过99.5%,初熔点为101~103℃,收率达到92.0%~92.5%;以溶剂法M为原料时,其他条件不变,改变M/环己胺/过氧化氢/次氯酸钠/水为1/2.0/0.80/0.35/33.3、过氧化氢质量分数为10%,亦可制得促进剂CBS,其纯度为99.61%,初熔点为101.8℃,收率达到93.3%。
The accelerant N-cyclohexyl-2-benzo-thiazole sulfonamide（ CBS） was synthesized by mixed-oxidation method with acid-alkali method 2-mercaptobenzothiazole（ simplified as M） and solvent method M as raw material respectively. The effects of amount of oxidant,cyclohexanamine and sodium hypochlorite,content of hydrogen peroxide,temperature and time of oxidation reaction on the quality of products were investigated,and the most suitable process conditions were determined. The results showed thant the purity of accelerant CBS was more than 99. 5%,initial melting point was 101-103 ℃ and yield reached 92. 0%-92. 5% under the conditions of acid-alkali-method M/cyclohexylammonium/hydrogen peroxide/sodium hypochlorite/water（ mole ratio）1/2. 0/0. 7/0. 40/33. 3,mass fraction of hydrogen peroxide30%,oxidation temperature of hydrogen peroxide 35 ℃ and oxidation time 2. 0 h,oxidation temperature of sodium hypochlorite 35 ℃ and oxidation time 1. 5-2. 0 h. And the purity of accelerant CBS was 99. 61%,initial melting point was101. 8 ℃ and yield reached 93. 3% with changing solvent method M/cyclohexylammonium/hydrogen peroxide/sodium hypochlorite/water（ mole ratio） 1/2. 0/0. 80/0. 35/33. 3 and mass fraction of hydrogen peroxide 10%.
作者
王浩
于萍
杜丽丽
宋彦哲
WANG Hao1, YU Ping1, DU Li-li2, SONG Yan-zhe2(1. School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100, China; 2. Shandong Yanggu Huatai Chemical Co Ltd , Liaocheng 252311, Chin)
出处
《合成橡胶工业》
CAS
CSCD
北大核心
2018年第3期167-171,共5页
China Synthetic Rubber Industry
