高温液态水中稀硫酸催化下氰基酰胺盐水解制备1,1-环己基二乙酸

Synthesis of 1,1-Cyclohexanediacetic Acid Catalyzed by Dilute Sulfuric Acid in High-Temperature Liquid Water

针对1,1-环己基二乙酸工业化生产中存在的污染和腐蚀问题,提出了高温液态水中α,α’-二氰基-1,1-环己基二乙酰亚胺铵盐在稀硫酸催化下水解制备1,1-环己基二乙酸的方法,测定了不同初始质量浓度(0.01～0.1 g/mL)、不同反应温度(160～280℃)以及不同硫酸浓度(0%～15%)对α,α’-二氰基-1,1-环己基二乙酰亚胺铵盐在高温液态水中水解生成1,1-环己基二乙酸的影响。结果表明,在原料初始质量浓度为0.05 g/mL,催化剂稀硫酸浓度为15%,反应温度为220℃的条件下,目标产物1,1-环己基二乙酸的最高收率可以达到88.31%,高于浓硫酸催化工艺。同时,稀硫酸催化工艺的绿色性大大高于浓硫酸工艺。

Serious pollution and corrosion problems 1,1-cyclohexanediacetic acid paper, a exist in the new method industrialized production of concerning hydrolysis of 1,1-cyclohexanediacetimide,α, α＇-dicyano-compd with ammonia catalyzed by dilute sulfuric acid in high-temperature liquid water（HTLW） was proposed. The influence of initial concentration （0.01-0.1 g/mL）, reaction temperature （160-280 ℃） and sulfuric-acid concentration （0%-15%） on the yield of 1,1-cyclohexanediacetic acid was systematically investigated. The results show that 88.31% yield of 1,1-cyclohexanediacetic acid could be reached at the reaction temperature of 220 ℃, sulfuric-acid concentration of 15% and initial mass concentration of 0.05 g/mL, which is higher than industrial process catalyzed with concentrated sulfuric acid. Also, the new process with dilute sulfuric-acid is much greener.