CAJ | 학술논문

采用溶胶-凝胶法制备了HZSM-5分子筛负载SO42?/TiO2固体超强酸催化剂，利用直接酯化法催化合成三羟甲基丙烷油酸酯。通过IR、XRD、BET、SEM对催化剂进行了表征，结果表明TiO2以纳米颗粒的形式附着于HZSM-5分子筛表面，且负载后催化剂的比表面积高达309.2m2/g，比HZSM-5分子筛提高了45.6m2/g，且催化剂具有强酸性（?13.8<H0<?12.14）。探讨了沉淀 pH 值、焙烧温度、焙烧时间等催化剂制备条件对 SO42?/TiO2-HZSM-5固体超强酸催化剂催化三羟甲基丙烷油酸酯酯化反应活性的影响。结果表明在沉淀pH=8、硫酸的浸渍浓度为0.5mol/L、浸渍时间为30min、焙烧温度为550℃、焙烧时间4h的条件下，SO42?/TiO2-HZSM-5固体超强酸催化剂催化活性最高，三羟甲基丙烷油酸酯的酯化率高达97.6%；抗乳化性能良好，油水分离时间为5min。SO42?/TiO2-HZSM-5固体超强酸催化剂在重复使用6次的情况下，酯化率下降8.8%，催化剂的重复使用性能良好。
채용용효-응효법제비료HZSM-5분자사부재SO42?/TiO2고체초강산최화제，이용직접지화법최화합성삼간갑기병완유산지。통과IR、XRD、BET、SEM대최화제진행료표정，결과표명TiO2이납미과립적형식부착우HZSM-5분자사표면，차부재후최화제적비표면적고체309.2m2/g，비HZSM-5분자사제고료45.6m2/g，차최화제구유강산성（?13.8<H0<?12.14）。탐토료침정 pH 치、배소온도、배소시간등최화제제비조건대 SO42?/TiO2-HZSM-5고체초강산최화제최화삼간갑기병완유산지지화반응활성적영향。결과표명재침정pH=8、류산적침지농도위0.5mol/L、침지시간위30min、배소온도위550℃、배소시간4h적조건하，SO42?/TiO2-HZSM-5고체초강산최화제최화활성최고，삼간갑기병완유산지적지화솔고체97.6%；항유화성능량호，유수분리시간위5min。SO42?/TiO2-HZSM-5고체초강산최화제재중복사용6차적정황하，지화솔하강8.8%，최화제적중복사용성능량호。
The catalyst of solid superacid SO42?/TiO2 supported on HZSM-5 was prepared by sol-gel process. The trimethylolpropane oleate was synthesized by direct esterification. The catalyst was characterized by IR,XRD,BET,and SEM. The results show that SO42?/TiO2 with the form of nanoparticles is supported on the surface of HZSM-5,the BET surface area of the catalyst is up to 309.2m2/g,increasing 45.6m2/g compared with HZSM-5,and the catalyst is with better solid acidity. The effects of catalyst preparation conditions on catalytic reactivity were studied. The optimal condition for the preparation of the catalyst was obtained as follows:the pH for deposition is 8, impregnation concentration of H2SO4 is 0.5mol/L,impregnation time is 30min,calcination temperature and time are 550℃ and 4h,respectively. Under the optimal condition,solid superacid SO42?/TiO2-HZSM-5 catalyst has the best the catalytic performance,the esterification rate of trimethylolpropane oleate is as high as 97.6%,the product can exhibit excellent emulsification resistive property,and oil-water separation time is 5min. After solid superacid SO42?/TiO2-HZSM-5 catalyst is reused 6 times,the esterification rate of trimethylolpropane oleate decreases by 8.8%,i.e. the catalyst shows good reusability.