吡咯烷衍生物的合成研究.pdf

1、河北工業(yè)大學(xué)碩士學(xué)位論文吡咯烷衍生物的合成研究姓名：文彥瓏申請學(xué)位級別：碩士專業(yè)：應(yīng)用化學(xué)指導(dǎo)教師：趙繼全2011-03河北工業(yè)大學(xué)碩士學(xué)位論文 vSTUDY ON SYNTHESIS OF PYRROLIDINE DERIVATIVES ABSTRACT In this thesis, a series of solid acid catalyst for the amination of tetrahydrofuran to py

2、rrolidine were prepared by hydrothermal synthesis and impregnation. Their catalysis on the reaction was investigated on a fixed-bed reactor and the experimental results revealed that H-ZSM-5(80) showed good catalytic per

3、formances. The parameters which influence the reaction with H-ZSM-5(80) as catalyst were studied and the optimum conditions were obtained, which the reaction temperature is 350 ℃, the molar ratio of ammonia to tetrahydro

4、furan is 6:1 and the contact time is 6.9 s under atmospheric pressure. Under the optimized reaction conditions the conversion of tetrahydrofuran reached up to 82.9% with pyrrolidine selectivity of 75.2%. In addition the

5、lifetime of catalyst was also investigated and it was found the catalyst can be effective at least for 600h under the optimized reaction conditions. During this period the conversion of tetrahydrofuran maintained higher

6、80% and the selectivity of pyrrolidine was above 65%. The possible reasons for the deterioration of performances of the catalyst were discussed after characterization of the catalyst by X-ray diffraction, N2-adsorption a

7、nd NH3-TPD. Comparison of the characterization results of used sample of the catalyst with that of the fresh one revealed that the structure of the catalyst was maintained after the catalytic run. The deterioration of th

8、e catalyst is attributed to the carbon deposition on the surface of catalyst, which blocked up the smaller holes and covered the acid centers in the matrix of the catalyst. The performances of the catalyst can be recover

9、ed by oxidation on line. The catalyst was also applied to the synthesis of N-methyl-pyrrolidine from tetrahydrofuran and methylamine and excellent results were received. The optimized parameters, which are that the reac