CAJ | 학술논문

以Dawson型磷钨酸（H6P2W18O62·13H2O）和硝酸铜为原料，通过复分解法合成了新型Dawson型磷钨酸铜，并以磷钨酸铜为催化剂催化1，4-丁二醇环化脱水合成四氢呋喃（THF），利用FTIR， XRD，EDS，SEM，Py-IR，NH3-TPD等方法对磷钨酸铜进行了表征。考察了磷钨酸铜催化剂催化合成THF的工艺。表征结果显示，磷钨酸铜具有Dawson结构，分子式为Cu2H2P2W18O62·nH2O，分子形态呈椭球状，同时具有Lewis酸中心和Br?nsted酸中心。与H6P2W18O62·nH2O相比，磷钨酸铜的Lewis酸性强、酸强度增强、但酸量降低。实验结果表明，适宜的反应条件为：催化剂用量3.3%（w）（基于1，4-丁二醇的用量）、反应温度180℃、反应时间35 min，在此条件下THF收率为96.7%。催化剂重复使用5次后，THF收率仍可达到93.3%。
이Dawson형린오산（H6P2W18O62·13H2O）화초산동위원료，통과복분해법합성료신형Dawson형린오산동，병이린오산동위최화제최화1，4-정이순배화탈수합성사경부남（THF），이용FTIR， XRD，EDS，SEM，Py-IR，NH3-TPD등방법대린오산동진행료표정。고찰료린오산동최화제최화합성THF적공예。표정결과현시，린오산동구유Dawson결구，분자식위Cu2H2P2W18O62·nH2O，분자형태정타구상，동시구유Lewis산중심화Br?nsted산중심。여H6P2W18O62·nH2O상비，린오산동적Lewis산성강、산강도증강、단산량강저。실험결과표명，괄의적반응조건위：최화제용량3.3%（w）（기우1，4-정이순적용량）、반응온도180℃、반응시간35 min，재차조건하THF수솔위96.7%。최화제중복사용5차후，THF수솔잉가체도93.3%。
A new Dawson type copper phosphotungstate catalyst was prepared from Dawson type phosphotungstic acid and cupric nitrate by double decomposition method,and was characterized by means of FTIR,XRD,SEM,EDS,Py-IR and NH3-TPD. The catalyst was used in the cyclodehydration of 1,4- butan ediol to tetrahydrofuran(THF). The results showed that the copper phosphotungstate existed in the form of spheres and kept the Dawson str ucture. There were both Br?nsted and Lewis acid centers in the catalyst and its molecular formula was Cu2H2P2W18O62·nH2O. Compared to H6P2W18O62·nH2O,the acid strength of the copper phosphotungstate increased, but its total acidity decreased. Under the optimal reaction conditions of mass ratio of catalyst to 1, 4-butanediol 3.3%,reaction temperature 180℃ and reaction time 35 min,t he yield of THF reached 96.7%. And after it was reused fi ve times,the yield still reached 93.3%.