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1.
TS-1分子筛催化苯酚和草酸二甲酯合成草酸二苯酯   总被引:5,自引:0,他引:5  
碳酸二苯酯;酯交换;TS-1分子筛催化苯酚和草酸二甲酯合成草酸二苯酯  相似文献   

2.
苯酚和草酸二甲酯酯交换反应产物的气相色谱分析   总被引:8,自引:0,他引:8  
提出了苯酚和草酸二甲酯酯交换合成碳酸二苯酯反应的终产物碳酸二苯酯和中间产物草酸二苯酯的气相色谱分析方法 ,采用OV 10 1色谱柱基线分离了碳酸二苯酯、草酸二苯酯及其相关化合物 ,外标法定量测定了碳酸二苯酯和草酸二苯酯 ,其相关系数分别为 1.0 0 0 3和 0 .995 0 ;方法的标准偏差RSD分别为 3.42 %和2 .5 8%;回收率分别为 93.3%~ 10 4.0 %和 95 .0 %~ 10 4.0 %;检出限分别为 8.1× 10 - 2 和 7.7× 10 - 2 g L。  相似文献   

3.
Zn(OAc)2·2H2O催化苯酚和草酸二甲酯酯交换合成草酸二苯酯   总被引:3,自引:0,他引:3  
研究了以Zn(OAc2·2H2O为催化剂时苯酚和草酸二甲酯酯交换合成草酸二苯酯的反应.采用气相色谱/质谱联用仪对主、副产物进行了定性,确定了中间产物甲基苯基草酸酯,并对反应过程的模式进行了探讨.考察了催化剂的催化性能及影响反应的因素.采用XRD技术对催化剂进行了表征,探讨了其失活原因.  相似文献   

4.
苯酚和草酸二甲酯在不同分子筛催化下的酯交换反应   总被引:4,自引:0,他引:4  
研究了以TS-1、H-ZSM-5、Hβ和H-丝光沸石等不同分子筛为催化剂,苯酚和草酸二甲酯酯交换合成草酸二苯酯反应。通过对催化剂进行吸附吡啶的红外光谱和NH3-TPD表征,考察了不同分子筛催化剂的酸性和酸强度对草酸二苯酯合成反应的影响,确定了催化剂上的弱酸中心是催化苯酚和草酸二甲酯酯交换合成草酸二苯酯反应的活性位,且催化剂的酸性中心越多,酸量越大,催化活性越好。催化剂上的强酸中心促进了副产物苯甲醚的生成。  相似文献   

5.
余晓鹏  张付宝 《分子催化》2018,32(4):334-341
采用溶胶-凝胶法在碱性条件下制备了一系列MoO_3/SiO_2催化剂用于草酸二甲酯和苯酚酯交换反应,并利用XRD、IR、XPS、NH3-TPD等表征催化剂结构.结果表明:弱酸中心是草酸二甲酯和苯酚酯交换反应的活性中心.当MoO_3负载量为12%(重量百分比),p H为9.1时的MoO_3/SiO_2催化剂具有更高的催化性能,这可能与该催化剂表面Mo物种分散更好和更高的酸量有关.在1.20 g MoO_3/SiO_2催化剂,0.20 mol苯酚,n(草酸二甲酯)/n(苯酚)=2,180℃反应3 h的条件下,苯酚转化率达70.0%,甲基苯基草酸酯和草酸二苯酯选择性分别为88.4%和11.5%.  相似文献   

6.
研究了几种有机钛化合物对草酸二甲酯(DMO)与苯酚酯交换反应的催化性能,发现催化活性及选择性顺序依次为二氯二茂钛钛酸四苯酯钛酸丁酯乙酰丙酮氧钛钛酸乙酯钛酸异丙酯,表明二氯二茂钛是一种性能较好的酯交换催化剂.在n(Cp2TiCl2)=0.001 mol、n(DMO)=0.3 mol、n(Phenol)=0.2 mol、T=180℃、t=2 h优化工艺条件下,苯酚转化率可达44.0%,甲基苯基草酸酯(MPO)和草酸二苯酯(DPO)收率分别达37.8%和6.1%,酯交换总选择性为99.8%.  相似文献   

7.
研究了几种有机钛化合物对草酸二甲酯(DMO)与苯酚酯交换反应的催化性能,发现催化活性及选择性顺序依次为二氯二茂钛>钛酸四苯酯>钛酸丁酯>乙酰丙酮氧钛>钛酸乙酯>钛酸异丙酯,表明二氯二茂钛是一种性能较好的酯交换催化剂。在n(Cp2TiCl2) = 0.001 mol、n (DMO) =0.3mol、n (Phenol) = 0.2mol、T=180癈、t=2h优化工艺条件下,苯酚转化率可达44.0%,甲基苯基草酸酯(MPO)和草酸二苯酯(DPO)收率分别达37.8%和6.1%,酯交换总选择性为99.8%。  相似文献   

8.
催化剂对碳酸二甲酯与苯酚酯交换反应的影响   总被引:6,自引:0,他引:6  
甲基苯基碳酸酯;碳酸二苯酯;催化剂对碳酸二甲酯与苯酚酯交换反应的影响  相似文献   

9.
杜治平  姚洁  王公应 《合成化学》2006,14(3):303-305,313
以钛酸四丁酯催化碳酸乙烯酯与乙酸苯酯酯交换合成碳酸二苯酯(DPC)。GC-MS定性分析表明,反应液中含主产物DPC,中间体2-乙酰氧乙基苯基碳酸酯(1),副产物乙二醇二乙酸酯、乙二醇苯醚乙酸酯和苯酚。1的结构经1H NMR,13C NMR,FT-IR和EI-MS确证。  相似文献   

10.
碳酸二苯酯(DPC)是非光气法生产聚碳酸酯(PCs)的重要原料,具有多种酯交换法合成路线,如碳酸二甲酯(DMC)与苯酚酯交换法、DMC与苯基乙酸酯(PA)酯交换法、草酸二甲酯(DMO)与苯酚酯交换法等.本文对比测定了几种金属乙酰丙酮配合物和有机钛化合物对碳酸二甲酯(DMC)与苯基乙酸酯(PA)酯交换合成DPC反应的催化性能,结果表明,乙酰丙酮氧钛[TiO(acac)2]是一种良好的酯交换催化剂,具有优良的催化性能.在反应条件θ=180℃,n(PA)=0.8 mol,n(DMC)/n(PA)=1/2,n(TiO(acac)2)/n(PA)=0.006,t=4 h下,DMC转化率可达74.9%,甲基苯基碳酸酯(MPC)和DPC的选择性分别可达56.9%和38.9%.探索并提出了TiO(acac)2催化DMC与PA酯交换合成DPC反应的机理.  相似文献   

11.
TiO2/SiO2催化苯酚和草酸二甲酯酯交换合成草酸二苯酯   总被引:5,自引:0,他引:5  
Diphenylcarbonate (DPC)isabasicmaterialfornon phosgene productionof polycarbonates .Severalalternativenon phosgenemethodsforDPCsynthesishavealsobeenproposed ,oneofthemisthetranses terificationofdimethyloxalate (DMO)withphenoltodiphenyloxalate (DPO)andthedecarbonylationofDPOtoDPC .Inthisprocess ,thesynthesisofDPOfolloweda 2 stepreactionmoduleoftransesterifi cationofDMOwithphenoltomethylphenyloxalate(MPO)andthedisproportionationofMPOtoDPOandDMO[1] .UbeIndustriesreportedthatconven…  相似文献   

12.
 研究了Sn改性TS-1催化剂催化苯酚和草酸二甲酯(DMO)酯交换合成草酸二苯酯(DPO)反应。以Sn改性TS-1为催化剂时,Sn活性中心和Lewis酸中心协同作用催化苯酚和DMO酯交换合成DPO反应。因为Sn的加入,在保持MPO和DPO高选择性的同时,DMO转化率显著提高。而且Sn活性中心有利于MPO歧化反应生成DPO,从而大大提高了DPO的选择性。但是,当Sn负载量大于2%时,SnO2由均匀分布在TS-1表面改变为以晶体状态存在,从而导致DMO转化率的大幅降低。  相似文献   

13.
The transesterification of dimethyl oxalate (DMO) with phenol is studied on various Ti-containing phosphate (Ti-P-O) catalysts. The weak acid-base characteristics of Ti-P-O catalysts are responsible for the high activity and selectivity to methyl phenyl oxalate (MPO) and diphenyl oxalate (DPO).  相似文献   

14.
Diphenyl oxalate was synthesized from transesterification of dimethyl oxalate with phenol over TS-1(2.5 wt% Ti)catalyst.TS-1 catalyst,as a beterogeneous catalyst,showed excellent selectivity of diphenyl oxalate and methylphenyl oxalate compared with other homogeneous catalysts.Lewis acid sites on TS-1 catalyst were the active sites for transesterification of dimethyl oxalate with phenol.the high selectivity was closely related to the weak acid sites over TS-1.  相似文献   

15.
The influence of molybdenum content on the catalytic performance in the transesterification of dimethyl oxalate (DMO) with phenol to methyl phenyl oxalate (MPO) and diphenyl oxalate (DPO) was investigated. The results indicated that the MoO3/Al2O3 catalyst with 14 wt% Mo content gave maximal DPO yield with 6.1% and 75.1% DMO conversion. The component, structure and phase of MoO3/Al2O3 catalysts were characterized by means of X-ray diffraction (XRD), BET specific surface area, temperature-programmed desorption of ammonia (NH3-TPD), and FTIR analysis of adsorbed pyridine. This revised version was published online in June 2006 with corrections to the Cover Date.  相似文献   

16.
The 12-molybdosphoric acid mixed with titania (MPA-TiO2) was found to be a novel and efficient catalyst for the synthesis of diphenyl carbonate (DPC) via transesterification of dimethyl carbonate (DMC) and phenol. The X-ray diffraction (XRD) and infrared (IR) techniques were employed to characterize the prepared catalysts. The effect of the weight ratio of the 12-molybdosphoric acid to titania on the transesterification was investigated. A 13.1% yield of DPC and an 11.6% yield of methyl phenyl carbonate (MPC) were obtained over MPA-TiO2 with the weight ratio of MPA to TiO2 as 5:1.  相似文献   

17.
梅付名  李光兴 《合成化学》2003,11(4):320-326
在298.15K,101.325kPa条件下,液态碳酸二甲酯(DMC)的标准Gibbs自由能和熵分别估算为-472.3kJ*mol-1和245.2J*mol-1*K-1.在298K~523K计算了由DMC和苯酚生成碳酸二苯酯(DPC)和苯甲醚反应的热力学性质(ΔrH0m,ΔrS0m,ΔrG0m和平衡常数).计算出的热力学性质表明,DMC和苯酚酯交换合成DPC反应是吸热的,并且在热力学上是不利的.研究了n-Bu2SnO, Ti(OC4H9)4, AlCl3和ZnCl2四种酯交换法合成DPC反应的催化剂,其中n-Bu2SnO具有最高的催化活性.热力学计算和实验结果均表明,合成DPC反应的最佳温度为453K.当以n-Bu2SnO为催化剂,n(苯酚)∶n(DMC)=4∶1时,DPC的产率和选择性分别为43.0%和88.7%.  相似文献   

18.
A high-purity sample of methyl phenyl carbonate (MPC) was obtained by developing a novel reaction route followed by a series of separation and purification procedures. Identification and quantification of the MPC sample (98.32%) was performed by a gas chromatography–mass spectrometry and Karl Fisher titration. The laboratory-prepared MPC was then used as a standard to optimize quantitative analysis of the products synthesized by transesterification of dimethyl carbonate and phenol. The advantage of the improved method was that MPC can be quantified directly rather than being calculated by subtracting the yield of diphenyl carbonate (DPC) and by-product anisole from the conversion of dimethyl carbonate (DMC). The resulting method was validated for linearity, precision, accuracy, detection limit, and quantification limit. With the improved method, simultaneous accurate quantification of DMC, MPC, DPC, phenol, and anisole in the transesterification products can be achieved. This enables evaluation of the activity and selectivity of different catalysts and control of the reaction processes.   相似文献   

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