溶胶-凝胶法制备磷钨酸-硅胶催化合成苹果酯

采用溶胶-凝胶法制备了一系列磷钨酸-硅胶催化剂(PW/SG),考察了该催化剂催化乙酰乙酸乙酯与乙二醇液相缩合制备苹果酯的反应性能。实验结果表明,PW质量分数为40%时的PW/SG催化剂表现出最佳的催化活性;40%PW/SG催化剂制备苹果酯的最佳工艺条件为:n(乙酰乙酸乙酯)∶n(乙二醇)=1∶1.2,催化剂用量占反应物质量的0.36%,带水剂环己烷用量占反应物体积的30%,反应温度383K,反应时间90min;在此条件下,乙酰乙酸乙酯的转化率可达95.5%,苹果酯的选择性大于97%;催化剂稳定性实验表明,经5次重复使用,40%PW/SG催化剂的活性基本保持不变,乙酰乙酸乙酯转化率稳定在95.0%左右。     

磷钨钼杂多酸掺杂聚苯胺催化合成丁醛乙二醇缩醛

报道了以磷钨钼杂多酸掺杂聚苯胺为催化剂,通过丁醛和乙二醇反应合成了丁醛乙二醇缩醛。系统考察了醛醇物质的量比、催化剂用量以及反应时间诸因素对产品收率的影响。确定适宜的工艺条件为n(丁醛)∶n(乙二醇)=1∶1.5,催化剂的质量为反应物料总质量的0.8%,反应时间1.0 h。在此反应条件下,丁醛乙二醇缩醛的收率可达71.1%。     

单质碘催化合成丁醛乙二醇缩醛

以单质碘为催化剂,通过丁醛和乙二醇反应合成了丁醛乙二醇缩醛。探讨了单质碘对缩酮反应的催化活性,较系统地研究了醛醇物质的量比、催化剂用量和反应时间诸因素对产品收率的影响。实验表明：在n（丁醛）∶n（乙二醇）=1∶1.5、催化剂用量为反应物料总质量的0.4%、带水剂环己烷的用量为8mL和反应时间45min的优化条件下,丁醛乙二醇缩醛的收率可达77.6%.     

后缩醛改性聚醋酸乙烯乳液的研制

介绍了一种后缩醛改性聚醋酸乙烯乳液的制备方法，使聚醋酸乙烯乳液的耐水性、抗冻性能、粘接强度和流动性等有明显改善，可用于制备乳胶漆或其他对耐水性能有特殊要求的领域。     

新型有机-无机杂化物(TB0.5Zr0.5H0.5PW)催化合成苯甲醛乙二醇缩醛反应

通过离子交换法制备了系列季铵盐锆盐共掺杂磷钨酸催化剂,利用SEM、FT-IR、XRD、XPS、TGA-DTG以及正丁胺电位法等技术手段对催化剂结构、酸度进行表征,并对其催化缩醛反应性能进行研究。考察了催化剂用量、醇醛摩尔比、带水剂量和反应时间对苯甲醛乙二醇缩醛产率的影响。研究表明,TB_0.5Zr_0.5H_0.5PW(TB为四丁基溴化铵)固体酸催化剂具有优异的催化性能,催化剂强的Bronsted酸性、Bronsted与Lewis酸中心间的协同效应及“假液相”特性是该催化剂具有高活性的原因。以TB_0.5Zr_0.5H_0.5PW为催化剂,经响应面优化所得苯甲醛乙二醇缩醛最佳制备工艺条件为：乙二醇与苯甲醛摩尔比1.5:1,TB_0.5Zr_0.5H_0.5PW用量为苯甲醛质量的1.9%,反应时间3 h,带水剂环己烷量12.6 mL,该条件下苯甲醛乙二醇缩醛产率为94.6%。TB_0.5Zr_0.5H_0.5PW固体酸催化剂在重复使用6次后仍然表现出优异的催化性能,表明该催化剂具有较好的工业应用前景。关键词：磷钨酸;季铵盐;缩醛反应;苯甲醛乙二醇缩醛;催化技术 中图分类号：TQ655 文献标识码： A 文章编号：1003-5214 (2020) 01-0000-00     

A novel method to prepare poly(vinyl alcohol) water-soluble fiber with narrowly dissolving temperature range

Poly(vinyl alcohol) (PVA) is an important water-soluble polymer. In this study, a novel method has been developed for preparing water-soluble PVA fiber with narrowly dissolving temperature range via wet spinning of partly acetalized PVA. The structures and properties of the fiber were characterized by IR, ¹H-NMR, DSC, WAXD, tensile strength tester, etc. IR and NMR spectra showed that acetal groups were successfully generated on the lateral chains of PVA with the catalysis of acid. As a small quantity of CH₂O was added, the introduction of the acetal group could reduce both the hydrophilicity of amorphous region and the crystallinity of PVA water-soluble fiber, and hence narrowed the dissolving temperature range of fiber. However, the dissolving temperature range was broadened with a further increase of CH₂O amount, because of the large decrease of crystallinity and crystallite perfection. When the CH₂O added amount reached up to 20%, the acetalized PVA was completely insoluble, so that the spinning process could not be carried out. The breaking strengths of most acetalized fibers were beyond 4 cN/dtex, which satisfied the ordinary use of industrial and domestic field. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

带有磺酸基团和羰基酸团的新固体酸的合成及其在缩醛化反应中的催化性能简

The novel solid acid with both sulfonic and carbonyl acid groups has been synthesized from 3-（（2-sulfoethoxy） carbonyl）acrylic acid and tetraethyl orthosilicate （TEOS）. The catalytic activities were investigated through the acetalization. The results showed that the novel solid acid was very efficient for the reactions with the high yields. The high acidity, high stability and reusability were the key feature of the novel solid acid. Moreover, the sulfonic and carbonyl acid groups could cooperate during the catalytic process, which improved its catalytic activities. The catalyst shows recyclability, and hold great potential for replacement of homogeneous catalysts.     

Postsynthesis of hierarchical core/shell ZSM-5 as an efficient catalyst in ketalation and acetalization reactions

Hierarchical core/shell Zeolite Socony Mobil-five (ZSM-5) zeolite was hydrothermally postsythesized in the solution of NaOH and diammonium surfactant via a dissolution-reassembly strategy. The silica and alumina species were firstly dissolved partially from the bulky ZSM-5 crystals and then were in situ reassembled into the MFI-type nanosheets with the structure-directing effect of diammonium surfactant, attaching to the out-surface of ZSM-5 core crystals. The mesopores thus were generated in both the core and shell part, giving rise to a micropore/mesopore composite material. The micropore volume and the acidity of the resultant hybrid were well-preserved during this in situ recrystallization process. Possessing the multiple mesopores and enlarged external surface area, the core/shell ZSM-5 zeolite exhibited higher activity in the ketalation and acetalization reactions involving bulky molecules in comparison to the pristine ZSM-5.     

Al2O3对AlPO4催化剂的结构及其缩醛化反应活性的影响

采用溶胶-凝胶法制备了系列AlPO₄-Al₂O₃催化剂,利用XRD、TG-DTA、NH₃-TPD和催化剂评价等方法,研究了制备条件对催化剂结构和缩醛化反应催化性能的影响,结果表明,Al₂O₃的存在不仅能提高AlPO4的热稳定性,而且可以调节催化剂的表面酸性性能。在适宜的缩醛化反应条件下,400 ℃焙烧和Al₂O₃质量分数为15%的AlPO₄-Al₂O₃催化剂样品具有较好的催化活性,1,2-丙二醇转化率达28.1%,AlPO₄-Al₂O₃催化剂的缩醛化反应活性与表面弱酸中心的酸量成顺变关系。     

十二烷基磺酸铁催化合成苯甲醛1,2-丙二醇缩醛

以十二烷基磺酸铁为催化剂,苯甲醛、1,2-丙二醇为原料,研究合成了苯甲醛1,2-丙二醇缩醛.分别考察了反应时间、催化剂用量、原料配比、带水剂用量等条件对产物收率的影响.结果表明:十二烷基磺酸铁是合成苯甲醛1,2-丙二醇缩醛的良好催化剂,在n(苯甲醛):n(1,2-丙二醇)=1.0∶1.3,催化剂用量为反应物料总质量的1...