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Rare earth solid superacid SO4 ^ 2-/TiO2/Sm ^ 3 + Catalytic Synthesis of isooctyl


Tim at 500 ℃ of 3h, which have rare earth solid superacid SO Ding i0m1.3 ethylhexyl adipate with the synthesis of the watershed, mixer,[link widoczny dla zalogowanych], thermometer four flasks, by adding a certain amount of sorbic acid, 2-ethylhexyl alcohol and a rare earth catalyst, heat refluxing. Regular intervals of time the acid value of reaction solution,[link widoczny dla zalogowanych], acid value according to GB1668-81 method to the reaction system to determine the acid esterification rate changes. Esterification rate = (1 an acid value of a time before the reaction / response to the initial acid solution) × l00% after reaction, the reaction to the weak acid solution and then were treated with water,[link widoczny dla zalogowanych], dilute sodium carbonate solution, water washing,[link widoczny dla zalogowanych], drying, vacuum distillation to collect 166-172 ℃ / 2300Pa the fractions for the products. 2 Results and discussion 2.1 Rare earth solid acid So2-Niom interested in the IR analysis shown in Figure 1. The figure in the 1134cm-t, 1040cm obvious at super acid characteristics. This is typical of the reported location of the solid superacid existence of the corresponding characteristic absorption peak of results. To prove: that the catalyst is the solid super acid. Analysis of 22 surface acidity of nitrobenzene using Hammett indicator (H a 11.4) in the determination of the color reaction of the acid catalyst strength Ho <a 11.4, the intensity of concentrated sulfuric acid, H-11.94, showing that the acid strength than concentrated sulfuric acid, a super acid characteristics. On the boat Jane: Qun male born in 1971, Master of polymer modified and fine homes in the teaching and research work into published many articles No. 5 Chen Q: rare earth solid superacid S042-FFiOz. , Sm3 \2.5g rare earth catalyst refluxing for different refluxing time for analysis, determination of the esterification rate. The results in Table 1. Table 1, reaction time on the rate of esterification can be seen from Table l, reaction time increases, can increase the esterification rate, the reaction time of 1 hour, the reaction system, no change in the basic rate of esterification, indicating that esterification has been reached balance, therefore, the reaction time chosen l_0h. 2.4 The amount of catalyst on the reaction of adipic acid with 0.1mol, 0.55mol2 one-ethylhexyl alcohol, refluxing 1.0h, changing the amount of catalyst, the results shown in Table 2, Table 2, the amount of dip of the catalyst Rate can be seen from Table 2, the esterification rate increased with the amount of catalyst is increased. To 4.0g and then increase the amount of catalyst, the esterification rate of decline. Therefore, under experimental conditions, the ideal amount of catalyst is 2.5g. 2.5 mole ratio on the reaction of adipic acid 0.1tool, 255 refluxing 1.0h catalyst for a change in 2-ethylhexyl alcohol consumption, results in Table 3. Wrap 3 molar ratio on esterification of waxy Chapter of Table 3 shows, alkyd less than 5.5:1, mole ratio is conducive to increased esterification rate increase. When the mole ratio exceeds 5.5:1. System esterification rate. From the reaction equilibrium, the increased alcohol consumption is conducive to a balanced move, but excessive alcohol use, will reduce the concentration of the catalyst, the esterification rate is not conducive to the improvement. 2.6 product identification products obtained by the synthesis of this Law is a colorless, transparent liquid product of the refractive index measured n ~ = 1.4372 (the literature value 1.4369). In its IR spectrum, 25003500cmi does not appear the characteristic absorption peak of carboxyl, 1725OB'I-absorption peak appears Chiu cane, 3 Conclusions (1) rare earth solid superacid catalyst sO. Ⅶ OgSm Catalytic Synthesis is ETHYLHEXYL good catalyst compared with the concentrated sulfuric acid, mild reaction, after the convenient, virtually no equipment corrosion, do not pollute the environment, catalytic esterification rate, is a great development the future of environment-friendly catalyst for the esterification. (2) rare earth solid superacid s00gsm Synthesis of dioctyl has two optimum conditions are: acid molar ratio 1:5.5, reaction time 1.0h, the amount of adipic acid catalyst 2.5g/mol.
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