Method for preparating ethyl linoleate by catalysis of composite solid ultra-strong acid
A solid superacid and ethyl linoleate technology, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of high cost, damage, and product quality decline of solid superacids, and achieve Good industrial application prospects, good selectivity and high reactivity
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Embodiment 1
[0016] Composite solid superacid catalyzed method for preparing ethyl linoleate, wherein composite solid superacid SO 4 2- / TiO 2 -SiO 2 The catalyst was prepared as follows, taking 4.88g (0.02mol) Ti(SO 4 ) 2 Dissolve in 20ml of distilled water to make a 1:4 (W / V) solution, add 28% ammonia solution dropwise under stirring, adjust to pH=9 to complete the reaction, and obtain amorphous Ti(OH) 4 Precipitate, then use 2mol / L HNO 3 The solution is adjusted and precipitated to PH = 3, and a certain amount of ethanol aqueous solution of ethyl orthosilicate is added dropwise at 80°C to obtain Ti(OH) with different molar ratios. 4 and Si(OH) 4 After the dropwise addition, continue to stir vigorously at room temperature for 1 hour, dry the obtained sol at 110°C, grind, sieve with a 100-mesh sieve, impregnate with 1mol / l sulfuric acid, suction filter, and dry dry, and finally fired at 450°C for 4 hours to obtain TiO 2 A series of compound SO with different contents 4 2- / TiO ...
Embodiment 2
[0023] The method for the preparation of ethyl linoleate by the composite solid superacid catalysis described in embodiment 1, in the reactor with water separator, condensation pipe, nitrogen protection device, thermometer and magnetic force stirring, add linoleic acid, Dehydrated alcohol and the TiO prepared by the method described in embodiment 1 2 Composite solid superacid SO with a mass percentage of 8.2% and regenerated after 5 uses 4 2- / TiO 2 -SiO 2 Catalyst, the amount of catalyst accounts for 3% of the linoleic acid quality, the mol ratio of linoleic acid and dehydrated alcohol is 1: 4, stirs under the protection of nitrogen, reacts under reflux temperature for 8 hours, isolates the product after cooling to room temperature, uses 0.1 The acid value of the sample was titrated with mol / L KOH standard solution, and the esterification rate of linoleic acid was calculated to be 90.2%.
Embodiment 3
[0025] Prepare SO by the method described in Example 1 4 2- / TiO 2 -SiO 2 Solid superacid catalyst, in which TiO 2 accounting for SO 4 2- / TiO 2 -SiO 2 The mass percentage content is 8.2%, and the Ti(OH) in the control catalyst preparation process4 and Si(OH) 4 The calcination temperature of the mixed sol was 500° C., other conditions for catalyst preparation were the same as those described in Example 1, and the calculated esterification rate of linoleic acid was 88.6%.
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