Method for synthesizing acetate through ester exchange path
A technology of acetate and transesterification, which is applied in the direction of chemical instruments and methods, reaction preparation of ester groups and hydroxyl groups, molecular sieve catalysts, etc., and can solve problems such as side reactions, environmental pollution, complex difficulties, etc.
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[0050] 1) Preparation of Mesoporous Molecular Sieve K-MOR
[0051] 50 g of purchased microporous (10 Å-2 nm) H-MOR molecular sieves were first treated with 1 mol / L NaNO 3 Ion exchange poisoning acid site: solid-liquid ratio is 1g : 10 mL. Exchange at 80°C for 2h, filter and wash. After three consecutive exchanges, dry at 120°C overnight, and calcined at 500°C for 4 hours to obtain microporous K-MOR. Put the microporous K-MOR in a composite base (it can be two or more of alkali metal and ammonium hydroxide, such as lithium hydroxide, sodium hydroxide, potassium hydroxide and ammonium hydroxide, etc.) In an alkaline solution with a concentration of 0.1-2mol / L, it is heat-treated at 80°C for 10 hours. The heat-treated K-MOR molecular sieve was washed with deionized water to remove residual lye, and dried at 120 °C for 10 h to obtain a mesoporous molecular sieve carrier.
[0052] 2) Preparation of K-MOR carrier
[0053] Take 20 g of the mesoporous molecular sieve K-MOR prepar...
Embodiment 1
[0059] In a 10 L slurry bed reactor, the reaction pressure is 0.1 MPa, the reaction raw material methyl acetate: isooctyl alcohol = 1:1.5, each 100 g of the above-mentioned prepared basic catalysts are put into respectively, and the total volume of the reaction solution is 6 L. The reaction was mechanically stirred at a reaction temperature of 70°C. After 4 hours of reaction, samples were taken for chromatographic analysis and calculation. The effects of different catalysts on the conversion rate of raw materials are shown in Table 1.
[0060]
[0061] Reaction conditions: pressure: 0.1 MPa, raw material molar ratio: methyl acetate: isooctyl alcohol = 1:1.5, catalyst: 100g, reaction temperature 70°C, reaction time 4h.
[0062] It can be seen from Table 1 that different catalysts have a great influence on the catalyst activity. When the catalyst is a microporous H-MOR, since the catalyst has an acid active site, the catalyst has a very poor catalytic effect due to its lack of...
Embodiment 2
[0064] In a 10 L slurry bed reactor, the reaction pressure is 0.1 MPa, the molar ratio of the reaction raw material methyl acetate to various alcohols (ethanol, propanol, butanol, isobutanol, pentanol, isoamyl alcohol, benzyl alcohol) 1:1, put into the ZnO-MgO-La prepared above 2 o 3 / K-MOR catalyst 100 g, the total volume of the reaction solution is 6 L. The reaction was mechanically stirred at a reaction temperature of 160°C. After 4 hours of reaction, samples were taken for chromatographic analysis and calculation. The effects of different alcohol types on the conversion rate of raw materials are shown in Table 2.
[0065]
[0066] Reaction conditions: pressure: 0.1 MPa, molar ratio of raw materials: methyl acetate: alcohol = 1:1, catalyst: 100 g, reaction temperature 160 ℃, reaction time 4h.
[0067] It can be seen from Table 2 that the transesterification of methyl acetate and ethanol is adopted, the molar ratio of raw material alcohol to ester is 1:1, the reaction t...
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