Preparation method of catalyst for preparing ethylene glycol by hydrogenation of dimethyl oxalate
A technology for the preparation of dimethyl oxalate and hydrogen, which is applied in the preparation of organic compounds, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problems of high equipment precision, inconvenient manufacturing, Affect production efficiency and other issues to achieve the effect of improving production efficiency, high activity and selectivity, and shortening production time
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preparation example Construction
[0021] The preparation method of described catalyst is characterized in that: comprises the following steps:
[0022] 1. Dissolving the soluble salt of Ru and M in the mixed liquid of oleylamine and oleic acid, the volume mixing ratio of oleylamine and oleic acid is 1:1, so that the soluble salt of Ru and M can be fully dissolved in oleylamine In the mixed liquid with oleic acid;
[0023] 2. Take the octadecene solution as the organic solvent in the container, replace N times with helium gas in the container, stir and heat the organic solvent to 85°C under the condition of helium gas flow, and pass the sampler at a temperature of 85°C. Add the n-butyllithium n-heptane solution as a reducing agent to the container of the organic solvent at ℃ to react. After the temperature of the solution in the container returns to 85°C, add the mixed liquid prepared in step 1 to the container, and control the temperature in the container. After the reactant is kept at 85°C for 45 minutes, th...
Embodiment 1
[0031] In this example, a catalyst for the hydrogenation of dimethyl oxalate to ethylene glycol uses RuCu alloy as the active component and KIT-6 as the carrier. The specific surface area of KIT-6 is 600m 2 / g, the mass of RuCu alloy is 0.1wt% of the carrier. The following is the specific preparation process of the catalyst:
[0032] (1) Dissolve 0.0016 mmol of ruthenium acetylacetonate and 0.0016 mmol of copper acetylacetonate in a mixed solution of 4 ml of oleylamine and oleic acid (the volume ratio of oleylamine and oleic acid is 1:1), heat and stir to fully dissolve;
[0033] (2) Measure 20ml of octadecene and add it to a 50ml three-necked flask, replace it with helium for 5 times, stir and heat it to 85°C under a helium atmosphere, and quickly add 0.201ml of it with a disposable sampling needle at a concentration of 1mol / L n-butyllithium n-heptane solution, after the temperature in the three-necked flask is restored, continue to add the liquid prepared in step (1), kee...
Embodiment 2
[0039] In this example, a catalyst for the hydrogenation of dimethyl oxalate to ethylene glycol uses RuCu alloy as the active component and KIT-6 as the carrier. The specific surface area of KIT-6 is 600m 2 / g, the mass of RuCu alloy is 2wt% of the support. The following is the specific preparation process of the catalyst:
[0040] (1) Dissolve 0.0243 mmol of ruthenium acetylacetonate and 0.0243 mmol of copper acetate in a mixed solution of 4 ml of oleylamine and oleic acid (the volume ratio of oleylamine and oleic acid is 1:1), heat and stir to fully dissolve;
[0041] (2) Measure 20ml of octadecene and add it to a 50ml three-neck flask, replace it with helium for 5 times, stir and heat it to 85°C under a helium atmosphere, and quickly add 0.972ml of it with a disposable sampling needle at a concentration of 1mol / L n-butyllithium n-heptane solution, after the temperature in the three-necked flask is restored, continue to add the liquid prepared in step (1), keep the temper...
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