Catalyst for preparing divalent alcohol by hydrogenating dibasic acid ester and preparation method and application thereof
A dicarboxylic acid ester and catalyst technology, applied in metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve the complex preparation process, no industrial application precedent, and harsh conditions. and other problems, to achieve the effect of low reaction temperature, favorable for industrial application and improved stability
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Embodiment 1
[0031] Weigh 34.5g of sodium silicate to configure 200mL aqueous solution, weigh 24.1g of Cu(NO 3 ) 2 and 1.2g Ni(NO 3 ) 2Add deionized water to prepare a 200mL mixed salt solution, raise the temperature and keep it at 50°C, then add a sodium silicate aqueous solution dropwise under stirring, and control the pH value of the solution at the end of the reaction to 7.0; After washing with deionized water three times and suction filtering; the catalyst was dried at 80°C for 12 hours, and then calcined at 350°C for 6 hours to finally obtain catalyst A. Catalyst A was formed and screened to 20-40 mesh and placed in a reaction tube. With pure hydrogen at a flow rate of 100mL / min, it was reduced at 250°C for 6 hours and then adjusted to the reaction process conditions for hydrogenation reaction. Reaction raw material selects dimethyl oxalate.
[0032] Catalyst reaction conditions and results are shown in Table 1.
[0033] Table 1 Catalyst test data comparison
[0034] E...
Embodiment 2
[0036] Weigh 24.1g Cu(NO 3 ) 2 and 1.0g Mn(NO 3 ) 2 Add deionized water to prepare a mixed salt solution with a concentration of 0.2M, add dropwise 28% ammonia water, stir and mix evenly, and control the pH value to 11; into the salt solution and stirred for 2 hours; heated the above solution to 70°C, and reacted at constant temperature for 5 hours until the pH value of the solution at the end of the reaction was 7.0; after the reaction was completed, the feed solution was filtered while it was hot, and then washed three times with deionized water and then Suction filtration; the catalyst was dried at 90°C for 12 hours, and then calcined at 500°C for 6 hours to finally obtain catalyst B. Catalyst B was formed and screened to 20-40 mesh and placed in a reaction tube. With pure hydrogen at a flow rate of 100mL / min, it was reduced at 260°C for 4 hours and then adjusted to the reaction process conditions for hydrogenation reaction. Reaction raw material selects dimethyl oxalat...
Embodiment 3
[0039] Catalyst preparation is the same as in Example 2, the difference is that the deionized water washing is replaced by ethanol washing twice, the reaction raw material is diethyl oxalate, the reduction condition is that the hydrogen content gradually increases from 2% to 100%, and finally adjusted at 300 ° C for 4 hours. To the reaction process conditions to react.
[0040] Catalyst reaction conditions and results are shown in Table 1.
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