Hydrogenation catalyst for synthesizing 1, 3-butanediol as well as preparation method and application of hydrogenation catalyst
A technology of hydrogenation catalyst and butanediol, which is applied in the field 1, can solve problems such as dehydration or even polymerization of 3-hydroxybutyraldehyde, increase the difficulty of product separation and purification, affect product yield and purity, and achieve excellent activity and high The effect of stability and long service life
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[0041] A preparation method of hydrogenation catalyst, comprising the following steps:
[0042] (1) Dissolve nickel nitrate hexahydrate, magnesium nitrate hexahydrate, and aluminum nitrate nonahydrate in water to obtain solution A. In solution A, Ni 2+ , Mg 2+ and Al 3+ The concentrations are 0.05-0.2mol / L, 0.1-0.6mol / L, 0.1-0.3mol / L respectively; Sodium hydroxide and sodium carbonate are dissolved in water to obtain solution B, the concentration of sodium hydroxide and sodium carbonate in solution B 0.5-1.0mol / L and 0.1-0.5mol / L respectively.
[0043] (2) Add solution A and solution B dropwise into the reactor under continuous stirring, control the pH of the resulting mixed solution at 9.0-10.0, and react at 25-35°C, and perform aging for 6-12 hours after the dropwise addition.
[0044] (3) Filter the reaction solution obtained in step (2), and wash the filter cake with water until neutral.
[0045] (4) Dry the solid obtained in step (3) at 50-70°C to obtain Ni x Mg 6-x...
Embodiment 1
[0054] 3.63g Ni(NO 3 ) 2 ·6H 2 O, 16.03g Mg(NO 3 ) 2 ·6H 2 O, 9.38g Al(NO 3 ) 3 9H 2 O was dissolved in 200mL deionized water, stirred and dissolved to obtain solution A; 6.4g NaOH and 5.3g NaOH 2 CO 3 Dissolve in 200mL deionized water, stir and dissolve to obtain solution B; titrate solution A and solution B into the beaker at the same time under constant stirring at 30°C, control the pH of the mixed solution within 9.0-10.0 during the titration process, after the titration is completed Aging at room temperature for 6-12 hours; suction filter and wash the obtained product to neutrality, and then dry it in an oven at 60°C for 12 hours; grind the dried precursor and place it in a crucible, and raise the temperature in an air atmosphere at 5°C / min to 400°C, calcined for 4 hours, and hydrogen reduced the calcined solid at 750°C to obtain Ni / Mg 5 Al 2 o 8 catalyst.
[0055] Get the catalyst 5.0g prepared by the above method and disperse in 100mL concentration of 30% 3...
Embodiment 2
[0060] With reference to the same catalyst preparation and reaction steps in Example 1, the difference is that Ni(NO 3 ) 2 ·6H 2 O mass 0.73-7.26g, Mg(NO 3 ) 2 ·6H 2 The mass of O is 12.84-18.62g, and the reaction time is 1.5h. The conversion rate of 3-hydroxybutyraldehyde and the yield of 1,3-butanediol under different catalyst compositions are shown in Table 2.
[0061] Table 2. Ni with different compositions x / Mg 6-x Al 2 o 9-x The conversion rate of 3-hydroxybutyraldehyde and the yield of 1,3-butanediol obtained under
[0062] catalyst Ni 0.2 / Mg 5.8 Al 2 o 8.8
[0063] The results of Table 2 show that in this catalyst, the most suitable metal ratio is Ni: Mg: Al=1: 5: 2 (molar ratio), and the Ni content is too low to make hydrogenation active sites less, resulting in 3-hydroxyl Butyraldehyde conversion decreased. Excessive Ni may agglomerate Ni particles and reduce the conversion rate of 3-hydroxybutyraldehyde.
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