Preparation method and application of ruthenium catalyst for synthesizing 1,4-cyclohexanedicarboxylic acid
A technology of cyclohexanedicarboxylic acid and ruthenium catalysts, which is applied in the preparation and application field of ruthenium catalysts for the synthesis of 1,4-cyclohexanedicarboxylic acid, and can solve the problems of low hydrogenation activity, small particle size, easy agglomeration and deactivation, etc. problem, to achieve the effect of increasing utilization rate, reducing reaction temperature and pressure
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Embodiment 1
[0032] (1) Preparation of catalyst:
[0033] Add 100ml of water, 0.75g of 10% ruthenium trichloride, 0.52g of copper chloride dihydrate, and 5g of polyvinylpyrrolidone (PVP) into a four-neck flask, stir and reflux for 0.5 hours to fully dissolve them. After cooling, add 30g of 7wt% potassium borohydride aqueous solution dropwise in an ice-water bath for about 0.5 hours. After the dropwise addition, continue to stir for 0.5 hours; add 8.5g of 28% concentrated ammonia water; while stirring, add 6.25g of ethyl silicate dropwise After the dropwise addition was completed within 15 minutes, 7.5 g of titanium dioxide carriers were added, and the stirring was continued for 0.5 hours; the resulting solution was added to an autoclave, heated to 120° C., 1 MPa of hydrogen gas was introduced, treated for 2 hours, and centrifuged to obtain 15 g of catalyst slurry.
[0034] (2) Synthesis of 1,4-cyclohexanedicarboxylic acid by hydrogenation of terephthalic acid:
[0035]Add 15g of the catal...
Embodiment 2
[0040] (1) Preparation of catalyst:
[0041] Add 100ml of water, 0.75g of 10% ruthenium trichloride, 0.52g of copper chloride dihydrate, and 5g of polyvinylpyrrolidone (PVP) into a four-neck flask, stir and reflux for 0.5 hours to fully dissolve them. After cooling, add 30 g of 7wt% potassium borohydride aqueous solution dropwise in an ice-water bath for about 0.5 hours. After the dropwise addition, continue to stir for 0.5 hours; add 10 g of titanium dioxide carriers and continue to stir for 0.5 hours; add the resulting solution to the autoclave and heat up to At 120°C, 1 MPa of hydrogen gas was introduced, treated for 2 hours, and 15 g of the catalyst slurry was centrifuged.
[0042] (2) Synthesis of 1,4-cyclohexanedicarboxylic acid by hydrogenation of terephthalic acid:
[0043] Add 15g of the catalyst slurry prepared in the above step (1), 400g of water, and 50g of terephthalic acid into a 500ml hydrogenation kettle, heat up to 90°C, inject 3MPa hydrogen gas, and carry ou...
Embodiment 3
[0048] (1) Preparation of catalyst:
[0049] Add 100ml of water, 0.75g of 10% ruthenium trichloride, and 0.52g of copper chloride dihydrate into the four-neck flask, stir and reflux for 0.5 hour to fully dissolve them. After cooling, add 30g of 7wt% potassium borohydride aqueous solution dropwise in an ice-water bath for about 0.5 hours. After the dropwise addition, continue to stir for 0.5 hours; add 8.5g of 28% concentrated ammonia water; while stirring, add 6.25g of ethyl silicate dropwise After the dropwise addition was completed within 15 minutes, 7.5 g of titanium dioxide carriers were added, and the stirring was continued for 0.5 hours; the resulting solution was added to an autoclave, heated to 120° C., 1 MPa of hydrogen gas was introduced, treated for 2 hours, and centrifuged to obtain 15 g of catalyst slurry.
[0050] (2) Synthesis of 1,4-cyclohexanedicarboxylic acid by hydrogenation of terephthalic acid:
[0051] Add 15g of the catalyst slurry prepared in the above...
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