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Process for preparation of palladium/carbon catalysts
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A technology of carbon catalyst and oxidant, which is applied in the direction of catalyst activation/preparation, preparation of organic compounds, physical/chemical process catalysts, etc. It can solve the problems of complex preparation process, large equipment investment, and many washing steps, etc., and achieve simple preparation process , high activity and long service life
Inactive Publication Date: 2009-12-09
大连科诺催化有限公司
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Problems solved by technology
The existing problems are: the preparation process is complicated, there are many washing steps, and the water consumption is large. The pickling, dipping, reduction, drying and other processes are all carried out under certain temperature conditions, and corresponding equipment suitable for the process is required, and the investment in equipment is large.
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Embodiment 1
[0021] 1. Wash with water. Weigh 100g of 4-8 mesh activated carbon into the reactor, wash with water 3 times, use 300mL water for the first time, and 200mL water for the last two times, soak for 30 minutes each time, accompanied by stirring, and the washing water is discharged through the switch valve.
[0022] 2. Pickling. Add 200mL of hydrochloric acid solution with a concentration of 0.01N into the reactor, soak for 1 hour, accompanied by slight stirring, and let off the hydrochloric acid solution after washing.
[0023] 3. Impregnated adsorption. Mix 50 grams of palladium compound solution (containing 0.5 grams of palladium according to the preparation conversion) with 5 mL of 30% hydrogenperoxide, the molar ratio of metal palladium to oxidant is 1:10, dilute to 120 mL with water, stir and pour into the reactor, and soak for 0.5 hours. Drain the soaking solution.
[0030] 3. Impregnated adsorption. Mix 50 grams of palladium compound solution (containing 0.5 grams of palladium according to the preparation conversion) with 10 mL of 30% hydrogenperoxide, the molar ratio of metal palladium to oxidant is 1:20, and soak for 1 hour.
[0032] 5. Restore. Use 2 times the calculated amount of HCOONa, soak and reduce for 20 hours.
[0033] 6. Washing.
[0034] Parts not described in detail in this embodiment are the same as those in Embodiment 1.
Embodiment 3
[0036] 1. Wash with water.
[0037] 2. Pickling. Soak in 0.25N hydrochloric acid solution for 3 hours.
[0038] 3. Impregnated adsorption. Mix 50 grams of palladium compound solution (containing 0.5 grams of palladium according to the preparation conversion) with 15 mL of 30% hydrogenperoxide, the molar ratio of metal palladium to oxidant is 1:30, and soak for 2 hours.
[0040] 5. Restore. Use 4 times the calculated amount of HCOONa, soak and reduce for 15 hours.
[0041] 6. Washing.
[0042] Parts not described in detail in this embodiment are the same as those in Embodiment 1.
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Abstract
The invention relates to a preparation method of a palladium / carbon catalyst, which comprises the following process steps: washing and pickling a carrier with water; palladium adsorption, mixing a palladium compound solution and an oxidant, and the molar ratio of the metal palladium to the oxidant is 1:10~ 110, dipping or spraying the activated carbon with the mixed solution; neutralizing with alkali, so that the pH value of the liquid reaches 4.0~8.0; reducing, reducing the palladium in the palladium compound adsorbed on the activated carbon to metal palladium, and the amount of the reducing agent is a reducing equivalent of 1 to 10 times; washing with water to remove chloride ions to obtain catalyst products. The above steps are carried out in the same reactor at room temperature. The invention is characterized in that the preparation process is simple, the energy saving and water saving effects are remarkable, and the competitive adsorption of the impregnated material is realized, so that the active component of metal palladium can be evenly distributed on the activated carbon, and the obtained catalyst has small crystal grains, high activity and long service life.
Description
technical field [0001] The invention relates to a preparation method of a catalyst, in particular to a preparation method of a palladium / carbon catalyst used for hydrogenation refining of crude terephthalic acid. Background technique [0002] The palladium / carbon catalyst commonly used in the hydrogenation process of crude terephthalic acid, whether it is prepared by impregnation method or spraying method, the conventional process steps are: 1. Wash the activated carbon with water to remove the dust and loose parts on the surface of the carbon; 2. 1. Pickling the activated carbon, adjusting the structure of the functional group on the surface of the activated carbon by pickling; 3. Washing the activated carbon with water to neutrality; 4. Drying treatment; 5. Adsorbing palladium, using the impregnation method or spraying method to make the palladium distributed on the carrier activated carbon 6. Water washing and neutralization; 7. Reduction, add a reducing agent, and carry ...
Claims
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