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A kind of preparation method of palladium/carbon catalyst for selective hydrogenation with low loading ultra-small size
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A carbon catalyst, small size technology, applied in the field of palladium/carbon catalyst preparation, can solve the problems of large crystallite size, low Pd dispersion, low activity, etc., achieve small crystallite size, prevent agglomeration, and improve microporous structure Effect
Active Publication Date: 2016-01-20
SHENYANG RES INST OF NONFERROUS METALS
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[0011] The object of the present invention is just to solve the problem that prior art exists, promptly the Pd dispersity that exists in terephthalic acid hydrogenation palladium / carbon catalyst in known technology is low and crystallite size is too big, the problem that the activity caused is low , and provide a new low-load ultra-small size selective hydrogenation palladium / carbon catalyst preparation method
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Embodiment 1
[0039] 100g 4-8 mesh, specific surface area 1200m 2 Wash and soak 1.2mol / L nitric acid solution per gram of coconut-type activated carbon for 2 hours, then wash with water until neutral, dry at 110°C for 5 hours, soak in 263ml of 1.5g / L sodium borohydride aqueous solution, stir and impregnate, is solution A;
[0040] Weigh 0.59g palladium chloride and 0.087g additive A (additive A:Pd atomic molar ratio=0.3), dissolve in 0.5ml concentrated hydrochloric acid, add a small amount of water, stir and dissolve, then slowly add in the A solution to adjust the pH value of the solution to 7, stirred and reacted at 40°C for 3 hours, washed with pure water until neutral, and dried to obtain a catalyst product with a Pd content of 0.35%.
Embodiment 2
[0042] 100g 4-8 mesh, specific surface area 1200m 2 / g of coconut-type activated carbon was washed and soaked with 0.6mol / L hydrochloric acid solution for 2 hours, then washed with water until neutral, dried at 110°C for 5 hours, soaked in 200ml of 0.037wt.% formaldehyde solution, stirred and impregnated to obtain solution A ;
[0043] Weigh 0.34g of palladium chloride and 0.24g of additive B (additive B:Pd atomic molar ratio=1.2), dissolve in 0.4ml of concentrated hydrochloric acid, add a small amount of water, stir and dissolve, then slowly add to solution A to adjust the pH value of the solution to 9, stirred and reacted at 80°C for 8 hours, washed with pure water to neutrality, and dried to obtain a catalyst product with a Pd content of 0.20%.
Embodiment 3-10
[0045] According to each step and condition of embodiment 1, select different Pd-containing compounds and additives to prepare palladium-containing solution, change reducing agent, reduction pH value, reduction temperature, reduction time in addition, all the other are the same as embodiment 1, the conditions of change are shown in table 1.
[0046] Table 1 Example 3-10 Experimental conditions
[0047]
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Abstract
The invention relates to a preparation method of a low-loading-capacity ultra-small-size palladium / carbon catalyst for selective hydrogenation, and the preparation method is applicable to prepare a refined low-loading-capacity ultra-small-size loaded-type palladium / carbon catalyst for selective hydrogenation of crude terephthalic acid. The preparation method is characterized by comprising the following preparation steps: dipping an active carbon carrier subjected to acid washing or oxidation pretreatment in a reducing agent solution to obtain a reducing agent carrier solution, employing a palladium compound and an additive to prepare a palladium-containing solution, and slowly adding the palladium-containing solution into the reducing agent carrier solution to obtain the palladium / carbon catalyst. The prepared catalyst is high in ultra-small-size Pd microcrystalline content, low in Pd loading capacity and low in production cost, and also has the advantage of high 4-formylbenzoic acid conversion rate when the catalyst is applied to refining of crude terephthalic acid.
Description
technical field [0001] The invention relates to a preparation method of a palladium / carbon catalyst, in particular to a preparation method of a palladium / carbon catalyst for selective hydrogenation with a low-load ultra-small size, which is suitable for selective hydrogenation and refining of crude terephthalic acid Used in the preparation of low-load ultra-small-sized supported palladium / carbon catalysts. Background technique [0002] Supported palladium / carbon catalysts are mainly used for the selective hydrogenation of unsaturated organics, especially for the production of purified terephthalic acid (PTA). At present, most of the production of PTA in my country has introduced the high-temperature oxidation process of Amoco Company in the United States, which mainly includes two main processes: p-xylene (PX) oxidation and crude terephthalic acid (CTA) refining. The CTA produced by the air oxidation of p-xylene contains the incompletely oxidized intermediate product p-carb...
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