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Supported palladium/carbon catalyst for hydrogen refining and method for preparing the same

A technology of carbon catalyst and supported palladium, applied in the field of supported palladium/carbon catalyst and its preparation, can solve the problems of low carboxybenzaldehyde conversion rate, low Pd dispersion, poor thermal stability, etc., and achieve easy environmental protection treatment and use The effect of long life and high dispersion

Inactive Publication Date: 2009-07-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] One of the technical problems to be solved by the present invention is that the Pd dispersity of the Pd / C catalyst in the prior art is low, the crystallite content is low, the thermal stability is poor, and the problem that the conversion rate of raw material is low to carboxybenzaldehyde provides a kind of new use Supported Palladium / Carbon Catalyst for Hydrofining

Method used

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  • Supported palladium/carbon catalyst for hydrogen refining and method for preparing the same
  • Supported palladium/carbon catalyst for hydrogen refining and method for preparing the same
  • Supported palladium/carbon catalyst for hydrogen refining and method for preparing the same

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Pass 100 grams through a 4-mesh sieve but remain on an 8-mesh sieve, specific surface 1100 m 2 The coconut shell activated carbon per gram was washed with 200 milliliters of 0.4 mol / liter nitric acid aqueous solution for 2 hours. After removing the acid solution, the activated carbon was washed with deionized water until neutral, and then dried at 120° C. for 6 hours.

[0046] Preparation of Pd solution. Get 3.2 grams of palladium-containing 16% by weight chloropalladium acid aqueous solution, add deionized water to 40 milliliters, then add 2.16 grams of 10 weight percent additive A1 aqueous solution therein, and add deionized water until the solution volume is 60 milliliters, at this time The solution weighed 61 grams. After stabilizing for 180 minutes, add 10.3 grams of additive B and stir evenly. The above treated activated carbon was impregnated with the Pd-containing solution for 3 hours to obtain a catalyst precursor. The catalyst precursor was aged at room te...

Embodiment 2~11

[0048] Select different Pd compounds and different additives to prepare Pd-containing solutions, and the rest are the same as [Example 1]. The specific Pd compound, the content of the Pd compound in the Pd-containing solution (calculated as Pd), the specific additive, the molar ratio of additive A to Pd, and the weight percentage of additive B in the Pd solution are listed in Table 1.

Embodiment 12~18

[0050] According to the procedure of [Example 1], but select different additives to prepare the Pd-containing solution (see Table 1 for specific additives), and spray the Pd-containing solution on the activated carbon to obtain the catalyst precursor. In addition, the inorganic acid, the concentration of the inorganic acid, the pickling time, the drying time, the temperature, the reducing agent, the reducing treatment temperature and the reducing treatment time as shown in Table 2 were employed.

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Abstract

The invention relates to a load type palladium / carbon catalyst used for hydrogen refining and a preparation method, mainly solving the problems in the prior art that Pd dispersity of Pd / c catalyst is low, microcrystal content is low, thermal stability is weak, and conversion rate of p-carboxyl benzaldehyde raw material is low . In the invention, palladium loaded on carrier active carbon is in microcrystal form, wherein the microcrystal less than 2.5 nanometer accounts for 90wt% of the total weight of the microcrystal palladium, and solution used for dipping or spraying the active carbon carrier contains Pd compound. In a COOH(CH2)nCOOH additive and a BCH3(CH2)m(CH3)3NBr additive, n is an integer ranging from 0 to 3 and m is an integer ranging from 8 to 20, wherein, the technical proposal that m is an integer ranging from 8 to 20 well solves the problems. The invention can be applied to the industrial production of terephthalic acid hydrobon catalyst.

Description

technical field [0001] The invention relates to a supported palladium / carbon catalyst for hydrofinishing and a preparation method thereof. Background technique [0002] Supported palladium / carbon catalysts are widely used for the selective hydrogenation of unsaturated organics. In particular, the supported palladium / carbon catalyst is suitable for the purification of crude terephthalic acid, wherein certain impurities in crude terephthalic acid such as p-carboxybenzaldehyde (4-CBA for short) are converted into other compounds by hydrogenation , and then the terephthalic acid product can be separated and purified by crystallization. Because palladium / carbon catalyst usually adopts a single active component, its improvement research in the prior art mainly focuses on the structure of the support and the distribution of metal Pd on the support, and these aspects will indeed have a great impact on the performance of the catalyst. Impact. [0003] Since the terephthalic acid h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10G45/04
Inventor 钱斌杨为民畅延青陈大伟
Owner CHINA PETROLEUM & CHEM CORP
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