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Preparation method of hydrogenation catalyst

A hydrogenation catalyst and catalyst technology, applied in the direction of hydrogenation hydrocarbon production, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of uneven distribution of carrier surface, difficulty of complete impregnation, waste of utilization rate, etc., and achieve inhibition of polymerization , reduce production costs, and inhibit the effect of polymerization

Active Publication Date: 2013-05-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the hydrophobicity of activated carbon, it is particularly difficult to completely soak into the aqueous solution of inorganic palladium salt, so that the palladium active component cannot completely enter the deep pores of the carrier, and the utilization rate has a certain waste. The Pd / C catalyst prepared by inorganic palladium salt needs 350-550 ℃ high-temperature roasting, the formed active palladium grains are easy to accumulate to form larger grains, which makes the surface distribution of the carrier uneven, and the catalyst still contains a small amount of chloride ions or nitrate ions. The existence of these inorganic acid ions will make the catalyst It has a certain acidity and affects the activity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] a. Activated carbon carrier pretreatment

[0026] The carrier is coconut shell activated carbon with a particle size of 8-60 mesh, and its properties are as follows: the specific surface area is 968 m 2 / g, the pore volume is 1.15 ml / g, pH=4.7.

[0027] Prepare 200 milliliters of nitric acid and hydrogen peroxide mixed solution, wherein the concentration of nitric acid is 15wt%, and the concentration of hydrogen peroxide is 12wt%, and above-mentioned mixed solution is put into 2 liters of beakers, takes by weighing 100g gac and pours in the above-mentioned beaker, after stirring gently, Stand at room temperature for 4 hours, remove the residual liquid by filtration, wash with distilled water until neutral, and dry at 105°C for 4 hours.

[0028] b. Preparation of active component impregnation solution

[0029] Accurately weigh 1.073 g of palladium acetylacetonate in a 200 ml beaker, add organic solvent chloroform to dissolve, adjust the pH value of the impregnation sol...

Embodiment 2

[0033] a, with embodiment 1

[0034] b. Preparation of active component impregnation solution

[0035] Accurately weigh 1.073 g of palladium acetylacetonate in a 200 ml beaker, add the organic solvent chloroform to dissolve, adjust the pH value of the impregnation solution to 5 with formic acid, and prepare an impregnation solution containing 0.25 wt% palladium.

[0036] c. Loading active components

[0037] Catalyst design loads palladium amount 0.4wt%, measures 17 milliliters of impregnating solution containing palladium 0.25wt% in 200 milliliters beaker, makes palladium amount be 1.06 times of catalyst design load palladium weight, gets 10g above-mentioned pretreated active carbon and pours wherein, Stir lightly, let stand for 4 hours, filter to remove the residual liquid, dry at 110°C for 6 hours, and roast at 180°C for 6 hours to obtain the finished catalyst D-2.

Embodiment 3

[0039] a, with embodiment 1

[0040] b. Preparation of active component impregnation solution

[0041] Accurately weigh 1.073 g palladium acetylacetonate in a 200 ml beaker, add organic solvent benzene to dissolve, adjust the pH value of the impregnation solution to 4 with acetic acid, and prepare an impregnation solution containing 0.25 wt% palladium.

[0042] c. Loading active components

[0043] The amount of palladium loaded on the catalyst is 0.3wt%, and 13 milliliters of impregnation solution is taken in a 200 ml beaker, so that the amount of palladium is 1.08 times the weight of the palladium loaded on the catalyst, and 10 g of the above-mentioned pretreated activated carbon is poured into it, stirred gently, and allowed to stand After 7 hours, the residual liquid was removed by filtration, dried at 105°C for 4 hours, and calcined at 200°C for 5 hours to obtain the finished catalyst D-3.

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Abstract

The invention discloses a preparation method of a hydrogenation catalyst. The hydrogenation catalyst takes activated carbon as a carrier, and adopts palladium as an active metal component. The catalyst has a palladium content of 0.1wt%-0.7wt%. An impregnation method is employed to prepare the catalyst. Specifically, a palladium-containing impregnation solution is prepared by: dissolving palladium acetylacetonate in an organic solvent, and using a low carbon organic carboxylic acid to regulate the pH value of the impregnation solution. The method adopts a special process to prepare the palladium acetylacetonate impregnation solution, can make palladium crystal grains highly dispersed and loaded on the inner and outer surfaces of the activated carbon carrier, and at the same time, no inorganic ion is introduced, no high-temperature roasting is needed, and migration and grain growth of the palladium metal are effectively controlled, thus improving the activity and selectivity of the catalyst. Moreover, the utilization rate of noble metal palladium is enhanced, noble metal waste is avoided, and the cost is reduced. The hydrogenation catalyst is applicable to a selective hydrogenation process of unsaturated C4 hydrocarbon fraction. The polymerization reaction of unsaturated hydrocarbon on the catalyst surface can be effectively inhibited, and the service life of the catalyst is prolonged.

Description

technical field [0001] The invention relates to a preparation method of a hydrogenation catalyst, in particular to a preparation method of a highly unsaturated C4 hydrocarbon fraction compound selective hydrogenation catalyst. Background technique [0002] 1,3-butadiene is an important raw material for synthetic rubber. The waste gas from rubber factories contains about 40 v% of 1,3-butadiene and about 10 v% of alkynes. Due to the high cost of separation, it is difficult to recycle. Burned as waste gas, causing environmental pollution and waste of valuable C4 hydrocarbon resources. If a selective hydrogenation catalyst can be developed to hydrogenate the above-mentioned gas into liquefied petroleum gas that can be directly used, the problem of utilization of waste gas from rubber factories can be solved. At present, dienes and alkynes in the C4 hydrocarbon fraction are mostly removed by selective hydrogenation, and the selected catalysts are mostly palladium-platinum-silver...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44C07C5/03C07C9/08C07C9/10C07C9/12
Inventor 宋丽芝王海波勾连科薛冬
Owner CHINA PETROLEUM & CHEM CORP
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