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Regeneration method for palladium catalyst

The technology of a palladium catalyst and a solution is applied in the field of regeneration of palladium catalysts, and can solve the problems that the activity of the regenerated palladium catalyst cannot be reached, the activity of the palladium catalyst cannot reach the activity of the new palladium catalyst, and the regeneration is not thorough enough.

Active Publication Date: 2017-01-04
福建省福大百阳化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this invention has restored the activity of palladium catalyst to a certain extent, the regeneration of this method is not thorough enough and fails to solve the problem of catalyst activity reduction caused by the growth of palladium particles, resulting in the activity of regenerated palladium catalysts not reaching that of new palladium catalysts. At the same time, after repeated regenerations, the activity of the regenerated palladium catalyst cannot reach the necessary activity required for production, so it can only be scrapped

Method used

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  • Regeneration method for palladium catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] The regeneration method of the palladium catalyst of the present embodiment may further comprise the steps:

[0049] Pre-treatment: Sieve the spent palladium catalyst with a 10-mesh screen to remove particles with a particle size below 2mm to obtain the palladium catalyst to be regenerated.

[0050] Step 1: Weigh 100g of palladium catalyst to be regenerated (FAH-1Q fixed-bed palladium-alumina catalyst scrapped after 6 years of use) into a 500mL beaker, add 180mL of C 10 Aromatic hydrocarbons are soaked, and the aromatic hydrocarbons are separated after soaking for 30 minutes each time, and then the same amount of aromatic hydrocarbons as the first time is added, and soaked in this way for 9 times, and the aromatic hydrocarbons separated in the last time are light yellow;

[0051] Then add 160mL of sodium hydroxide (NaOH) solution with a concentration of 0.1mol / L and a temperature of 30-50°C to the palladium catalyst soaked in the above-mentioned aromatic hydrocarbons fo...

Embodiment 2

[0065] Repeat the step of embodiment one, just change the mol ratio of sodium chlorate and palladium into 1: 1.5 in wherein step 2, the mol ratio of sodium chlorate and hydrochloric acid is changed into 1: 10, promptly this example sodium chlorate consumption=0.000535614 ÷1.5×106.44÷0.99=0.0383911 (g), wherein 106.44 is the molar mass of sodium chlorate, and 0.99 is the purity of sodium chlorate, considering balance precision, getting 0.0384g) hydrochloric acid consumption is 0.000535614÷1.5×10÷0.012= 0.29756 (mL) is rounded to 0.30mL, the consumption of the sodium hydroxide that is used to regulate catalyst surface pH value still takes by weighing 0.06g in the ratio of embodiment one, the test method of palladium content, activity and compressive strength of catalyst is carried out Example 1 is carried out, and the data are shown in Table 1.

Embodiment 3

[0067] Repeat the step of embodiment one, just used Na when step 3 regulates catalyst surface pH value 2 CO 3 , the ionic equation of the hydrolysis of sodium carbonate is:

[0068] CO 3 2- +H 2 O==HCO 3- +OH -

[0069] HCO 3 - +H 2 OH 2 CO 3 +OH -

[0070] Visible 1 mole of sodium carbonate hydrolysis produces the alkalinity that is close to the alkalinity of 2 moles of sodium hydroxide, and setting sodium carbonate consumption is 0.10% of catalyzer weight (equivalent to NaOH consumption is 0.2% of catalyzer weight), for this reason Na 2 CO 3 Consumption=30×0.001÷0.995=0.03015(g), actually weigh 0.0302g, 0.995 is the NaOH purity, and the rest are carried out as in Example 1. The test data of palladium content, activity and compressive strength of the catalyst are shown in Table 1.

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Abstract

The invention provides a regeneration method for a palladium catalyst. According to the regeneration method, the palladium catalyst with the activity incapable of meeting the production requirements after being treated with the existing regeneration method can meet the requirement for activity or higher activity required by production. The regeneration method includes the following steps that 1, impurities are in a palladium catalyst needed to be regenerated are removed; 2, the palladium catalyst which is subjected to impurity removing is reacted with a sodium chlorate solution and hydrochloric acid; 3, the pH value of a solution reacted in the step 2 is adjusted to be 4 or above, and drying is carried out; 4, a sample dried in the step 3 is roasted.

Description

technical field [0001] The invention relates to the technical field of chemical production, in particular to a palladium catalyst regeneration method. Background technique [0002] In the production of hydrogen peroxide, palladium catalysts (Pd-Al 2 o 3 ), with the prolongation of the use time, its activity will gradually decrease. When the activity of the catalyst decreases to the point that it cannot maintain normal production, it must be activated and regenerated to restore most of the activity and meet the normal production requirements. At present, there are mainly three types of palladium catalyst regeneration: water vapor regeneration, aromatic hydrocarbon regeneration and oxidation liquid regeneration, or a combination of these methods. Among them, water vapor regeneration is the most commonly used method, that is, a large amount of water vapor is blown into the catalyst bed, and the organic matter and most of the inorganic salts attached to the catalyst surface ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/96
CPCB01J23/96B01J38/02B01J38/60B01J38/64
Inventor 王榕
Owner 福建省福大百阳化工科技有限公司
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