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Hydroxyl activated carbon supported palladium catalyst and preparation method thereof

A technology of palladium catalyst and activated carbon, which is applied in the field of hydroxyl activated carbon-supported palladium catalyst and its preparation, can solve the problems of low selectivity and conversion rate of palladium carbon, easy deactivation of nickel-based catalyst, high cost, etc., and achieve enhanced force and good adhesion The effect of point position and high utilization rate

Active Publication Date: 2020-10-30
GANNAN NORMAL UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there are two main methods for synthesizing 1,3-cyclohexanedione, one of which uses resorcinol as a raw material and undergoes hydrogenation reduction. Because the process is simple and environmentally friendly, it has become a common process in the world. The catalysts mainly focus on palladium carbon, nickel-based catalysts and platinum carbon, but the main problems of this kind of catalysts are: the selectivity and conversion rate of palladium carbon are low; nickel-based catalysts are easy to deactivate; The cost of the two catalysts is higher

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  • Hydroxyl activated carbon supported palladium catalyst and preparation method thereof
  • Hydroxyl activated carbon supported palladium catalyst and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1, a kind of preparation method of hydroxyl activated carbon supported palladium catalyst, its steps are as follows:

[0025] Step 1, the preparation of sodium zincate modified activated carbon,

[0026] a) treating activated carbon, treating the activated carbon with nitric acid with a mass fraction of 5% at a temperature of 80° C. for 2 hours, and washing it into neutrality;

[0027] b) To prepare sodium zincate solution, mix 0.1g of sodium hydroxide per 100mL of deionized water for preparation, dissolve sodium hydroxide in the corresponding amount of deionized water, add excess zinc powder, and react at a temperature of 40°C 1h, and then filter to remove insolubles to obtain a clear filtrate;

[0028] c) The activated carbon obtained in the above a) and the sodium zincate solution obtained in the above b) are made into a slurry, stirred at 60° C. for 20 min, then filtered, repeated stirring and filtering 3 times, and finally washed with deionized water un...

Embodiment 2

[0030] Embodiment 2, a kind of preparation method of hydroxyl activated carbon supported palladium catalyst, its steps are as follows:

[0031] Step 1, the preparation of sodium zincate modified activated carbon,

[0032] a) treating activated carbon, treating the activated carbon with nitric acid with a mass fraction of 5% at a temperature of 80° C. for 2 hours, and washing it into neutrality;

[0033] b) To prepare sodium zincate solution, mix 0.2g of sodium hydroxide per 100mL of deionized water for preparation, dissolve sodium hydroxide in corresponding amount of deionized water, add excess zinc powder, and react at a temperature of 40°C 1h, and then filter to remove insolubles to obtain a clear filtrate;

[0034] c) The activated carbon obtained in the above a) and the sodium zincate solution obtained in the above b) are made into a slurry, stirred at 60° C. for 20 min, then filtered, repeated stirring and filtering 3 times, and finally washed with deionized water until ...

Embodiment 3

[0036] Embodiment 3, a kind of preparation method of hydroxyl activated carbon supported palladium catalyst, its steps are as follows:

[0037] Step 1, the preparation of sodium zincate modified activated carbon,

[0038] a) treating activated carbon, treating the activated carbon with nitric acid with a mass fraction of 5% at a temperature of 80° C. for 2 hours, and washing it into neutrality;

[0039] b) To prepare sodium zincate solution, mix 0.5g of sodium hydroxide per 100mL of deionized water for preparation, dissolve sodium hydroxide in the corresponding amount of deionized water, add excess zinc powder, and react at a temperature of 40°C 1h, and then filter to remove insolubles to obtain a clear filtrate;

[0040]c) The activated carbon obtained in the above a) and the sodium zincate solution obtained in the above b) are made into a slurry, stirred at 60° C. for 20 min, then filtered, repeated stirring and filtering 3 times, and finally washed with deionized water unt...

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Abstract

The invention relates to a hydroxyl activated carbon loaded palladium catalyst. The hydroxyl activated carbon loaded palladium catalyst consists of sodium zincate modified activated carbon and palladium, wherein the mass load quantity of the palladium is 5 percent based on the mass of the activated carbon. The preparation method of the hydroxyl activated carbon loaded palladium catalyst comprisesthe following steps: preparing the sodium zincate from sodium hydroxide and metal zinc powder and modifying the activated carbon by the sodium zincate; and preparing slurry from the activated carbon modified by the sodium zincate, adding the slurry into a palladium chloride solution of 10 g / L, adjusting the pH of the solution to 9.0 by alkali liquid, continuously stirring for 1 hour, adding a formaldehyde solution into the slurry, adding the alkali liquid, maintaining the pH of the solution to 10, heating to 80 DEG C, performing heat preservation for 2 hours, and filtering and washing until that the solution does not have chloridions through AgNO3 solution detection. The catalyst is suitable for reaction for preparing 1,3-cyclohexanedione by resorcinol, can greatly improve the activity ofthe palladium carbon catalyst and increase the application times, and has good practical value.

Description

technical field [0001] The invention belongs to the technical field of preparation of noble metal catalysts, and in particular relates to a palladium catalyst supported on hydroxyl activated carbon and a preparation method thereof. Background technique [0002] Activated carbon is a porous inert material with a rich pore structure and a huge specific surface area. Due to the existence of unsaturation of activated carbon atoms, they will chemically combine atoms and atomic groups other than carbon components to form various surface functional groups. The type and quantity of activated carbon surface functional groups determine the surface chemical properties of activated carbon. The chemical properties determine the surface adsorption characteristics of activated carbon. Most of the studies on activated carbon gas phase adsorption show that in this type of interaction, the pore morphology (surface area and pore size distribution) of activated carbon is the main parameter. I...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/60B01J37/02C07C45/51C07C49/403
CPCB01J23/60B01J37/0207C07C45/512C07C49/403
Inventor 卢新宁高艳妮郁丰善李阳明刘建萍谢永荣华德润李剑李永敏程龙
Owner GANNAN NORMAL UNIV
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