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A method for recycling hydrogenation catalyst waste

A technology for hydrogenation catalysts and waste materials is applied in the field of recycling and reuse of hydrogenation catalyst waste materials, which can solve problems such as affecting the physicochemical properties of catalysts, and achieve the effects of efficient recovery, high activity, and reduced viscosity and acidity.

Active Publication Date: 2019-10-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This scheme can only be applied to the preparation of catalyst by kneading method, and it will affect the physicochemical properties of the catalyst

Method used

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  • A method for recycling hydrogenation catalyst waste
  • A method for recycling hydrogenation catalyst waste
  • A method for recycling hydrogenation catalyst waste

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Hydrogenation catalyst waste (containing 12 wt% MoO 3 and 2.1 wt% CoO, the balance being alumina) and weighed 15g after passing through a 200-mesh sieve. Add it to 20g of water for dispersion, then add 15g of 30% nitric acid, 10.5g of 85% phosphoric acid, 7.5g of tartaric acid and 65g of mixed acid solution of water. At this time, the mass ratio of nitric acid-phosphoric acid-organic acid-waste material-water is 0.3:0.6:0.5:1:6.8. Then the temperature was raised to 90° C., and then kept at the temperature for 60 minutes. After cooling to room temperature, 3 g of monoethanolamine was added to obtain the final waste material sol slurry.

[0048] Put 105g of macroporous alumina powder (dry basis 85) in the rolling pan, and spray 80ml of 18.5g of cobalt nitrate and 3.0g of oxalic acid into the macroporous alumina powder in the rolling pan under the condition of rotation. Aqueous solution, after the solution is sprayed, continue to rotate in the rolling pot for 30 minutes,...

Embodiment 2

[0053] Hydrogenation catalyst waste (containing 22.5 wt%MoO 3 and 3.1 wt% CoO, the balance being alumina) and weighed 20g after passing through a 200-mesh sieve. Add to 25g water for dispersion, then add 40g of 30% nitric acid, 14.1g of 85% phosphoric acid, 4g of citric acid and 35g of mixed acid solution of water. At this time, the mass ratio of nitric acid-phosphoric acid-organic acid-waste material-water is 0.6:0.6:0.2:1:4.5. Then heat up to 90°C and keep the temperature for 60 minutes, then add 4g of ethylenediamine after cooling to room temperature to obtain the final waste material sol slurry.

[0054] Put 172g of macroporous alumina powder (dry basis 85) in the rolling pan, and spray 140ml of 32g of cobalt nitrate and 1.9g of citric acid into the macroporous alumina powder in the rolling pan under the condition of rotation. Aqueous solution, after the solution is sprayed, continue to rotate in the rolling pot for 30 minutes, then place it for 3 hours, dry it at 110°C ...

Embodiment 3

[0059] Hydrogenation catalyst waste (containing 18.7 wt%MoO 3 and 2.8 wt% CoO, the balance being alumina) and weighed 18g after passing through a 200-mesh sieve. Add it to 18g of water for dispersion, then add 15g of 30% nitric acid, 10.6g of 85% phosphoric acid, 5.4g of malic acid and 50g of mixed acid solution of water. At this time, the mass ratio of nitric acid-phosphoric acid-organic acid-waste material-water is 0.25:0.5:0.3:1:4.45. Then the temperature was raised to 85° C., and then kept at the temperature for 60 minutes. After cooling to room temperature, 2 g of isopropylamine was added to obtain the final waste material sol slurry.

[0060] Put 100g of macroporous alumina powder (dry basis 85) in the rolling pan, and spray 80ml of 18.5g of cobalt nitrate and 3.5g of tartaric acid into the macroporous alumina powder in the rolling pan under the condition of rotation. Aqueous solution, after the solution is sprayed, continue to rotate in the rolling pot for 30 minutes,...

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Abstract

The invention discloses a recovery and reutilization method of a hydrogenation catalyst waste material. The method comprises the following contents of (1) crushing carriers and / or catalyst waste materials; then, selecting a sieve being 180 to 200 meshes for sieving; remaining the sieved powder for later use; (2) pulping the powder obtained in the step (1) for later use; obtaining slurry with the solid content being 15 to 55 weight percent; adding a nitric acid-phosphoric acid-organic acid solution under the stirring condition; raising the temperature to 65 to 100 DEG C; maintaining the constant temperature for 30 to 90min; cooling the materials to the room temperature; then, adding organic amine; performing uniform mixing; obtaining sol slurry of the waste material; (3) uniformly mixing waste material sol slurry, modified macroporous aluminum oxide powder, microporous aluminum oxide powder mixture and extrusion aids; performing mixed kneading, shaping, drying and roasting to obtain analuminum oxide carrier; (4) loading active ingredients to obtain hydrogenation catalysts. The method has the advantages that the hydrogenation catalyst waste material can be effectively recovered andreused; no waste water and waste slag are generated; no environment pollution exists; meanwhile, the catalyst obtained by the method has high catalysis activity.

Description

technical field [0001] The invention relates to a recycling method for hydrogenation catalyst waste materials. Background technique [0002] As the world's crude oil production is becoming more and more heavy, and the demand for clean oil products is increasing today, in the process of producing clean oil products, the hydrodesulfurization process technology of petroleum fractions plays an increasingly important role. The demand for hydrogen catalysts is also increasing. [0003] Usually, the carrier of the hydrogenation catalyst is activated alumina, and the metal components are non-noble metals. Generally, the metals of Group VIB and / or Group VIII are the active components. The metals of Group VIB are generally Mo and W, and the metals of Group VIII are generally Co, Ni. [0004] During the preparation of hydroprocessing catalysts, residues and wastes are generated in the form of raw materials, intermediate process products and catalyst residues. Because industrial wast...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/882B01J23/94C10G45/08
Inventor 孙进郭蓉周勇杨成敏段为宇姚运海丁莉刘丽
Owner CHINA PETROLEUM & CHEM CORP
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