Regeneration method and application of inactivated vanadium-phosphorus-oxygen catalyst

A vanadium phosphorus oxide and catalyst technology, which is applied in catalyst regeneration/reactivation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of complex process, failure to achieve catalyst regeneration, and many solvents involved, so as to achieve regeneration The effect of using

Active Publication Date: 2020-09-25
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Hao Xicai and others disclosed the patent CN103789550A "Recovery method of vanadium, potassium and silicon in spent vanadium catalyst". The spent vanadium catalyst is first transferred to the leach solution by water leaching and acid leaching. Because trioctylamine (TOA) has excellent selectivity to vanadium , and then the vanadium is transferred to the extraction phase by TOA-secondary octanol-kerosene, and the extraction phase is back-extracted by a mixed solution of sodium hydroxide and sodium chloride, and then the vanadium pentoxide is finally recovered by the vanadium precipitation and roasting process. These two methods The recovery of vanadium can be realized, but because the process involves strong acid and strong alkali, the requirements for equipment materials are relatively high, which may easily cause equipment damage, and the process is complicated, involving too many solvents, which may easily produce hazardous waste solutions and cause secondary pollution, which does not meet the requirements Environmental protection and economic requirements, and catalyst regeneration in the true sense has not been realized

Method used

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  • Regeneration method and application of inactivated vanadium-phosphorus-oxygen catalyst
  • Regeneration method and application of inactivated vanadium-phosphorus-oxygen catalyst
  • Regeneration method and application of inactivated vanadium-phosphorus-oxygen catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The deactivated vanadium phosphorus oxygen catalyst was crushed by mechanical grinding, and the catalyst below 60 mesh was sieved, and the temperature was raised to 700°C in a muffle furnace and kept for 5 hours;

[0030] Take 10g of the calcined sample and stir evenly with 80mL of isobutanol, 20mL of benzyl alcohol, and 3.6mL of water, and stir at 135°C for 16h to obtain a light blue precursor solution, filter and separate, wash with ethanol, and dry at 120°C for 12h to obtain light blue colored solid powder;

[0031] 20-40 mesh catalyst particles are obtained through molding, granulation, and sieving processes. After filling, under the atmosphere of butane mixed gas (butane 1.2-1.5%, oxygen 18-20%, nitrogen balance), the space velocity is 2000h -1 After activation at 430°C for 12h, it was evaluated at different temperatures of 400°C, 410°C, 420°C, and 430°C for 24h.

[0032] In this embodiment, the catalytic effect of the regenerated VPO catalyst and the deactivated ...

Embodiment 2

[0034] The deactivated VPO catalyst was crushed by mechanical grinding, and the part below 60 mesh was sieved, and the temperature was raised to 700°C in a muffle furnace and kept for 5 hours;

[0035] Take 10 g of the roasted sample and stir evenly with 80 mL of isobutanol and 20 mL of benzyl alcohol, and stir at 135 ° C for 16 hours. During this period, when the mixed solution gradually changes from dark green to dark gray (after about 10 minutes of reflux stirring), add 3.6 mL of water dropwise. A light blue precursor solution was obtained, separated by filtration, washed with ethanol, and dried at 120°C for 12 hours to obtain a light blue solid powder;

[0036] 20-40 mesh catalyst particles are obtained through molding, granulation, and sieving processes. After filling, in the atmosphere of butane mixed gas (1.2-1.5% butane, 18-20% oxygen, nitrogen balance) atmosphere, the space velocity is 2000h -1 , After activation at 430°C for 12h, evaluate at different temperatures of...

Embodiment 3

[0038] The deactivated VPO catalyst was crushed by mechanical grinding, and the part below 60 mesh was sieved, and the temperature was raised to 700°C in a muffle furnace and kept for 5 hours;

[0039] Take 10 g of the calcined sample and stir evenly with 80 mL of isobutanol and 20 mL of benzyl alcohol, and stir at 135 ° C for 16 hours. During this period, when the mixed solution gradually changes from dark green to dark gray (after about 10 minutes of reflux and stirring), add 3.6 mL of water and 0.5mL phosphoric acid (mass fraction: 85%) to obtain a light blue precursor solution, filter and separate, wash with ethanol, and dry at 120°C for 12h to obtain a light blue solid powder;

[0040] 20-40 mesh catalyst particles are obtained through molding, granulation, and sieving processes. After filling, under the atmosphere of butane mixed gas (butane 1.2-1.5%, oxygen 18-20%, nitrogen balance), the space velocity is 2000h -1After activation at 430°C for 12h, it was evaluated at di...

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Abstract

The invention relates to a regeneration method of an inactivated vanadium-phosphorus-oxygen catalyst. The regeneration method comprises the following steps: crushing the inactivated vanadium-phosphorus-oxygen catalyst, and roasting the catalyst at 550-750 DEG C in an air or oxygen atmosphere for 3-10 hours to obtain a roasted product; adding the roasted product into a mixed solvent containing isobutanol and benzyl alcohol, carrying out heating to 110-140 DEG C for refluxing, and keeping heating for 10-16 hours to obtain a reaction solution, wherein water is added into the mixed solvent; and filtering the reaction solution, carrying out washing with alcohol, conducting drying, and activating a product at 400-430 DEG C for 12-36 hours to obtain the regenerated vanadium-phosphorus-oxygen catalyst. According to the method, regeneration of the catalyst is achieved in a crystalline phase adjusting mode, cost is low, effect is good, and important application value is achieved.

Description

technical field [0001] The invention belongs to the field of regeneration of chemical resources, and relates to a regeneration method and application of a deactivated vanadium-phosphorus-oxygen catalyst. Background technique [0002] Vanadium phosphate oxide (VPO) catalyst is mainly used to catalyze the reaction of butane oxidation to maleic anhydride. The active phase is mainly vanadyl pyrophosphate. After deactivation, some vanadyl phosphate is produced, and the catalyst strength decreases, but the main crystal phase is still pyrophosphate oxygen. Vanadium, currently the catalyst is the most effective catalyst to catalyze the oxidation of butane to maleic anhydride. The production of VPO catalyst will consume a large amount of vanadium resources every year, and vanadium, as a strategic resource of the country, is mainly used in steel production. With the continuous deepening of research on redox flow batteries (VRFB), this part of investment may further increase in the fut...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J38/02B01J27/198C07D307/60
CPCB01J27/198B01J27/285B01J38/02C07D307/60Y02P20/584
Inventor 刘瑞霞张永康周志茂代飞董洁张瑞锐张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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