Regeneration method of precious metal dehydrogenation catalyst

A technology for dehydrogenation catalysts and precious metals, applied in catalyst regeneration/reactivation, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc., can solve alkali metal loss, metal aggregation, alumina carrier crystal Phase transition and other issues, to achieve the effect of easy operation, small temperature change, and prolong service life

Inactive Publication Date: 2016-06-22
LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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Problems solved by technology

When these two methods are used for catalyst regeneration, water vapor is introduced, which will not only cause the crystal phase transformation of the alumina carrier, but also cause the loss of alkali metal in the low-carbon alkane catalyst, and also cause metal aggregation to a certain extent.
[0008] It can be seen from the above regeneration methods of noble metal-based dehydrogenation catalysts that oxygen, halogen or water vapor are usually purposefully introduced during the regeneration process, although the problems of carbon deposition, metal accumulation and alkali metal loss are solved to a certain extent , but it often brings other side effects, and the above three problems cannot be taken into account at the same time, which inevitably results in the performance and life of the low-carbon alkane dehydrogenation regeneration catalyst

Method used

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  • Regeneration method of precious metal dehydrogenation catalyst

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Effect test

Embodiment 1

[0027] Weigh commercially available alumina carrier (γ phase, spherical, diameter 0.5mm, pore volume 0.71cm 3 / g, specific surface area 224m 2 / g) 30g, add deionized water dropwise to initial moistening, and the volume of consumed water is 27mL. Based on the weight content of 0.4% of the Sn element in the final catalyst, stannous chloride containing 0.12 g of Sn was weighed and dissolved in ethanol, and the volume was adjusted to 27 mL with ethanol. The prepared Sn-containing ethanol solution was added to 30 g of alumina carrier, mixed evenly, and aged at room temperature for 2 hours. Dry at 80°C for 8h, then bake at 600°C for 4h.

[0028] Based on the weight content of 0.5% of the Pt element in the final catalyst, weigh 0.18g of Pt-containing chloroplatinic acid and dissolve it in deionized water, set the volume to 27mL, add it to the Sn-containing alumina carrier, mix well, and age at room temperature for 4h. Dry at 100°C for 6h, and bake at 600°C for 4h. The sample obta...

Embodiment 2

[0031] After the C-1 fresh agent reacted for 72 hours, switch the raw material gas to pure hydrogen gas, purging for 1 hour, then the temperature dropped to 450°C, the pressure rose to 8MPa, and then hydrogen and tetralin were introduced at the same time. The speed is 1.5h -1 , the volume ratio of hydrogen to tetralin is 350:1, and the treatment time is 3h. After the treatment is over, switch to nitrogen, drop to normal pressure, and drop to room temperature, and the volumetric space velocity is 8.0h -1 The deactivated catalyst was cleaned by passing through cyclohexane for 2 hours, and then purged at 100° C. for 3 hours in a nitrogen atmosphere. Under a nitrogen atmosphere, raise the temperature of the deactivated catalyst to 400°C, and then pass a mixed gas of oxygen and nitrogen, the oxygen volume content in the mixed gas is 0.3%, and the volume space velocity is 1000h -1 , the processing time is 12h.

[0032] After the deactivated catalyst is treated with low-concentrat...

Embodiment 3

[0035] After C-1 primary regenerant reaction for 72 hours, the raw material gas is switched to pure hydrogen gas, purging for 1 hour, then the temperature drops to 400 ° C, the pressure rises to 10 MPa, and then hydrogen and tetralin are introduced at the same time. The air speed is 2.0h -1 , the volume ratio of hydrogen to tetralin is 200:1, and the treatment time is 2h. After the treatment is over, switch to nitrogen, drop to normal pressure, and drop to room temperature, the volumetric space velocity is 10.0h -1 Pass through cyclohexane to wash the deactivated catalyst for 1 h, and then purge at 80° C. for 4 h in a nitrogen atmosphere. Under a nitrogen atmosphere, raise the temperature of the deactivated catalyst to 350°C, and then pass a mixed gas of oxygen and nitrogen, the oxygen volume content in the mixed gas is 0.5%, and the volume space velocity is 500h -1 , the processing time is 8h.

[0036] After the deactivated catalyst is treated with low-concentration oxygen...

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Abstract

The invention discloses a regeneration method of a precious metal dehydrogenation catalyst. The regeneration method mainly solves the problems that in the regeneration process of a light-alkane dehydrogenation catalyst, reactive metal accumulates and alkali metal is lost. The method comprises the following steps that 1, in hydrogen atmosphere, hydrogen supply solvent is used for treating a deactivated catalyst; 2, the deactivated catalyst treated in the step 1 is subjected to charking in mixed atmosphere containing low-concentration oxygen; 3, the deactivated catalyst treated in the step 2 is subjected to alkali metal additive supplementing treatment, and then roasted in air to obtain the regenerated catalyst. According to the regeneration method of the precious metal dehydrogenation catalyst, dehydrogenation activity of the regenerated catalyst can reach the level of a fresh catalyst, meanwhile, in the regeneration process, temperature changes little, operation is easy, and the service life of the catalyst is prolonged.

Description

technical field [0001] The invention relates to a regeneration method of a low-carbon alkane dehydrogenation catalyst, in particular to a regeneration method of a noble metal-based catalyst for propane and isobutane dehydrogenation. Background technique [0002] The shale revolution in North America has brought a large amount of low-carbon alkanes resources, resulting in the lightening of raw materials for ethylene crackers and a sharp drop in propylene production. At the same time, under the background of increasingly scarce petroleum resources, the production of propylene has changed from purely relying on petroleum as a raw material to diversifying the technical route of raw material sources, and it has gradually become a trend. Dehydrogenation of propane by-produced in natural gas (conventional natural gas, shale gas, coalbed methane, combustible ice, etc.) to produce propylene is an effective way to solve this problem. In recent years, the technology of propane dehydro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J38/58B01J38/64B01J23/62
CPCB01J23/626B01J38/58B01J38/64
Inventor 张海娟王卫强李剑虹王国付李小玲孙林
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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