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Preparation method for activated-carbon-supported ruthenium-based ammonia synthesis catalyst

A technology of activated carbon and catalyst, which is applied in the field of preparation of activated carbon-supported ruthenium-based ammonia synthesis catalysts, which can solve the problems of reducing the ammonia synthesis performance of catalysts, affecting the dispersion of ruthenium metal and additives, and the decrease of dispersion, so as to achieve high ammonia synthesis reaction activity and Effect of heat resistance, good industrial application prospects

Inactive Publication Date: 2018-12-11
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During catalyst pretreatment and under ammonia synthesis reaction conditions, the number and properties of these oxygen-containing functional groups will change, which will affect the dispersion of ruthenium metal and additives, resulting in local enrichment of ruthenium metal and additives and a decrease in dispersion, thus Reduced ammonia synthesis performance of the catalyst

Method used

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  • Preparation method for activated-carbon-supported ruthenium-based ammonia synthesis catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take 5 g of activated carbon graphitized at 1850 °C in nitrogen, impregnate an equal volume of 0.05 g / mL ruthenium chloride solution to a mass ratio of Ru:C of 0.10:1, and dry at 120 °C for 4 hours; Reduction at 450°C for 6 hours, cooled to room temperature in the above atmosphere; the obtained sample was impregnated with barium nitrate aqueous solution until the molar ratio of Ba to Ru was 0.6:1, and dried at 120°C for 4 hours. Put the above sample in a tube furnace, pass through a mixed gas composed of nitric acid gas and oxygen-free gas at 300mL / min, and heat-treat at 80°C for 24 hours. In terms of volume percentage, the mixed gas is composed of: 3% nitric acid gas and 97% nitrogen gas.

Embodiment 2

[0017] Take 5g of activated carbon graphitized at 1850°C in nitrogen, impregnate an equal volume of 0.05g / mL ruthenium chloride solution to a mass ratio of Ru:C of 0.20:1, and dry at 120°C for 4 hours; Reduction at 450°C for 6 hours, cooled to room temperature in the above-mentioned atmosphere; the obtained sample was immersed in an aqueous potassium nitrate solution until the molar ratio of K to Ru was 1:1, and dried at 120°C for 4 hours. Put the above sample in a tube furnace, pass through 30mL / min of mixed gas composed of nitric acid gas and oxygen-free gas, and heat treat at 250°C for 1 hour. In terms of volume percentage, the mixed gas is composed of 90% nitric acid gas and 10% argon gas.

Embodiment 3

[0019] Take 5 g of activated carbon graphitized at 1850 °C in nitrogen, impregnate an equal volume of 0.015 g / mL nitrosoruthenium nitrate solution to a mass ratio of Ru:C of 0.3:1, and dry at 120 °C for 4 hours; Reduction at 450°C for 6 hours, and cooled to room temperature in the above atmosphere; the obtained samples were respectively impregnated with barium nitrate and potassium nitrate aqueous solutions until the molar ratios of Ba and K to Ru were 0.6:1 and 0.9:1 respectively, at 120 °C for 4 hours. Put the above sample in a tube furnace, pass through 900mL / min of mixed gas composed of nitric acid gas and oxygen-free gas, and heat treat at 150°C for 3 hours. In terms of volume percentage, the mixed gas is composed of: 20% nitric acid gas, 30% argon gas, and 50% nitrogen gas.

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Abstract

The invention discloses a preparation method for an activated-carbon-supported ruthenium-based ammonia synthesis catalyst. According to the preparation method, heat treatment is carried out on an activated-carbon-supported ruthenium-based catalyst containing an auxiliary for 0.2-30 hours in mixed gas composed of nitric acid gas and oxygen-free gas at 70-300 DEG C so as to obtain the activated-carbon-supported ruthenium-based ammonia synthesis catalyst, in the mixed gas, the volume ratio of the nitric acid gas is 1-90 vol%, the oxygen-free gas is mixed gas of nitrogen and one or more of zero-group inert gas in any proportion. Compared with the activated-carbon-supported ruthenium catalyst prepared through a traditional method, the catalyst has the advantages of being relatively high in ammonia synthesis activity and thermal stability and good in industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and relates to a noble metal catalyst supported by activated carbon and a preparation method thereof, in particular to a preparation method of an activated carbon-supported ruthenium-based ammonia synthesis catalyst. Background technique [0002] Supported ruthenium-based ammonia synthesis catalysts are known as the second-generation ammonia synthesis catalysts after iron catalysts because of their excellent performance. Among them, the ruthenium catalysts supported by activated carbon have high ammonia synthesis activity and have good industrial application prospects. . Under the conditions of high temperature and high pressure ammonia synthesis, the methanation reaction of ordinary activated carbon will lead to the loss of carbon carrier, which will cause the sintering of active components, thereby greatly reducing the ammonia synthesis activity and life of the catalyst, and affect...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/58B01J23/63B01J32/00C01C1/04
CPCB01J23/58B01J23/63B01J32/00C01C1/0411Y02P20/52
Inventor 林炳裕曹陈凤倪军林建新江莉龙
Owner FUZHOU UNIV
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