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Low load noble metal catalyst for dilute nitric acid reduction, preparation and application

A precious metal catalyst and dilute nitric acid technology, applied in the field of dilute nitric acid catalysis, can solve the problems of limited nitric acid conversion, low nitric acid concentration, high catalyst cost, etc., and achieve the effects of reduced production cost, good stability and good adaptability

Active Publication Date: 2019-03-08
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the concentration of nitric acid is too low, the reaction is more difficult
In the coal-to-ethylene glycol process, 2wt% dilute nitric acid is generated in the regeneration reaction kettle liquid, and the concentration of nitric acid is low, which limits the conversion of nitric acid
There are bibliographical reports using noble metal catalysts such as 3.5wt% Pd or Pt, which can effectively catalyze the reduction reaction of dilute nitric acid to generate nitrite, but the loading of noble metals is too high, and the catalyst cost is higher; 0.2-2% is used in the report of the patent (CN106565494A) Palladium is the active component, and 0-10% iron or titanium is the auxiliary agent. The prepared catalyst can effectively catalyze the reduction of dilute nitric acid, and the loading capacity of precious metals is reduced.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 0.259g of potassium nitrate solid, add 5.5g of deionized water to make an impregnation solution for additives; then take 5g of activated carbon particles between 14 mesh and 20 mesh, impregnate for 4 hours in equal volume, then dry at 100°C for 12 hours, N 2 Calcined at 200°C for 3 hours under protection to obtain a 2wt% K / AC standby sample.

[0024] Take 1.6ml of palladium nitrate solution (Pd content 4.688mg / mL) and add deionized water until the total mass of the mixed solution is 5.5g, configure it as an active component impregnation solution, take the K / AC prepared above, and impregnate it in equal volume for 4h, then Dry at 100°C for 12h, N 2 Burn at 300° C. for 3 h under protection to obtain a Pd-K / AC catalyst. The loading of Pd is 0.15%, and the loading of K is 2%. Catalyst A is recorded.

Embodiment 2

[0026] Adopt the method of embodiment 1, change the sodium nitrate of 0.259 potassium nitrate into 0.370, the mass content of Na is 2%, other remains unchanged, obtains Pd-Na / AC catalyst, the load of Pd is 0.15%, the load of Na The amount is 2%, and it is recorded as catalyst B.

Embodiment 3

[0028] Adopt the method of embodiment 1, change the amount of palladium nitrate solution, others remain unchanged, get respectively 0.53mL and 2.7mL palladium nitrate solution (Pd content 4.688mg / mL), make the loading capacity of auxiliary agent K respectively all be 2 %, and the catalysts with noble metal negative Pd loadings of 0.05% and 0.25%, respectively, are designated as Catalyst C and Catalyst D.

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Abstract

The invention provides a low load noble metal catalyst for dilute nitric acid reduction and belongs to the technical field of dilute nitric acid catalysis. Calculated as per the total mass of the catalyst, the catalyst comprises the following ingredients by mass percentage: 0.02-0.25% of active ingredient, 0.5-5% of assistant and the balance of carrier, wherein the active ingredient is one or moreof noble metals Pd, Pt and Rh; the assistant is an alkali metal element K or Na; and the carrier is active carbon. The invention further provides a preparation method of the catalyst, which comprisesthe steps: 1) preparing an assistant saline solution and an active ingredient saline solution in proportion, 2) loading the prepared assistant saline solution onto the active carbon carrier, and drying and roasting to form a standby sample, and 3) loading the prepared active ingredient saline solution onto the standby sample, and drying and roasting to form the catalyst. The loading capacity of noble metals in the catalyst is only 0.02-0.25%; when cost is lowered, the dilute nitric acid reduction can be effectively catalyzed to generate nitrous acid ester; a nitric acid conversion rate reaches above 90%; and nitrous acid ester selectivity reaches 100%.

Description

technical field [0001] The invention belongs to the technical field of dilute nitric acid catalysis, and specifically relates to a dilute nitric acid reduction low-load precious metal catalyst, its preparation and application. Background technique [0002] Ethylene glycol is a bulk chemical product and an important organic chemical raw material. my country has abundant coal resources, and the route of using coal to synthesize gas and oxalate to produce ethylene glycol is developing rapidly in my country. As of March 2018, a total of 17 coal (synthesis gas) to ethylene glycol (CTMEG) projects have been put into operation and successfully tested in China, forming a total ethylene glycol production capacity of 3 million tons per year. It is estimated that in 2022, together with the 17 projects that have been put into production and successfully tested, a total of about 13.5 million tons / year CTMEG production capacity will be formed. In the coal-to-ethylene glycol technical ro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/58C07C201/04C07C203/00
CPCB01J23/58C07C201/04C07C203/00
Inventor 李文龙宋元江李扬王科王雪峰董玲玉刘亚华
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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