CN108435166A - A kind of preparation method of free from chloride active carbon loading ruthenium ammonia synthesis catalyst - Google Patents
A kind of preparation method of free from chloride active carbon loading ruthenium ammonia synthesis catalyst Download PDFInfo
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- CN108435166A CN108435166A CN201810238806.2A CN201810238806A CN108435166A CN 108435166 A CN108435166 A CN 108435166A CN 201810238806 A CN201810238806 A CN 201810238806A CN 108435166 A CN108435166 A CN 108435166A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/46—Ruthenium, rhodium, osmium or iridium
- B01J23/462—Ruthenium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0213—Preparation of the impregnating solution
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/06—Washing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
- B01J37/18—Reducing with gases containing free hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/04—Preparation of ammonia by synthesis in the gas phase
- C01C1/0405—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
- C01C1/0411—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst characterised by the catalyst
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Abstract
A kind of preparation method of free from chloride active carbon loading ruthenium ammonia synthesis catalyst is related to one kind using ruthenic chloride as raw material, the preparation method of free from chloride ruthenium-based ammonia synthetic catalyst is made by handling removing chloride ion.The specific steps are using ruthenic chloride as raw material, standing, precipitation, washing, dissolving after addition water soluble alkali, free from chloride ruthenium presoma is obtained, loads on the activated carbon, then adds KNO3Auxiliary agent is to get to free from chloride active carbon loading ruthenium ammonia synthesis catalyst.Compared with ruthenium-based ammonia synthetic catalyst made from existing method, the present invention is using ruthenic chloride as raw material, cheap, preparation process is simple and convenient to operate, the loss of noble ruthenium is reduced in energy better removing chloride ion, preparation process, and catalyst activity obtained is higher.With good prospects for commercial application.
Description
Technical field
The present invention relates to the systems that a kind of ruthenium catalyst of nitrogen and hydrogen synthesis ammonia is used in the ammonia synthesizing industry of chemical fertilizer field
A kind of standby technology, and in particular to preparation method of no chlorine active carbon loading ruthenium ammonia synthesis catalyst.
Background technology
Ammonia synthesizing industry occupies very important status in national economy.Synthesis ammonia extreme portions are used to nitrogenous fertilizer, promote
Into the yield of grain, in addition to this in many Chemical Manufactures, ammonia is also indispensable important source material.Therefore, ammonia is synthesized
Invention, the development of technology have very great significance for mankind's tool.Currently used ammonia synthesis catalyst presoma is divided into two
Kind, chlorine-containing compound and without chlorine compound.If hydrate ruthenium trichloride is that more commonly the presoma of ruthenium containing chlorine, property are stablized, easily
It is dissolved in water, and price is cheaper than other ruthenium compounds, but the presence of chlorion can influence ammonia synthesis rate.
CN102580779A reports the ammonia synthesis catalyst and preparation method thereof that a kind of nitrosyl nitrate ruthenium is presoma, i.e., with ruthenium
Powder is blended in high-temperature process for raw material, by ruthenium powder and potassium nitrate and potassium hydroxide and potassium ruthenate intermediate is made, and then dissolving is made
It is simultaneously supported on absorbent charcoal carrier obtained activated carbon supported ruthenium catalyst by nitrosyl nitrate ruthenium.CN102698749A then will
Above-mentioned potassium ruthenate reacts the water-soluble ruthenium complex generated with ammonia and prepares ruthenium system ammonia synthesis catalyst using it as presoma.
Ruthenic acid aqueous solutions of potassium and polyhydroxy ethers, polyhydroxy aldehyde or polyhydroxyketone-aqueous solution are mixed to prepare polyhydroxy by CN102580778A
Ruthenium complex, to prepare free from chloride activated carbon supported ruthenium system ammonia synthesis catalyst.It must be with ruthenium powder in above-mentioned preparation method
For raw material, potassium ruthenate is prepared at high temperature, and condition is harsh, and preparation process is complicated.CN 1133492C are with Al2O3For carrier,
RuCl3It for presoma, after being immersed on carrier, is washed with aqueous slkali, then with hydrazine hydrate reduction, washing removes chlorion.CN
Ruthenium is impregnated on absorbent charcoal carrier by 101362080A using ruthenic chloride as raw material, then will by oxalates and alkaline precipitating agent
Ruthenium salt is with Ru (OH)4Or RuO2 2H2The form of O loads on activated carbon, and being washed with deionized to cleaning solution does not have chlorion.
Both techniques are provided prepares the method without chlorine ruthenium-based ammonia synthetic catalyst with ruthenic chloride.But ruthenic chloride is first supported on load
On body, it is washed with water removing chlorion, part ruthenium loss is had in washing process, is washed after load, the loss amount of ruthenium is maximum
It is likely to be breached 10%, is a huge waste for noble metal, and uses the method washed before load, ruthenium is in catalyst
In preparation process almost without what lose, remarkable in economical benefits, catalyst activity and stability can also stability contorting, urge
Agent product quality is more controllable；Moreover, because the hydroxyl of the chlorion and activated carbon surface in ruthenic chloride, the groups such as carboxyl combine
Intensity is larger, keeps the chlorion wash time after load very long, it is difficult to thoroughly remove chlorion to the greatest extent, cause chlorion to catalyst
Industrially the use of high-temperature high-pressure apparatus brings larger security risk.The present invention makes the presoma of catalyst of ruthenic chloride,
Chlorion is just removed before load, catalyst is avoided to occur safety problem in the application, improves the cost performance and product of catalyst
Quality.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to propose that a kind of presoma of ruthenium containing chlorine prepares the nothing of high activity
The method of chlorine active carbon loading ruthenium ammonia synthesis catalyst.The present invention uses ruthenic chloride for raw material, cheap, and cost is relatively low.
And it is not necessarily to hydrazine hydrate reduction process, simple for process, easy to operate, raw material free of losses.
To realize that goal of the invention, the present invention adopt the following technical scheme that：
A kind of preparation method of free from chloride active carbon loading ruthenium ammonia synthesis catalyst is added soluble using ruthenic chloride as raw material
It stands, precipitate after aqueous slkali, washing, dissolving, obtaining free from chloride ruthenium presoma, above-mentioned no chlorine ruthenium presoma is supported on activated carbon
It on carrier, restores in reducing atmosphere, then adds KNO3Auxiliary agent is to get to no chlorine ruthenium-based ammonia synthetic catalyst.
The water soluble alkali solution is one or more of lithium hydroxide, sodium hydroxide, potassium hydroxide aqueous solution.
The amount ratio of the substance of ruthenic chloride and water soluble alkali is 1:3~1:6.
The time of repose is 1-12h.
The washing methods is one kind in centrifugation, suction filtration, and cleaning solution is absolute ethyl alcohol, and washing times are 5-15 times.
Solution used is dissolved for nitric acid, and the amount ratio of the substance of ruthenium and acid is 1:1-1:30.
It is one kind in infusion process, coprecipitation that the ruthenium presoma and auxiliary agent, which are supported on the method on carrier,.It is described to go back
Original is handled 0.2-48 hours in 160-600 DEG C of hydrogen-containing gas, and the volume ratio of hydrogen is 2%-100% wherein in hydrogen-containing gas.
The beneficial effects of the present invention are：
Compared with existing preparation method, the present invention is first prepared with ruthenic chloride and is loaded again on the activated carbon without chlorine ruthenium presoma, is reduced
The loss of ruthenium in activated carbon supported ruthenium catalyst metal, catalyst activity and stability can also stability contorting, catalyst production
Quality is more controllable, and does not have hydrazine hydrate reduction step, simple for process, easy to operation.Chlorion, energy are washed using ethanol procedure
Rapid thorough removing chloride ion, therefore prepared catalyst activity is higher.Be one kind efficiently without the activated carbon supported ruthenium of chlorine
Base ammonia synthetic catalyst preparation method has good prospects for commercial application.
Specific implementation mode
To make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiment, the present invention is made
Further to be described in detail, exemplary embodiment of the invention and its explanation are only used for explaining the present invention, are not intended as to this
The restriction of invention.
Embodiment 1：
Take 0.1 mol/L RuCl3100 mL of aqueous solution, in whipping process be added be added dropwise 0.6 mol/L KOH it is water-soluble
50 mL of liquid, stands 1 h after mixing, gained mixture is centrifuged 3 min with the rotating speed of 3000 r/min, supernatant is outwelled, then
Absolute ethyl alcohol and stirring, centrifugation, washing is added.Repeat above-mentioned washing process 5 times, the icp analysis of cleaning solution is displayed without ruthenium metal
The presence of ion.The HNO of 20 mL is added into obtained sediment3Solution (3 mol/L), makes it completely dissolved, and then soaks
In stain to activated carbon, the ruthenium amount of metal added in terms of quality of activated carbon is 10%.By prepared sample containing 75% hydrogen
It restores 6 hours in 450 DEG C in nitrogen and hydrogen mixture atmosphere, is cooled to room temperature in above-mentioned atmosphere.Finally, the sample of gained is impregnated
Potassium nitrate aqueous solution in terms of quality of activated carbon potassium amount of metal be 12% to get to no chlorine ruthenium-based ammonia synthetic catalyst.
Embodiment 2：
Divide and takes 0.2 mol/LRuCl350 mL of aqueous solution, in whipping process be added be added dropwise 1.0 mol/L KOH it is water-soluble
30 mL of liquid, stands 10 h after mixing, gained mixture is centrifuged 3 min with the rotating speed of 3000 r/min, supernatant is outwelled,
Add absolute ethyl alcohol and stirring, centrifugation, washing.Repeat above-mentioned washing process 15 times, the icp analysis of cleaning solution is displayed without ruthenium gold
Belong to the presence of ion.The HNO of 80 mL is added into obtained sediment3Solution (1 mol/L), makes it completely dissolved, then
It is impregnated on activated carbon, the ruthenium amount of metal added in terms of quality of activated carbon is 10%.By prepared sample containing 25% hydrogen
Nitrogen and hydrogen mixture atmosphere in 500 DEG C restore 4 hours, be cooled to room temperature in above-mentioned atmosphere.Finally, the sample of gained is soaked
For stain potassium nitrate aqueous solution in terms of quality of activated carbon, potassium amount of metal is 12% to get to no chlorine ruthenium-based ammonia synthetic catalyst.
Comparative example 1：
It is raw material to take commercially available nitric acid ruthenium, and the ruthenium amount of metal added in terms of quality of activated carbon is 10%.Prepared sample is existed
It restores 6 hours in 450 DEG C in nitrogen and hydrogen mixture atmosphere containing 75% hydrogen, is cooled to room temperature in above-mentioned atmosphere.Finally, by institute
For the sample dipping potassium nitrate aqueous solution obtained in terms of quality of activated carbon, potassium amount of metal is 12% to get to before being with nitric acid ruthenium solution
Drive body without chlorine ruthenium-based ammonia synthetic catalyst.
Comparative example 2：
By suitable 0.1 mol/L RuCl3Aqueous solution is impregnated on activated carbon, the ruthenium metal added in terms of quality of activated carbon
Amount is 10%.Prepared sample is restored 6 hours in nitrogen atmosphere in 450 DEG C, is cooled to room temperature in above-mentioned atmosphere.Most
Afterwards, by the sample of gained dipping potassium nitrate aqueous solution in terms of quality of activated carbon, potassium amount of metal is 12% to get to ruthenic chloride
Solution is the ruthenium-based ammonia synthetic catalyst of presoma.
Comparative example 3：
By suitable 0.1 mol/L RuCl3Aqueous solution is impregnated on activated carbon, the ruthenium metal added in terms of quality of activated carbon
Amount is 10%.By prepared sample 1mol L-1It after potassium hydroxide solution impregnates 12 hours, washs 72 hours, drying.Most
Afterwards, by the sample of gained dipping potassium nitrate aqueous solution in terms of quality of activated carbon, potassium amount of metal is 12%, in hydrogen atmosphere in
450 DEG C restore 6 hours, obtain ruthenium-based ammonia synthetic catalyst.
The activity rating of catalyst carries out in high pressure activating test device, and reactor inside diameter is the fixed bed of 12 mm.It surveys
During examination, by 0.3 g catalyst with the quartz sand by volume 1 of grain size:20 are mixed, and be seated in reactor etc.
In warm area.Reaction gas is nitrogen, the hydrogen gaseous mixture that ammonia high-temperature catalytic cracks, H-N ratio 3:1.Table 1 is listed in reaction item
After part stablizes 10 hours, each embodiment and comparative example catalyst 9 MPa, 400 DEG C, 2.4 × 105 cm3 g-1 h-1Ammonia
Synthetic reaction rate test result.
1 ~ 3 ammonia synthesis active testing result of 1 embodiment 1 ~ 2 of table and comparative example（mmolNH3 g-1 h-1）And ruthenium loss late
As can be seen from the table, under the same conditions, the ammonia synthesis rate of catalyst of the present invention can be with nitric acid ruthenium than tradition
The catalyst activity of presoma is high by 19% or more, catalyst activity high 56% prepared by more direct than ruthenic chloride supported active high-area carbon with
On, there is preferable prospects for commercial application.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification should all belong to the covering scope of the present invention.
Claims (8)
1. a kind of preparation method of free from chloride active carbon loading ruthenium ammonia synthesis catalyst, which is characterized in that with ruthenic chloride be original
Material is added standing, precipitation, washing, dissolving after water soluble alkali solution, free from chloride ruthenium presoma is obtained, by above-mentioned no chlorine ruthenium forerunner
Body is supported on absorbent charcoal carrier, and KNO is then added in reduction3Auxiliary agent is to get to no chlorine ruthenium-based ammonia synthetic catalyst.
2. a kind of preparation method of free from chloride active carbon loading ruthenium ammonia synthesis catalyst according to claim 1, special
Sign is that water soluble alkali solution is one or more of lithium hydroxide, sodium hydroxide, potassium hydroxide aqueous solution.
3. a kind of preparation method of free from chloride active carbon loading ruthenium ammonia synthesis catalyst according to claim 1, special
Sign is that the amount ratio of the substance of ruthenic chloride and water soluble alkali is 1:3~1:6.
4. a kind of preparation method of free from chloride active carbon loading ruthenium ammonia synthesis catalyst according to claim 1, special
Sign is, time of repose 1-12h.
5. a kind of preparation method of free from chloride active carbon loading ruthenium ammonia synthesis catalyst according to claim 1, special
Sign is that washing methods is one kind in centrifugation, suction filtration, and cleaning solution is absolute ethyl alcohol, and washing times are 5-15 times.
6. a kind of preparation method of free from chloride active carbon loading ruthenium ammonia synthesis catalyst according to claim 1, special
Sign is, dissolves solution used for nitric acid, the amount ratio of the substance of ruthenium and acid is 1:1-1:10.
7. a kind of preparation method of free from chloride active carbon loading ruthenium ammonia synthesis catalyst according to claim 1, special
Sign is that ruthenium presoma and auxiliary agent are supported on the method on carrier as one kind in infusion process, coprecipitation.
8. a kind of preparation method of free from chloride active carbon loading ruthenium ammonia synthesis catalyst according to claim 1, special
Sign is that the reduction is handled 0.2-48 hours in 160-600 DEG C of hydrogen-containing gas, the volume of hydrogen wherein in hydrogen-containing gas
Than for 2%-100%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108970610A (en) * | 2018-07-23 | 2018-12-11 | 福州大学 | A kind of preparation method of active carbon loading ruthenium ammonia synthesis catalyst |
| KR20210109358A (en) * | 2020-02-27 | 2021-09-06 | 한국화학연구원 | Elimination Method of Chlorine in Inorganics Using Bases and Selective Catalytic Reduction(SCR) Catalysts Manufactured Thereby |
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| KR20210109358A (en) * | 2020-02-27 | 2021-09-06 | 한국화학연구원 | Elimination Method of Chlorine in Inorganics Using Bases and Selective Catalytic Reduction(SCR) Catalysts Manufactured Thereby |
| KR102382083B1 (en) | 2020-02-27 | 2022-04-01 | 한국화학연구원 | Elimination Method of Chlorine in Inorganics Using Bases and Selective Catalytic Reduction(SCR) Catalysts Manufactured Thereby |
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