CN105435620A - Denitration agent and preparation method thereof - Google Patents
Denitration agent and preparation method thereof Download PDFInfo
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- CN105435620A CN105435620A CN201510887303.4A CN201510887303A CN105435620A CN 105435620 A CN105435620 A CN 105435620A CN 201510887303 A CN201510887303 A CN 201510887303A CN 105435620 A CN105435620 A CN 105435620A
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- nitrate
- parts
- denitrfying agent
- chloride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/81—Solid phase processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/54—Nitrogen compounds
- B01D53/56—Nitrogen oxides
- B01D53/565—Nitrogen oxides by treating the gases with solids
Abstract
The invention provides a denitration agent and a preparation method thereof, and belongs to the technical field of catalytic cracking auxiliaries. The denitration agent is prepared from 60-85 parts of activated aluminum oxide, 1-10 parts of compound of a noble metal element, 1-5 parts of chloride of rear earth elements, 1-15 parts of nitrate of transition metal elements, 1-10 parts of nitrate of alkaline earth metal elements and 20-200 parts of water. The denitration agent can effectively decrease the concentration of NOx in flue gas, and meanwhile carbon monoxide in the flue gas is not consumed in the working process.
Description
Technical field
A kind of denitrfying agent and preparation method thereof, belongs to assistant for calalytic cracking technical field.
Background technology
Catalyst circulates between reactor and regenerator, usually when leaving reactor, containing coke about 3 ~ 10wt% on catalyst, the coke of the oxygen burning-off deposition in air must be used in regenerator to recover catalytic activity.The coke that catalyst deposits mainly reaction condensate, main component is carbon and hydrogen, when cracked stock sulfur-bearing and nitrogen, also containing sulphur and nitrogen in coke.The catalyst warp of carbon deposit and oxygen carry out regenerative response, generate CO
2, CO and H
2o, also containing SOx and NOx in regenerated flue gas.Along with the development of society, environmental issue more and more comes into one's own, and this just requires that the nitrogen oxide in regenerated flue gas (being called for short NOx) can not discharge beyond standards.In existing catalytic cracking unit, have and be much provided with CO burning stove with a large amount of carbon monoxide utilizing regenerator to generate (reaction is exothermic reaction, and fuel factor is quite large, is enough to provide the heat needed for this device thermal balance).
Existing catalytic cracking unit reduces NOx emission except by except denitrification apparatus, mainly by using denitrfying agent.Applicant is found by research, and existing denitrfying agent mainly exists following problem: first, and the NOx in regenerated flue gas can only be reduced to 200mg/Nm by existing denitrfying agent
3left and right, under more and more severeer environmental requirement, can not adapt to need of production.Secondly, existing denitrfying agent, while consumption NOx, nearly all consumes carbon monoxide, furnace operation is below floated and even can not run well very greatly.Significantly can reduce NOx concentration in regenerated flue gas in the urgent need to one (is at least reduced to 100mg/Nm at present
3), do not consume again the denitrfying agent of carbon monoxide.
Summary of the invention
The technical problem to be solved in the present invention is: overcome the deficiencies in the prior art, provides a kind of denitrfying agent and preparation method thereof, and this denitrfying agent can effectively reduce NOx concentration in flue gas, does not consume the carbon monoxide in flue gas in the course of work simultaneously.
The technical solution adopted for the present invention to solve the technical problems is: this denitrfying agent, it is characterized in that, be made up of the raw material of following weight portion: the compound 1 ~ 10 part of activated alumina 60 ~ 85 parts, precious metal element, the chloride 1 ~ 5 part of rare earth element, 1 ~ 15 part, the nitrate of transition metal, 1 ~ 10 part, the nitrate of alkali earth metal, 20 ~ 200 parts, water.
This denitrfying agent, it is characterized in that, be made up of the raw material of following weight portion: the compound 1 ~ 5 part of activated alumina 60 ~ 75 parts, precious metal element, the chloride 3 ~ 5 parts of rare earth element, 10 ~ 15 parts, the nitrate of transition metal, 3 ~ 5 parts, the nitrate of alkali earth metal, 30 ~ 50 parts, water.
This denitrfying agent, is characterized in that: the specific area 100 ~ 260m of described activated alumina
2/ g, in carrier, the mass percent shared by particle of particle diameter 40 ~ 105 μm is more than or equal to 60%, pore volume 0.15 ~ 0.3ml/g, bulk density 0.85g/ml.
The compound of described precious metal element is after the simple substance use aqua regia dissolution of precious metal element, the product that drying obtains.
The simple substance of described precious metal element is gold or platinum.
The chloride of described rare earth element is the chlorate of one or more in lanthanum, cerium, praseodymium, neodymium.
The nitrate of iron, cobalt, nickel, copper or zinc selected by the nitrate transition metal of described transition metal.
The nitrate of described alkali earth metal is the nitrate of magnesium, strontium, barium.
The preparation method of this denitrfying agent, is characterized in that, adopts following steps:
A) by the nitrate of the chloride of the compound of precious metal element, rare earth element, transition metal, the nitrate of alkali earth metal and water by weight ratio be mixed with solution, stir;
B) be placed in agitator tank by the activated alumina taken by weight, solution step a) prepared adds agitator tank, obtains semi-finished product after stirring;
C) semi-finished product be positioned in drying oven dry, dry 1 ~ 5 hour for 100 ~ 300 DEG C, 700 ~ 750 DEG C of roastings after 1 ~ 2 hour finished product.
Applicant finds under study for action: carbon monoxide is the gas of a kind of incendivity recycling, and all consumes carbon monoxide in the existing denitrfying agent course of work, and carbon monoxide cannot carry out secondary utilization as the flammable energy.And in large-scale industrial production, the year growing amount of carbon monoxide is huge, the use of existing denitrfying agent result in a large amount of energy wastes.Applicant is by studying discovery further, and the reason causing existing denitrfying agent to consume carbon monoxide is in the course of the work: the precious metal in denitrfying agent exists the effect of absorption, activation to nitric oxide.
Applicant research in determine that the mechanism of action of denitrfying agent of the present invention is as follows: through step a) ~ c) operation after, in this denitrfying agent obtained: precious metal element, rare earth element, transition metal and alkaline-earth metal exist with the form of metal oxide respectively, the design that various metals component in conjunction uses, makes the denitration rate of this denitrfying agent higher.In this denitrfying agent course of work, utilize how intermetallic interaction, optionally the NOx in regenerated flue gas is carried out adsorbing and decomposing, simultaneously according to the specific metal ratio in raw material of the present invention, by the shielding of the selective action of precious metal sorbing carbon monoxide.
Combustion-supporting reaction mechanism: (Pr represents precious metal)
Adsorption activation: Pr+O
2→ Pr-O
Be oxidized combustion-supporting: Pr-O+CO(or C) → Pr+CO
2↑
Denitration reaction mechanism: (Me and Pe represents different metals respectively)
Me+NH
3→Me:NH
2-H
Pe+NO→Pe:N=O
Me:NH
2-H+Pe:N=O→N
2↑+H
2O+Me+Pe
When the ratio of various metals reaches the parts by weight of raw materials ratio of the present invention's restriction, this denitrfying agent obtained is in the process of smoke treatment: precious metal Pr can mask the adsorptivity of CO by metal M e and Pe.
Activated alumina, has another name called activated bauxite, in white powder.In this area, the aluminium oxide used in the catalyst, is specially called activated alumina usually, and it is the solid material of a kind of porous, high degree of dispersion.In the present invention, activated alumina uses as carrier.Preferably, activated alumina is that Shandong Aluminium Industrial Corp produces; Preferably, activated alumina specific area 100 ~ 260m
2/ g, particle diameter 40 ~ 105 μm>=60%, pore volume 0.15 ~ 0.3ml/g, bulk density 0.85g/ml, the performance parameter of above activated alumina can ensure that activated alumina has larger surface area, its micropore surface possesses better absorption property, surface-active and excellent heat endurance, can component effectively in the solution that a) obtains of adsorption step, improves the denitration rate of this denitrfying agent.
The chloride of the rare earth element described in the present invention is the chloride of the rare earth element comprising the crystallization water.Such as, in the present invention, the lanthanum chloride of indication is LaCl
36H
2o(pale yellow crystals shape), cerium chloride is CeCl
36H
2o(white crystalline), praseodymium chloride is PrCl
36H
2the green granular crystal thing of O(), neodymium chloride is NdCl
36H
2o(purple crystals), the chloride comprising the rare earth element of the crystallization water is commercially available prod, is easier to buy obtain, and is directly dissolved in distilled water during the operation of step a).Preferably, the water in this denitrfying agent raw material is distilled water, does not contain or containing few metal cation component, can avoid producing interference to the roasting of step c) of the present invention in distilled water.
After in the present invention, the simple substance of precious metal element uses aqua regia dissolution, chloroazotic acid is consumed by reaction in the simple substance process of dissolving precious metal element, form the complex compound of precious metal element and the mixed liquor of water, the product obtained after drying is the compound of precious metal element.The compound of precious metal element in step a) with solid-state interpolation.May contain the chloroazotic acid of denier in the compound of precious metal element or not participate in the impurity of reaction, but shared mass percent is lower than one thousandth, negligible.
Compared with prior art, the beneficial effect that a kind of denitrfying agent of the present invention and preparation method thereof has is: this denitrfying agent can effectively reduce NOx concentration in flue gas, does not consume the carbon monoxide in flue gas in the course of work simultaneously.First, applicant devises precious metal element, rare earth element, transition metal and alkali earth metal conbined usage, by the metallic element coupling of many races, to realize selective absorption NOx fast and accurately, key effect is served in the decomposition reaction of NOx, make denitration rate higher, the concentration of emission of NOx reaches 100mg/Nm
3and below.Secondly, applicant finds to cause the reason of carbon monoxide consumption to be the adsorption activation of precious metal to carbon monoxide under study for action.Eliminating precious metal to the adsorption activation of carbon monoxide by studying the nitrate finally determining interpolation 1 ~ 10 part of alkali metal, not consuming carbon monoxide, for the even running of follow up device lays the foundation.Further, be can be used as the incendivity energy by the carbon monoxide that denitrfying agent of the present invention retains, there is the effect of energy-saving and emission-reduction.
Detailed description of the invention
Embodiment 1 ~ 5 is detailed description of the invention of a kind of denitrfying agent of the present invention and preparation method thereof, and wherein embodiment 1 is most preferred embodiment.The nitrate of the various metals added in embodiment 1 ~ 5 Raw be commercially available, with the nitrate of the metal of the crystallization water.The activated alumina that the activated alumina that embodiment 1 ~ 5 uses is produced for Shandong Aluminium Industrial Corp, specific area 100 ~ 260m
2/ g, particle diameter 40 ~ 105 μm>=60%, pore volume 0.15 ~ 0.3ml/g, bulk density 0.85g/ml.After chloroplatinic acid used in embodiment 1 ~ 5 adopts and platinum simple substance is used aqua regia dissolution, drying obtains, the compound of gold used be the simple substance of gold through aqua regia dissolution, dryly to obtain.
Embodiment 1
In the present embodiment, component proportion by weight, activated alumina 75 parts, chloroplatinic acid 5 parts, neodymium chloride 5 parts, copper nitrate 12 parts, magnesium nitrate 3 parts, distilled water 30 parts;
The preparation method of the present embodiment is as follows:
A) by chloroplatinic acid, neodymium chloride, copper nitrate, magnesium nitrate, distilled water by weight ratio be mixed with solution, stir;
B) be placed in agitator tank by activated alumina, solution step a) prepared adds agitator tank, obtains semi-finished product after stirring;
C) semi-finished product be positioned in drying oven dry, dry 5 hours for 120 DEG C, 750 DEG C of roastings after 1 hour finished product.
Embodiment 2
In the present embodiment, component proportion by weight, activated alumina 60 parts, chloroplatinic acid 10 parts, cerium chloride 5 parts, copper nitrate 15 parts, barium nitrate 10 parts, distilled water 30 parts;
The preparation method of the present embodiment is as follows:
A) by chloroplatinic acid, cerium chloride, copper nitrate, barium nitrate, distilled water by weight ratio be mixed with solution, stir;
B) be placed in agitator tank by activated alumina, solution step a) prepared adds agitator tank, obtains semi-finished product after stirring;
C) semi-finished product be positioned in drying oven dry, dry 5 hours for 100 DEG C, 750 DEG C of roastings after 1 hour finished product.
Embodiment 3
In the present embodiment, component proportion by weight, compound 5 parts, lanthanum chloride 5 parts, cobalt nitrate 15 parts, magnesium nitrate 5 parts, the distilled water 30 parts of activated alumina 70 parts, gold;
The preparation method of the present embodiment is as follows:
A) by the compound of gold, lanthanum chloride, cobalt nitrate, magnesium nitrate, distilled water by weight ratio be mixed with solution, stir;
B) be placed in agitator tank by activated alumina, solution step a) prepared adds agitator tank, obtains semi-finished product after stirring;
C) semi-finished product be positioned in drying oven dry, dry 5 hours for 150 DEG C, 750 DEG C of roastings after 1 hour finished product.
Embodiment 4
In the present embodiment, component proportion by weight, compound 2 parts, praseodymium chloride 3 parts, copper nitrate 7 parts, strontium nitrate 3 parts, the distilled water 30 parts of activated alumina 85 parts, gold;
The preparation method of the present embodiment is as follows:
A) by the compound of gold, praseodymium chloride, copper nitrate, strontium nitrate, distilled water by weight ratio be mixed with solution, stir;
B) be placed in agitator tank by activated alumina, solution step a) prepared adds agitator tank, obtains semi-finished product after stirring;
C) semi-finished product be positioned in drying oven dry, dry 5 hours for 300 DEG C, 750 DEG C of roastings after 1 hour finished product.
Embodiment 5
In the present embodiment, component proportion by weight, activated alumina 80 parts, chloroplatinic acid 1 part, lanthanum chloride 5 parts, copper nitrate 10 parts, magnesium nitrate 4 parts, distilled water 30 parts; The preparation method of the present embodiment is as follows:
A) by chloroplatinic acid, lanthanum chloride, copper nitrate, magnesium nitrate, distilled water by weight ratio be mixed with solution, stir;
B) be placed in agitator tank by activated alumina, solution step a) prepared adds agitator tank, obtains semi-finished product after stirring;
C) semi-finished product be positioned in drying oven dry, dry 5 hours for 120 DEG C, 750 DEG C of roastings after 1 hour finished product.
Performance test is tested
From the denitrfying agent prepared by embodiment 1 ~ 5, sample 100g respectively, be numbered and detect its performance.Denitration performance and combustion-supporting Performance Detection (namely detecting the Expenditure Levels of carbon monoxide): be the ratio of 98 ~ 100:2 according to the weight ratio of major catalyst and denitrfying agent, to respectively the denitrfying agent that embodiment 1 ~ 5 obtains be joined in the major catalyst of catalytic cracking unit, be then placed in Catalytic Cracking Evaluation device respectively and detect.The operating parameter of simulation catalytic cracking unit is: regenerator temperature 720 ~ 740 DEG C, and simulation regenerated flue gas includes CO, NOx, SOx, N
2and NH
3, test result is in table 1.
Table 1 embodiment 1 ~ 5 the performance test results
。
Can be found out by embodiment 1 ~ 5, denitrfying agent denitration performance of the present invention is excellent, and can reach more than 80% for NOx removal efficiency, the highest NOx removal efficiency can reach 87%.And can be found out by table 1, embodiment 1 ~ 5 is extremely low for CO removal efficiency, prove that denitrfying agent of the present invention consumes carbon monoxide hardly while process NOx, the carbon monoxide be retained is collected in subsequent technique, purifying, recycling, can obtain outstanding economic benefit.
The above is only preferred embodiment of the present invention, and be not restriction the present invention being made to other form, any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the Equivalent embodiments of equivalent variations.But everyly do not depart from technical solution of the present invention content, any simple modification, equivalent variations and the remodeling done above embodiment according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (9)
1. a denitrfying agent, it is characterized in that, be made up of the raw material of following weight portion: the compound 1 ~ 10 part of activated alumina 60 ~ 85 parts, precious metal element, the chloride 1 ~ 5 part of rare earth element, 1 ~ 15 part, the nitrate of transition metal, 1 ~ 10 part, the nitrate of alkali earth metal, 20 ~ 200 parts, water.
2. a kind of denitrfying agent according to claim 1, it is characterized in that, be made up of the raw material of following weight portion: the compound 1 ~ 5 part of activated alumina 60 ~ 75 parts, precious metal element, the chloride 3 ~ 5 parts of rare earth element, 10 ~ 15 parts, the nitrate of transition metal, 3 ~ 5 parts, the nitrate of alkali earth metal, 30 ~ 50 parts, water.
3. a kind of denitrfying agent according to claim 1, is characterized in that: the specific area 100 ~ 260m of described activated alumina
2/ g, in carrier, the mass percent shared by particle of particle diameter 40 ~ 105 μm is more than or equal to 60%, pore volume 0.15 ~ 0.3ml/g, bulk density 0.85g/ml.
4. a kind of denitrfying agent according to claim 1, is characterized in that: the compound of described precious metal element is after the simple substance use aqua regia dissolution of precious metal element, the product that drying obtains.
5. a kind of denitrfying agent according to claim 4, is characterized in that: the simple substance of described precious metal element is gold or platinum.
6. a kind of denitrfying agent according to claim 1, is characterized in that: the chloride of described rare earth element is the chlorate of one or more in lanthanum, cerium, praseodymium, neodymium.
7. a kind of denitrfying agent according to claim 1, is characterized in that: the nitrate of iron, cobalt, nickel, copper or zinc selected by the nitrate transition metal of described transition metal.
8. a kind of denitrfying agent according to claim 1, is characterized in that: the nitrate of described alkali earth metal is the nitrate of magnesium, strontium, barium.
9. the preparation method of a kind of denitrfying agent described in any one of claim 1 ~ 8, is characterized in that, adopts following steps:
A) by the nitrate of the chloride of the compound of precious metal element, rare earth element, transition metal, the nitrate of alkali earth metal and water by weight ratio be mixed with solution, stir;
B) be placed in agitator tank by the activated alumina taken by weight, solution step a) prepared adds agitator tank, obtains semi-finished product after stirring;
C) semi-finished product be positioned in drying oven dry, dry 1 ~ 5 hour for 100 ~ 300 DEG C, 700 ~ 750 DEG C of roastings after 1 ~ 2 hour finished product.
Priority Applications (1)
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|---|---|---|---|
| CN201510887303.4A CN105435620A (en) | 2015-12-07 | 2015-12-07 | Denitration agent and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510887303.4A CN105435620A (en) | 2015-12-07 | 2015-12-07 | Denitration agent and preparation method thereof |
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Family
ID=55546517
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106731643A (en) * | 2016-12-21 | 2017-05-31 | 李国栋 | A kind of denitrfying agent and preparation method thereof |
| CN112354358A (en) * | 2020-09-17 | 2021-02-12 | 山东骏飞环保科技有限公司 | Catalytic cracking oxygen-poor regeneration denitration agent and preparation method thereof |
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Application publication date: 20160330 |