CN102962061A - Multifunctional catalyst for removing NOX and SOX in catalytic cracking regeneration flue gas and preparation method of multifunctional catalyst - Google Patents
Multifunctional catalyst for removing NOX and SOX in catalytic cracking regeneration flue gas and preparation method of multifunctional catalyst Download PDFInfo
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Abstract
The invention relates to a multifunctional catalyst for removing NOX and SOX in catalytic cracking regeneration flue gas and a preparation method of the multifunctional catalyst. The multifunctional catalyst is prepared by respectively carrying out steeping, drying, baking and roasting on carrier microspheric alumina by rare-earth-type desulfuration steeping liquor A, rare-earth-type denitration steeping liquor B and noble metal salt steeping liquor C. The multifunctional catalyst has the effects of removing the NOX and the SOX in the FCC (Fluid Catalytic Cracking) regeneration flue gas and supporting combustion of CO (carbon monoxide), and the adding amount of the multifunctional catalyst in equipment is 0.5%; the removing rate of the NOX in the regeneration flue gas can reach 70% or more, and the removing rate of the SOX in the regeneration flue gas can reach 40% or more; and the multifunctional catalyst has the good effect of supporting the combustion of the CO, and can increase the yield of propylene for 2.0% or more. Compared with the conventional process device for desulfurization and denitration of the regeneration flue gas, the multifunctional catalyst has the advantages of not needing fixed investment and being low in use cost; compared with the similar desulfurization and denitrification catalyst, the multifunctional catalyst has higher NOX and SOX removing rates; and the adding amount of the multifunctional catalyst is 10%-20% of that of the conventional desulfurization and denitrification catalyst, so that the normal production and operation of the equipment cannot be influenced. Thus, the multifunctional catalyst for removing the NOX and the SOX in the catalytic cracking regeneration flue gas has remarkable economic and social benefits.
Description
Technical field:
The invention belongs to catalysis technical field, be specifically related to a kind of multifunction catalyst that removes regeneration fume from catalytic cracking NOx, SOx and preparation method thereof, particularly relate to and a kind ofly can remove simultaneously NOx in the regeneration fume from catalytic cracking, SOx, and have multifunction catalyst of CO combustion aid function and preparation method thereof.
Background technology:
Along with China's rapid development of economy, more and more higher to the demand of the energy, and the shortage of oil is further serious; The feedstock oil ubiquity of present domestic refinery is heaviness, in poor quality gradually; And one of main method of refinery's production gasoline is FCC (fluid catalytic cracking), and its main device comprises reactor and regenerator; Feedstock oil is delivered into the riser of reactor, by be cracked into distillate after the FCC catalyst mix contacts; Simultaneously, catalyst is because green coke loses activity; Catalyst behind the inactivation enters the regenerator coke burning regeneration through behind the stripping, the nitrogen-containing compound that contains in the coke and sulfide meeting nitrogen oxide oxide, oxysulfide and the incomplete CO of partial combustion; According to statistics, the discharging of SOx and NOx respectively in the duty gas 6%～7% and 10% of total discharging in the FCC catalyst regeneration process.This type of emission is one of main atmosphere pollution, and they mainly cause greenhouse effects, causes the pollutant of atmosphere acidifying, formation acid rain, and NOx still causes the principal element of photochemical fog; In order to reduce NOx, SOx discharge capacity, most countries has all been formulated the discharge standard of NOx, SOx, forbids that strictly the discharging of nitrogen oxide, oxysulfide exceeds the permission standard level.Owing to physicochemical environment special in the FCC regenerator (high temperature, multiple gases and a plurality of reaction coexistence), up to the present, can when addition is 0.5%, effectively remove simultaneously these several pollutants without any a kind of catalyst, and have the combustion-supporting effect of CO.
Summary of the invention:
Purpose of the present invention is exactly for above-mentioned the deficiencies in the prior art, and a kind of multifunction catalyst that removes regeneration fume from catalytic cracking NOx, SOx is provided.
Another object of the present invention provides a kind of multifunction catalyst that removes regeneration fume from catalytic cracking NOx, SOx and preparation method thereof.
The objective of the invention is to be achieved through the following technical solutions:
A kind of main component that removes the multifunction catalyst of regeneration fume from catalytic cracking NOx, SOx is:
The carrier microballoons aluminium oxide
Rare-earth type desulfurization maceration extract A
Rare-earth type denitration maceration extract B
Precious metal salt maceration extract C
By the carrier microballoons aluminium oxide through rare-earth type desulfurization maceration extract A, rare-earth type denitration maceration extract B, precious metal salt maceration extract C flood respectively, dry oven dry, roasting make.
A kind of preparation method who removes the multifunction catalyst of regeneration fume from catalytic cracking NOx, SOx is comprised of following steps substantially:
The preparation of a, rare-earth type desulfurization maceration extract A:
After 100 kilograms of rare-earth salts and 10～15 kilograms of mixing of citric acid, add the dissolving of 500～520L deionized water and stirring and be configured to rare-earth type desulfurization maceration extract A
The preparation of b, rare-earth type denitration maceration extract B:
After 100 kilograms of rare-earth salts, 10～12 kilograms of cupric oxalates and 15～25 kilograms of mixing of citric acid, add the dissolving of 500～520L deionized water and stirring and be configured to rare-earth type denitration maceration extract B
C, take off the preparation of NOx, SOx catalyst:
500 kilograms of carrier microballoons aluminium oxide are put into cone blender, spray maceration extract A, carry out the about 5～10min of the saturated dipping in hole, emit the solid material behind the dipping, and after placing 2～3 hours, move in mesh-belt kiln or other the dynamic drying equipment in 120～130 ℃ of oven dry 2～2.5 hours, then 280～300 ℃ of pyrolysis 1 hour change in roller kilns or the tunnel cave 600 ℃ of roastings 2～2.5 hours; Spray again maceration extract B after the cooling, carry out the about 5～10min of the saturated dipping in hole, emit the solid material behind the dipping, and after placing 2～3 hours, move in mesh-belt kiln or other the dynamic drying equipment in 120～130 ℃ of oven dry 2～2.5 hours, then 280～300 ℃ of pyrolysis 1～1.5 hour change in roller kilns or the tunnel cave 600 ℃ of roastings 2～2.5 hours; Must become a pint NOx, SOx catalyst finished product after the cooling.
D, precious metal salt maceration extract C
After 0.2～0.25 kilogram of precious metal salt and 2～2.5 kilograms of mixing of cupric oxalate, add the dissolving of 100-102L deionized water and stirring and be configured to precious metal salt maceration extract C
The preparation of e, the combustion-supporting effect of increase CO:
500 kilograms of the products of step c are put into cone blender, spray maceration extract C, carry out the about 5～10min of the saturated dipping in hole, emit the solid material behind the dipping, in 120～130 ℃ of oven dry 2～2.5 hours, then change in roller kilns or the tunnel cave 600 ℃ of roastings 2～3 hours in immigration mesh-belt kiln or other the dynamic drying equipment; After the cooling finished product have a combustion-supporting effect of CO take off NOx, SOx catalyst finished product.
Purpose of the present invention can also be achieved through the following technical solutions:
Rare-earth type desulfurization maceration extract A uses rare-earth salts to adopt vanadic acid rare earth La VO
4
Rare-earth type denitration maceration extract B uses rare-earth salts to adopt antimony acetate
Precious metal salt maceration extract C uses precious metal salt to be platinum nitrate
The carrier microballoons aluminium oxide
Citric acid
Cupric oxalate
Beneficial effect: when low addition, can effectively remove NOx, SOx in the FCC regenerated flue gas, and have the combustion-supporting effect of good CO.Can effectively reduce pollutant emission, reach GB and require discharge standard, use flue gas desulfurization and denitrification equipment and FCC feedstock oil hydrogenation technique by contrast, the present invention adopts multiple-effect Catalysts for Reducing flue gas NOx, SOx discharging, and main innovate point is as follows:
1, need not hydrogen source: if carry out FCC feedstock oil hydroprocessing technique, the hydrogen source guarantee of reliable abundance must be arranged, the oil refining industry of China also has most of enterprise to belong to medium-sized and small enterprises, its secondary operations does not match, and does not possess the hydrogenation ability, simultaneously, the hydrogenation technique cost is high, and the process unit investment is large.
If 2 use the regeneration flue gas desulfurization denitration device, also can reach the effect of desulphurization and denitration, but its investment, maintenance cost height, catalytic unit for 1,000,000 ton/years, the equipment investment of regeneration flue gas desulfurization denitration is about 5,000 ten thousand yuan, year maintenance cost is about 2,000 ten thousand yuan, and it does not possess the combustion-supporting effect of CO; The refinery still needs to add separately the CO combustion adjuvant when producing, and has further improved refinery's production cost.And the device of same scale uses multi-functional NOx, the SOx catalyst of taking off, and a year Meteorological only is 500～8,000,000 yuan.Using multi-functional NOx, SOx catalyst for reaching pollutant emission standard, is one of most economical approach of oil plant lifting energy-saving and emission-reducing.
3, this catalyst has the characteristics of low, the good desulfurization off sulfide effect of addition and the combustion-supporting effect of CO, the out of stock catalyst of the desulfurization of present domestic commercialization, addition is substantially 3～5%, and addition is crossed the normal operating that senior general affects device, is unfavorable for the device steady production.
The specific embodiment:
Below just embodiment be described in further detail:
A kind of main component that removes the multifunction catalyst of regeneration fume from catalytic cracking NOx, SOx is:
The carrier microballoons aluminium oxide
Citric acid
Cupric oxalate
Precious metal salt
Rare-earth type desulfurization maceration extract A
Rare-earth type denitration maceration extract B
Precious metal salt maceration extract C
A kind of preparation method who removes the multifunction catalyst of regeneration fume from catalytic cracking NOx, SOx is comprised of following steps substantially:
The preparation of a, rare-earth type desulfurization maceration extract A:
After 100 kilograms of rare-earth salts and 10～15 kilograms of mixing of citric acid, add the dissolving of 500～520L deionized water and stirring and be configured to rare-earth type desulfurization maceration extract A
The preparation of b, rare-earth type denitration maceration extract B:
After 100 kilograms of rare-earth salts, 10～12 kilograms of cupric oxalates and 15～25 kilograms of mixing of citric acid, add the dissolving of 500～520L deionized water and stirring and be configured to rare-earth type denitration maceration extract B
C, take off the preparation of NOx, SOx catalyst:
500 kilograms of carrier microballoons aluminium oxide are put into cone blender, spray maceration extract A, carry out the about 5～10min of the saturated dipping in hole, emit the solid material behind the dipping, and after placing 2～3 hours, move in mesh-belt kiln or other the dynamic drying equipment in 120～130 ℃ of oven dry 2～2.5 hours, then 280～300 ℃ of pyrolysis 1 hour change in roller kilns or the tunnel cave 600 ℃ of roastings 2～2.5 hours; Spray again maceration extract B after the cooling, carry out the about 5～10min of the saturated dipping in hole, emit the solid material behind the dipping, and after placing 2～3 hours, move in mesh-belt kiln or other the dynamic drying equipment in 120～130 ℃ of oven dry 2～2.5 hours, then 280～300 ℃ of pyrolysis 1～1.5 hour change in roller kilns or the tunnel cave 600 ℃ of roastings 2～2.5 hours; Must become a pint NOx, SOx catalyst finished product after the cooling.
D, precious metal salt maceration extract C
After 0.2～0.25 kilogram of precious metal salt and 2～2.5 kilograms of mixing of cupric oxalate, add the dissolving of 100-102L deionized water and stirring and be configured to precious metal salt maceration extract C
The preparation of e, the combustion-supporting effect of increase CO:
500 kilograms of the products of step c are put into cone blender, spray maceration extract C, carry out the about 5～10min of the saturated dipping in hole, emit the solid material behind the dipping, in 120～130 ℃ of oven dry 2～2.5 hours, then change in roller kilns or the tunnel cave 600 ℃ of roastings 2～3 hours in immigration mesh-belt kiln or other the dynamic drying equipment; After the cooling finished product have a combustion-supporting effect of CO take off NOx, SOx catalyst finished product.
F, quantitative package are positioned over dry shady and cool place.
Embodiment 1:
The preparation of a, rare-earth type desulfurization maceration extract A:
After 100 kilograms of rare-earth salts and 12 kilograms of mixing of citric acid, add the dissolving of 500L deionized water and stirring and be configured to rare-earth type desulfurization maceration extract A
The preparation of b, rare-earth type denitration maceration extract B:
After 100 kilograms of rare-earth salts, 10 kilograms of cupric oxalates and 20 kilograms of mixing of citric acid, add the dissolving of 500L deionized water and stirring and be configured to rare-earth type denitration maceration extract B
C, take off the preparation of NOx, SOx catalyst:
500 kilograms of carrier microballoons aluminium oxide are put into cone blender, spray maceration extract A, carry out the about 8min of the saturated dipping in hole, emit the solid material behind the dipping, and after placing 2 hours, move in mesh-belt kiln or other the dynamic drying equipment in 120 ℃ of oven dry 2 hours, then 285 ℃ of pyrolysis 1 hour change in roller kilns or the tunnel cave 600 ℃ of roastings 2 hours; Spray again maceration extract B after the cooling, carry out the about 8min of the saturated dipping in hole, emit the solid material behind the dipping, and after placing 2 hours, move in mesh-belt kiln or other the dynamic drying equipment in 120 ℃ of oven dry 2 hours, then 285 ℃ of pyrolysis 1 hour change in roller kilns or the tunnel cave 600 ℃ of roastings 2 hours; Must become a pint NOx, SOx catalyst finished product after the cooling.
D, precious metal salt maceration extract C
After 0.2 kilogram of precious metal salt and 2 kilograms of mixing of cupric oxalate, add the dissolving of 100L deionized water and stirring and be configured to precious metal salt maceration extract C
The preparation of e, the combustion-supporting effect of increase CO:
500 kilograms of the products of step c are put into cone blender, spray maceration extract C carries out the about 8min of the saturated dipping in hole, emits the solid material behind the dipping, in 120 ℃ of oven dry 2 hours, then change in roller kilns or the tunnel cave 600 ℃ of roastings 2 hours in immigration mesh-belt kiln or other the dynamic drying equipment; After the cooling finished product have a combustion-supporting effect of CO take off NOx, SOx catalyst finished product.
F, quantitative package are positioned over dry shady and cool place.
Embodiment 2:
The preparation of a, rare-earth type desulfurization maceration extract A:
After 100 kilograms of rare-earth salts and 15 kilograms of mixing of citric acid, add the dissolving of 510L deionized water and stirring and be configured to rare-earth type desulfurization maceration extract A
The preparation of b, rare-earth type denitration maceration extract B:
After 100 kilograms of rare-earth salts, 12 kilograms of cupric oxalates and 25 kilograms of mixing of citric acid, add the dissolving of 510L deionized water and stirring and be configured to rare-earth type denitration maceration extract B
C, take off the preparation of NOx, SOx catalyst:
500 kilograms of carrier microballoons aluminium oxide are put into cone blender, spray maceration extract A, carry out the about 10min of the saturated dipping in hole, emit the solid material behind the dipping, and after placing 2.5 hours, move in mesh-belt kiln or other the dynamic drying equipment in 130 ℃ of oven dry 2.5 hours, then 300 ℃ of pyrolysis 1 hour change in roller kilns or the tunnel cave 600 ℃ of roastings 2.5 hours; Spray again maceration extract B after the cooling, carry out the about 10min of the saturated dipping in hole, emit the solid material behind the dipping, and after placing 3 hours, move in mesh-belt kiln or other the dynamic drying equipment in 130 ℃ of oven dry 2.5 hours, then 300 ℃ of pyrolysis 1.5 hours change in roller kilns or the tunnel cave 600 ℃ of roastings 2.5 hours; Must become a pint NOx, SOx catalyst finished product after the cooling.
D, precious metal salt maceration extract C
After 0.25 kilogram of precious metal salt and 2.5 kilograms of mixing of cupric oxalate, add the dissolving of 102L deionized water and stirring and be configured to precious metal salt maceration extract C
The preparation of e, the combustion-supporting effect of increase CO:
500 kilograms of the products of step c are put into cone blender, spray maceration extract C, carry out the about 10min of the saturated dipping in hole, emit the solid material behind the dipping, in 130 ℃ of oven dry 2.5 hours, then change in roller kilns or the tunnel cave 600 ℃ of roastings 3 hours in immigration mesh-belt kiln or other the dynamic drying equipment; After the cooling finished product have a combustion-supporting effect of CO take off NOx, SOx catalyst finished product.
F, quantitative package are positioned over dry shady and cool place.
Claims (9)
1. multifunction catalyst that removes regeneration fume from catalytic cracking NOx, SOx is characterized in that: the carrier microballoons aluminium oxide through rare-earth type desulfurization maceration extract A, rare-earth type denitration maceration extract B, precious metal salt maceration extract C flood respectively, dry oven dry, roasting make.
2. the multifunction catalyst that removes regeneration fume from catalytic cracking NOx, SOx according to claim 1 is characterized in that: carrier employing alumina microsphere.
3. the multifunction catalyst that removes regeneration fume from catalytic cracking NOx, SOx according to claim 1, it is characterized in that: after 100 kilograms of rare-earth salts and 10～15 kilograms of mixing of citric acid, add the dissolving of 500～520L deionized water and stirring and be configured to rare-earth type desulfurization maceration extract A.
4. the multifunction catalyst that removes regeneration fume from catalytic cracking NOx, SOx according to claim 1, it is characterized in that: after 100 kilograms of rare-earth salts, 10～12 kilograms of cupric oxalates and 15～25 kilograms of mixing of citric acid, add the dissolving of 500～520L deionized water and stirring and be configured to rare-earth type denitration maceration extract B.
5. the multifunction catalyst that removes regeneration fume from catalytic cracking NOx, SOx according to claim 1, it is characterized in that: after 0.2～0.25 kilogram of precious metal salt and 2～2.5 kilograms of mixing of cupric oxalate, add the dissolving of 100-102L deionized water and stirring and be configured to precious metal salt maceration extract C.
6. rare-earth type desulfurization maceration extract A according to claim 3 is characterized in that: rare-earth type desulfurization maceration extract A use rare-earth salts employing vanadic acid rare earth La VO
4
7. rare-earth type denitration maceration extract B according to claim 4 is characterized in that: rare-earth type denitration maceration extract B use rare-earth salts employing antimony acetate.
8. precious metal salt maceration extract C according to claim 5, it is characterized in that: precious metal salt maceration extract C uses precious metal salt to be platinum nitrate.
9. the multifunction catalyst that removes regeneration fume from catalytic cracking NOx, SOx according to claim 1 is characterized in that, comprises following order and step:
The preparation of a, rare-earth type desulfurization maceration extract A:
After 100 kilograms of rare-earth salts and 10～15 kilograms of mixing of citric acid, add the dissolving of 500～520L deionized water and stirring and be configured to rare-earth type desulfurization maceration extract A
The preparation of b, rare-earth type denitration maceration extract B:
After 100 kilograms of rare-earth salts, 10～12 kilograms of cupric oxalates and 15～25 kilograms of mixing of citric acid, add the dissolving of 500～520L deionized water and stirring and be configured to rare-earth type denitration maceration extract B
C, take off the preparation of NOx, SOx catalyst:
500 kilograms of carrier microballoons aluminium oxide are put into cone blender, spray maceration extract A, carry out the about 5～10min of the saturated dipping in hole, emit the solid material behind the dipping, and after placing 2～3 hours, move in mesh-belt kiln or other the dynamic drying equipment in 120～130 ℃ of oven dry 2～2.5 hours, then 280～300 ℃ of pyrolysis 1 hour change in roller kilns or the tunnel cave 600 ℃ of roastings 2～2.5 hours; Spray again maceration extract B after the cooling, carry out the about 5～10min of the saturated dipping in hole, emit the solid material behind the dipping, and after placing 2～3 hours, move in mesh-belt kiln or other the dynamic drying equipment in 120～130 ℃ of oven dry 2～2.5 hours, then 280～300 ℃ of pyrolysis 1～1.5 hour change in roller kilns or the tunnel cave 600 ℃ of roastings 2～2.5 hours; Must become a pint NOx, SOx catalyst finished product after the cooling.
D, precious metal salt maceration extract C
After 0.2～0.25 kilogram of precious metal salt and 2～2.5 kilograms of mixing of cupric oxalate, add the dissolving of 100-102L deionized water and stirring and be configured to precious metal salt maceration extract C
The preparation of e, the combustion-supporting effect of increase CO:
500 kilograms of the products of step c are put into cone blender, spray maceration extract C, carry out the about 5～10min of the saturated dipping in hole, emit the solid material behind the dipping, in 120～130 ℃ of oven dry 2～2.5 hours, then change in roller kilns or the tunnel cave 600 ℃ of roastings 2～3 hours in immigration mesh-belt kiln or other the dynamic drying equipment; After the cooling finished product have a combustion-supporting effect of CO take off NOx, SOx catalyst finished product.
F, quantitative package are positioned over dry shady and cool place.
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| CN105727983A (en) * | 2014-12-11 | 2016-07-06 | 中国石油天然气股份有限公司 | Cocatalyst for fluid catalytic cracking and preparation method thereof |
| CN106975477A (en) * | 2017-05-04 | 2017-07-25 | 龙岩紫荆创新研究院 | SCR denitration preparation method and catalyst |
| CN115770585A (en) * | 2021-09-09 | 2023-03-10 | 中国石油化工股份有限公司 | For reducing NO in flue gas X And SO X Discharged catalyst, preparation method thereof and flue gas SO removal X And NO X Method (2) |
| WO2024017252A1 (en) * | 2022-07-19 | 2024-01-25 | Basf Corporation | Catalytic article comprising vanadium-containing catalyst and oxidation catalyst |
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| CN1890021A (en) * | 2003-12-05 | 2007-01-03 | 英特凯特公司 | Mixed metal oxide sorbents |
| CN1631531A (en) * | 2003-12-24 | 2005-06-29 | 中国科学院生态环境研究中心 | Purifying catalyst for nitrogen oxides in sulfur containing oxygen enriching tail gas |
| CN1958732A (en) * | 2006-02-16 | 2007-05-09 | 刘希尧 | Quadruple effect auxiliary agent in use for FCC technique |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105727983A (en) * | 2014-12-11 | 2016-07-06 | 中国石油天然气股份有限公司 | Cocatalyst for fluid catalytic cracking and preparation method thereof |
| CN105727983B (en) * | 2014-12-11 | 2018-05-04 | 中国石油天然气股份有限公司 | Cocatalyst for fluid catalytic cracking and preparation method thereof |
| CN106975477A (en) * | 2017-05-04 | 2017-07-25 | 龙岩紫荆创新研究院 | SCR denitration preparation method and catalyst |
| CN115770585A (en) * | 2021-09-09 | 2023-03-10 | 中国石油化工股份有限公司 | For reducing NO in flue gas X And SO X Discharged catalyst, preparation method thereof and flue gas SO removal X And NO X Method (2) |
| WO2024017252A1 (en) * | 2022-07-19 | 2024-01-25 | Basf Corporation | Catalytic article comprising vanadium-containing catalyst and oxidation catalyst |
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