CN107344098A - A kind of preparation method of catalyst for PTA vent gas treatments - Google Patents
A kind of preparation method of catalyst for PTA vent gas treatments Download PDFInfo
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- CN107344098A CN107344098A CN201610298283.1A CN201610298283A CN107344098A CN 107344098 A CN107344098 A CN 107344098A CN 201610298283 A CN201610298283 A CN 201610298283A CN 107344098 A CN107344098 A CN 107344098A
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- catalyst
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- honeycomb ceramic
- cordierite honeycomb
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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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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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
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/656—Manganese, technetium or rhenium
- B01J23/6562—Manganese
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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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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Abstract
The present invention relates to a kind of preparation method of the catalyst for PTA vent gas treatments, active oxidation aluminized coating is coated on cordierite honeycomb ceramic, the dosage of activated alumina is the 15 30% of cordierite honeycomb ceramic weight, cordierite honeycomb ceramic after coating is soaked in deionized water, then the moisture in the cordierite honeycomb ceramic duct after coating is removed, it is immersed in again in isometric activity component impregnation liquid, is finally dried, be calcined, produced.The catalyst activity component of catalyst of the present invention is uniformly distributed, and will not in PTA tail gas poisoning and deactivation, the performance for improving catalyst and the preparation cost for reducing catalyst.
Description
Technical field
The present invention relates to a kind of method for being used to handle the load of PTA tail gas ceramic honeycomb catalysts active component, using the present invention
Method carries out the load of catalyst activity component, that is, active component is uniformly distributed, avoids the waste of active component again,
To improving the performance of catalyst and reducing the preparation cost of catalyst, there is extraordinary effect.
Background technology
At present, industrial production p-phthalic acid (PTA) mainly uses high-temperature liquid-phase oxidizing process, is with paraxylene (PX)
For raw material, cobalt acetate, manganese acetate are catalyst, the reaction system that bromide is accelerator, air is oxidant.Along with
PX is oxidized to PTA, there is the generation of the side reaction such as PX and acetic acid burning, and combustion product mainly has CO, CO2And acetic acid
The organic matters such as methyl esters.The PTA exhaust gas treatment technologies of commercial Application mainly have two classes, i.e. thermal oxide and catalytic oxidation technologies, its
Middle catalytic oxidation technologies can make operation temperature reduce by 400~600 DEG C by means of the effect of catalyst.Therefore, catalytic oxidation is
Processing waste gas containing esters is most direct, most efficient method.
At present, such exhaust gas treatment catalyst, which typically uses, coats activated alumina as carrier on cordierite honeycomb ceramic, load
Noble metal and catalyst aid are active component.Activated alumina on cordierite honeycomb ceramic is referred to as coating, and the intensity of coating exists
Determine the service life of catalyst.For the relatively low honeycomb catalyst of strength of coating, it is general use increase noble metal dosage with
Catalyst life is improved, but manufacturing cost greatly increases.
In the preparation technology of this kind of catalyst, the load of active component typically uses excessive infusion process and equi-volume impregnating, this
Two methods cut both ways.Excessive infusion process can ensure the uniformity of active component load, but inevitably have portion
Divide active component not load on a catalyst, cause to waste, this method is nowadays seldom used；Though and equi-volume impregnating
So avoid waste, but easily cause active component disperse it is uneven.
The Chinese patent of Application No. 200510060542.9 discloses a kind of rare-earth composite porous aluminium oxide loaded palladium catalyst
Preparation method, the catalyst using cordierite ceramic honeycomb as carrier, using colloidal sol dip coating coat hydrated alumina, heat inhale
Attached method cerium-carrying-Zirconium oxide and carried metal palladium active component (i.e. equi-volume impregnating), in 10000~30000h-1It is empty
Under speed, catalyst is respectively 180~200 DEG C and 260~280 DEG C to the complete oxidation temperature of toluene and ethyl acetate.This side
Catalyst there is active component and disperse the problem of uneven made from method, and the bromide in PTA tail gas easily makes catalyst
Poisoning, so as to fail.
Therefore, a kind of suitable active component carrying method is found, that is, active component is uniformly distributed, avoids activity again
The waste of component, and activity can be kept in environment existing for bromide, to improving the performance of catalyst and reducing catalyst
Preparation cost, all tool be of great significance.
The content of the invention
It is scattered not it is an object of the invention to overcome the catalyst for being used for PTA vent gas treatments in the prior art active component to be present
The problem of uniform, there is provided a kind of preparation method of catalyst for PTA vent gas treatments, obtained catalyst activity component are equal
Even distribution, the performance for improving catalyst and the preparation cost for reducing catalyst.
Technical scheme
A kind of preparation method of catalyst for PTA vent gas treatments：Activated alumina is coated on cordierite honeycomb ceramic
Coating, the dosage of activated alumina is the 15-30% of cordierite honeycomb ceramic weight, by the cordierite honeycomb ceramic after coating
Soak in deionized water, then remove the moisture in the cordierite honeycomb ceramic duct after coating, then the body such as be immersed in
In long-pending activity component impregnation liquid, finally dried, be calcined, get product catalyst.
Further, the time that the cordierite honeycomb ceramic after coating soaks in deionized water is 1~12h；
Further, the method for removing the moisture in the cordierite honeycomb ceramic duct after coating is to use centrifuge, and centrifugation turns
Speed is 400-1000r/min, time 5-20min.
Further, in the activity component impregnation liquid, the chloroplatinic acid containing 50-1000mg/L, 25-500mg/L palladium bichlorides,
1-30g/L cerous nitrates and 2-100g/L manganese nitrates.
Further, the time of the dipping in activity component impregnation liquid is 12~48h.
Further, the temperature of the drying is 110-130 DEG C, time 10-16h.
Further, the sintering temperature is 380-450 DEG C, time 10-18h.
Beneficial effect：Using catalyst made from present invention process, catalyst activity component is uniformly distributed, and will not be
Poisoning and deactivation in PTA tail gas, the performance for improving catalyst and the preparation cost for reducing catalyst.
Embodiment
With reference to specific embodiment, the invention will be further described.In following embodiments, experiment is using identical activity
Component maceration extract, while be compared using equi-volume impregnating and excessive infusion process, finally by the work to finished catalyst
Property analysis judge remarkable result of the embodiment of the present invention compared with first two dipping method.
Embodiment 1
Active oxidation aluminized coating is coated on cordierite honeycomb ceramic, the dosage of activated alumina is cordierite honeycomb ceramic weight
The 15% of amount, the cordierite honeycomb ceramic for coating activated alumina is soaked into 1h in deionized water, then thrown away with centrifuge
Moisture in its duct, centrifuge speed 500r/min, time 10min, then put it into isometric active component
Maceration extract is impregnated.Dip time is 12h, toasts 12h at 120 DEG C thereafter, and 12h is calcined at 400 DEG C, you can
Obtain finished catalyst.Activity component impregnation liquid composition：Chloroplatinic acid containing 200mg/L, 100mg/L palladium bichlorides, 30g/L
Cerous nitrate and 50g/L manganese nitrates.
Comparative example 1-1
Equi-volume impregnating：The cordierite honeycomb ceramic for coating activated alumina is put into the activearm sub-dip isometric with it
Stain liquid is impregnated.The composition of activity component impregnation liquid is consistent with embodiment 1.Dip time is 12h, thereafter at 120 DEG C
Lower baking 12h, is calcined 12h, you can obtain finished catalyst at 400 DEG C.
Comparative example 1-2
Excessive infusion process：It is 2 that the cordierite honeycomb ceramic for coating activated alumina, which is put into its volume ratio,:1 activearm
Maceration extract is divided to be impregnated.The composition of activity component impregnation liquid is consistent with embodiment 1.Dip time is 12h, thereafter at 120 DEG C
Lower baking 12h, is calcined 12h, you can obtain finished catalyst at 400 DEG C.
Embodiment 2
Active oxidation aluminized coating is coated on cordierite honeycomb ceramic, the dosage of activated alumina is cordierite honeycomb ceramic weight
The 20% of amount, the cordierite honeycomb ceramic for coating activated alumina is soaked into 6h in deionized water, then thrown away with centrifuge
Moisture in its duct, centrifuge speed 700r/min, time 15min, then put it into isometric active component
Maceration extract is impregnated.Dip time is 48h, toasts 15h at 130 DEG C thereafter, and 14h is calcined at 450 DEG C, you can
Obtain finished catalyst.Activity component impregnation liquid composition：Chloroplatinic acid containing 600mg/L, 500mg/L palladium bichlorides, 10g/L
Cerous nitrate and 80g/L manganese nitrates.
Comparative example 2-1
Equi-volume impregnating：The cordierite honeycomb ceramic for coating activated alumina is put into the activearm sub-dip isometric with it
Stain liquid is impregnated.The composition of activity component impregnation liquid is consistent with embodiment 2.Dip time is 48h, thereafter at 130 DEG C
Lower baking 15h, is calcined 14h, you can obtain finished catalyst at 450 DEG C.
Comparative example 2-2
Excessive infusion process：It is 2 that the cordierite honeycomb ceramic for coating activated alumina, which is put into its volume ratio,:1 activearm
Maceration extract is divided to be impregnated.The composition of activity component impregnation liquid is consistent with embodiment 2.Dip time is 48h, thereafter at 130 DEG C
Lower baking 15h, is calcined 14h, you can obtain finished catalyst at 450 DEG C.
Embodiment 3
Active oxidation aluminized coating is coated on cordierite honeycomb ceramic, the dosage of activated alumina is cordierite honeycomb ceramic weight
The 30% of amount, the cordierite honeycomb ceramic for coating activated alumina is soaked into 10h in deionized water, then got rid of with centrifuge
The moisture gone out in its duct, centrifuge speed 900r/min, time 5min, then put it into isometric activearm
Maceration extract is divided to be impregnated.Dip time is 24h, toasts 12h at 120 DEG C thereafter, 16h is calcined at 400 DEG C, i.e.,
It can obtain finished catalyst.Activity component impregnation liquid composition：Chloroplatinic acid containing 800mg/L, 300mg/L palladium bichlorides, 20g/L
Cerous nitrate and 30g/L manganese nitrates.
Comparative example 3-1
Equi-volume impregnating：The cordierite honeycomb ceramic (carrier) for coating activated alumina is put into isometric with it
Activity component impregnation liquid is impregnated.The composition of activity component impregnation liquid is consistent with the above.Dip time is 24h, is existed thereafter
12h is toasted at 120 DEG C, is calcined 16h at 400 DEG C, you can obtain finished catalyst.
Comparative example 3-2
Excessive infusion process：It is 2 that the cordierite honeycomb ceramic (carrier) for coating activated alumina, which is put into its volume ratio,:1
Activity component impregnation liquid impregnated.The composition of activity component impregnation liquid is consistent with the above.Dip time is 12h, thereafter
12h is toasted at 120 DEG C, is calcined 16h at 400 DEG C, you can obtain finished catalyst.
Performance test
After the finished catalyst that embodiment and comparative example are obtained, using fixed-bed catalytic evaluating apparatus, with methyl acetate
Conversion ratio is index, and its activity is evaluated.The operating condition of evaluation test：300 DEG C of temperature, air speed 30000h-1,
The concentration 100mg/m of methyl acetate3.Analysis comparing result is shown in Table 1.
Table 1
| Methyl acetate conversion ratio (%) | |
| Embodiment 1 | 99.15 |
| Comparative example 1-1 | 95.12 |
| Comparative example 1-2 | 93.15 |
| Embodiment 2 | 99.95 |
| Comparative example 2-1 | 95.41 |
| Comparative example 2-2 | 90.32 |
| Embodiment 3 | 99.56 |
| Comparative example 3-1 | 94.36 |
| Comparative example 3-2 | 92.16 |
Using the methyl acetate conversion ratio of catalyst made from the inventive method than existing it can be seen from the test result of upper table
High using catalyst made from equi-volume impregnating and excessive infusion process in technology, this explanation is using made from the inventive method
The activity of catalyst is better than comparative example.
Claims (7)
1. the preparation method of a kind of catalyst for PTA vent gas treatments, it is characterised in that coated on cordierite honeycomb ceramic
Active oxidation aluminized coating, the dosage of activated alumina is the 15-30% of cordierite honeycomb ceramic weight, by the cordierite honeybee after coating
Nest ceramics soak in deionized water, then remove the moisture in the cordierite honeycomb ceramic duct after coating, then be immersed in
In isometric activity component impregnation liquid, finally dried, be calcined, get product catalyst.
2. it is used for the preparation method of the catalyst of PTA vent gas treatments as claimed in claim 1, it is characterised in that after coating
The time that cordierite honeycomb ceramic soaks in deionized water is 1~12h.
3. it is used for the preparation method of the catalyst of PTA vent gas treatments as claimed in claim 1, it is characterised in that remove and apply
The method of the moisture in cordierite honeycomb ceramic duct after layer is to use centrifuge, centrifugal rotational speed 400-1000r/min, when
Between be 5-20min.
4. it is used for the preparation method of the catalyst of PTA vent gas treatments as claimed in claim 1, it is characterised in that the activity
In component maceration extract, the chloroplatinic acid containing 50-1000mg/L, 25-500mg/L palladium bichlorides, 1-30g/L cerous nitrates and 2-100g/L
Manganese nitrate.
5. it is used for the preparation method of the catalyst of PTA vent gas treatments as claimed in claim 1, it is characterised in that in activity
The time of dipping in component maceration extract is 12~48h.
6. it is used for the preparation method of the catalyst of PTA vent gas treatments as claimed in claim 1, it is characterised in that the baking
Dry temperature is 110-130 DEG C, time 10-16h.
7. the preparation method of the catalyst for PTA vent gas treatments as described in any one of claim 1 to 6, it is characterised in that
Further, the sintering temperature is 380-450 DEG C, time 10-18h.
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| CN201610298283.1A CN107344098B (en) | 2016-05-06 | 2016-05-06 | Preparation method of catalyst for PTA tail gas treatment |
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| CN201610298283.1A CN107344098B (en) | 2016-05-06 | 2016-05-06 | Preparation method of catalyst for PTA tail gas treatment |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111054374A (en) * | 2018-10-16 | 2020-04-24 | 中国石油化工股份有限公司 | Catalytic combustion catalyst for PTA oxidized tail gas and application thereof |
| CN111921527A (en) * | 2020-08-20 | 2020-11-13 | 南京蓝领环境科技有限公司 | Method for treating honeycomb ceramic catalyst active component load containing VOCs waste gas |
| CN113042048A (en) * | 2021-03-23 | 2021-06-29 | 江苏三一环境科技有限公司 | VOCs treatment catalyst and preparation method and application thereof |
| CN113877603A (en) * | 2020-07-01 | 2022-01-04 | 中国石油化工股份有限公司 | Monolithic catalyst, process for producing the same, and process for purifying exhaust gas containing bromine-containing organic substance |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111054374A (en) * | 2018-10-16 | 2020-04-24 | 中国石油化工股份有限公司 | Catalytic combustion catalyst for PTA oxidized tail gas and application thereof |
| CN113877603A (en) * | 2020-07-01 | 2022-01-04 | 中国石油化工股份有限公司 | Monolithic catalyst, process for producing the same, and process for purifying exhaust gas containing bromine-containing organic substance |
| CN113877603B (en) * | 2020-07-01 | 2024-03-26 | 中国石油化工股份有限公司 | Monolithic catalyst, method for producing the same, and method for purifying exhaust gas containing bromine-containing organic matter |
| CN111921527A (en) * | 2020-08-20 | 2020-11-13 | 南京蓝领环境科技有限公司 | Method for treating honeycomb ceramic catalyst active component load containing VOCs waste gas |
| CN113042048A (en) * | 2021-03-23 | 2021-06-29 | 江苏三一环境科技有限公司 | VOCs treatment catalyst and preparation method and application thereof |
| CN113042048B (en) * | 2021-03-23 | 2024-01-30 | 江苏三一环境科技有限公司 | VOCs (volatile organic compounds) treatment catalyst and preparation method and application thereof |
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