CN105312053A - Loaded type Pt-Pd-Mn-Ce catalyst, preparation method therefor and application of loaded type Pt-Pd-Mn-Ce catalyst in clay recovery process for treating and adsorbing sulfides in PX - Google Patents
Loaded type Pt-Pd-Mn-Ce catalyst, preparation method therefor and application of loaded type Pt-Pd-Mn-Ce catalyst in clay recovery process for treating and adsorbing sulfides in PX Download PDFInfo
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- CN105312053A CN105312053A CN201410365912.9A CN201410365912A CN105312053A CN 105312053 A CN105312053 A CN 105312053A CN 201410365912 A CN201410365912 A CN 201410365912A CN 105312053 A CN105312053 A CN 105312053A
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Abstract
The invention discloses a loaded type Pt-Pd-Mn-Ce catalyst, a preparation method therefor and application of the loaded type Pt-Pd-Mn-Ce catalyst in a clay recovery process for treating and adsorbing sulfides in PX. According to the catalyst, cordierite is coated with activated alumina so as to serve as a carrier, noble metals, i.e., platinum and palladium, zirconia and manganous nitrate are loaded to the carrier, the loaded amount of Pt is 200-600g/m<3>, the loaded amount of Pd is 50-200g/m<3>, the loaded amount of Mn is 20-40kg/m<3>, and the loaded amount of Ce is 5-15kg/m<3>. By adopting the method disclosed by the invention, the temperature of combustion of the PX and toluene in exhaust gas generated by the clay recovery process for adsorbing the sulfides in the PX can be effectively lowered, the PX and the toluene in the exhaust gas can be fully combusted without introducing external energy, and thus, the exhaust gas reaches emission standards.
Description
Technical field
The present invention relates to waste gas catalyst in a kind of absorption PX medium sulphide content clay powder recycling technique, comprise its preparation method and the application in process kind of absorption PX medium sulphide content clay powder recycling technique.
Background technology
The industrial method by bleaching earth adsorption, the sulfide in process PX, usually, carclazyte, after inefficacy, is buried after being purged by high pressure nitrogen, but due to the absorption property of carclazyte good, although purged by high pressure nitrogen, still have part PX and toluene remaining, bury and easily cause secondary pollution afterwards.In recent years, part producer proposes carclazyte to carry out roasting at 600 ~ 700 DEG C, and the complete carclazyte of roasting utilizes again.But because in the process of roasting, carclazyte inevitably discharges PX and toluene, the gas that roasting is discharged does not reach environmental administration's requirement, this processing method delays to realize.The gas temperature of roasting discharge is 200 DEG C, well below the ignition temperature of PX and toluene.How purifying this part tail gas, is that can this clay powder recycling method the key of commercial Application.
Adopt the method for catalytic combustion to reduce the ignition temperature of PX and toluene in gas, reached the object of process, but had no report about the method for the PX processed under the low temperature of 200 DEG C in this type of gas and toluene.
CN200510060542.9 discloses a kind of preparation method of rare-earth composite porous aluminium oxide loaded palladium catalyst, this catalyst take cordierite ceramic honeycomb as carrier, adopt the coating of colloidal sol dip coating hydrated alumina, hot absorption method cerium-carrying-Zirconium oxide and carried metal palladium active component, at 10000 ~ 30000h
-1under air speed, the complete oxidation temperature of catalyst to toluene and ethyl acetate is respectively 180 ~ 200 DEG C and 260 ~ 280 DEG C.But this patent does not mention bromide to catalyst activity and the impact in life-span.
The method that the exhaust fume catalytic that US4983366 discloses a kind of hydrocarbon-containifirst and carbon monoxide transforms and relevant purifier, this method makes waste gas by salic, silica and/or the zeolite containing oxide or barium, manganese, copper, chromium and nickel, again by the catalyst containing platinum and/or palladium or rhodium, this catalyst is specially adapted to the waste gas processing the generation of vinyl chloride process units.This catalyst do not mention high-strength coating on noble metal with and the impact of catalyst life.
CN95197182.4 discloses the Catalyst And Method of the gas of a kind of process containing the organic compound of halogenation, non-halogenated organic compound, carbon monoxide or its mixture, and the feature of this catalyst is the oxide containing at least one platinum group metal, zirconia and at least one manganese, cerium or cobalt.This catalyst do not mention high-strength coating on noble metal with and the impact of catalyst life.
Visible, do not administer the report of waste gas in absorption PX medium sulphide content clay powder recycling technique at present for Production by Catalytic Combustion Process, for this type of gas system, need catalyst to have very high oxidation activity and stability to PX and toluene.
Summary of the invention
The object of this invention is to provide a kind of use in absorption PX medium sulphide content clay powder recycling technique catalyst, catalyst preparation method and adopt this catalyst to apply in absorption PX medium sulphide content clay powder recycling technique.
To achieve these goals, the present invention is by the following technical solutions:
A kind of support type Pt-Pd-Mn-Ce catalyst, adopting and cordierite applies activated alumina is carrier, and by load while of noble metal platinum, palladium and zirconia and manganese nitrate thereon, load capacity is respectively: Pt:200 ~ 600g/m
3, Pd:50 ~ 200g/m
3, Mn:20 ~ 40kg/m
3, Ce:5 ~ 15kg/m
3.
The preparation method of above-mentioned support type Pt-Pd-Mn-Ce catalyst, comprises the following steps: by boehmite: water: urea: red fuming nitric acid (RFNA) mixes by the mass ratio of 1:1:0.5:0.1, ball milling 48 hours; Vacuum coating method is adopted to be coated on cordierite honeycomb ceramic by slurry, after coating, with the raffinate in pressure-air blowout ceramic honey comb duct, the ceramic honey comb applied is put 48 hours in ambient temperatare, then at 120 DEG C dry 6 hours, roasting 6 hours at 600 DEG C; The manganese nitrate aqueous solution of chloroplatinic acid, palladium bichloride, six nitric hydrate zirconiums and mass ratio 50% is become homogeneous phase solution by load capacity proportions, and adopt equi-volume impregnating load on ceramic honey comb, load capacity is: Pt:200 ~ 600g/m
3, Pd:50 ~ 200g/m
3, Mn:20 ~ 40kg/m
3, Ce:5 ~ 15kg/m
3, after load at 120 DEG C dry 6 hours, roasting 6 hours at 350 DEG C, obtained support type Pt-Pd-Mn-Ce catalyst.
Above-mentioned support type Pt-Pd-Mn-Ce catalyst is applied in process absorption PX medium sulphide content clay powder recycling technique, and comprise the following steps: Pt-Pd-Mn-Ce catalyst is placed in carclazyte calciner tail end, the PX in recovery carclazyte tail gas and toluene are at 5000 ~ 40000h
-1air speed under, carry out catalytic combustion at the temperature of 150 ~ 200 DEG C, change into water and carbon dioxide, purification after discharge.
Adopt support type Pt-Pd-Mn-Ce catalyst of the present invention, effectively can reduce the PX in absorption PX medium sulphide content clay powder recycling technique generation waste gas and toluene ignition temperature, do not need to introduce external energy, the PX in this emission gases and toluene just can be made to burn completely, reach discharge standard.
Detailed description of the invention
Below the specific embodiment of the present invention is described in detail, but it is pointed out that protection scope of the present invention not by the restriction of these detailed description of the invention, but determined by claims.
Embodiment 1
Boehmite and water are pressed the mass ratio of 1:1, boehmite and urea to mix by the mass ratio of 1:0.1 by the mass ratio of 1:0.5, boehmite and red fuming nitric acid (RFNA), ball milling 48 hours.Vacuum coating method is adopted to be coated on cordierite honeycomb ceramic by slurry, after coating, with the raffinate in pressure-air blowout ceramic honey comb duct, the ceramic honey comb applied is put 48 hours in ambient temperatare, then at 120 DEG C dry 6 hours, roasting 6 hours at 600 DEG C.The manganese nitrate aqueous solution of chloroplatinic acid solid, palladium bichloride solid, six nitric hydrate zirconium solids and mass ratio 50% is mixed with homogeneous phase solution (the unit catalyst load capacity that the proportionate relationship of four kinds of materials sees below), adopt equi-volume impregnating load on ceramic honey comb, load capacity is: Pt:200g/m
3, Pd:50g/m
3, Mn:20kg/m
3, Ce:5kg/m
3, after load at 120 DEG C dry 6 hours, at 350 DEG C, roasting 6 hours, was designated as catalyst I.Catalyst is placed in carclazyte calciner tail end, reclaims PX in carclazyte tail gas and toluene temperature 200 DEG C, air speed 5000h
-1carry out catalytic combustion, change into water and carbon dioxide, discharge after purification.
Clean-up effect: PX clearance is 99%, toluene removal rate 99%.
Embodiment 2
Boehmite and water are pressed the mass ratio of 1:1, boehmite and urea to mix by the mass ratio of 1:0.1 by the mass ratio of 1:0.5, boehmite and red fuming nitric acid (RFNA), ball milling 48 hours.Vacuum coating method is adopted to be coated on cordierite honeycomb ceramic by slurry, after coating, with the raffinate in pressure-air blowout ceramic honey comb duct, the ceramic honey comb applied is put 48 hours in ambient temperatare, then at 120 DEG C dry 6 hours, roasting 6 hours at 600 DEG C.The manganese nitrate aqueous solution of chloroplatinic acid, palladium bichloride, six nitric hydrate zirconiums and mass ratio 50% is mixed with homogeneous phase solution (the unit catalyst load capacity that the proportionate relationship of four kinds of materials sees below), adopt equi-volume impregnating load on ceramic honey comb, load capacity is: Pt:600g/m
3, Pd:200g/m
3, Mn:40kg/m
3, Ce:15kg/m
3, after load at 120 DEG C dry 6 hours, at 350 DEG C, roasting 6 hours, was designated as catalyst I I.Catalyst is placed in carclazyte calciner tail end, reclaims PX in carclazyte tail gas and toluene temperature 150 DEG C, air speed 40000h
-1under carry out catalytic combustion, change into water and carbon dioxide, purification after discharge.
Clean-up effect: PX clearance is 90%, toluene removal rate 90%.
Embodiment 3
Boehmite and water are pressed the mass ratio of 1:1, boehmite and urea to mix by the mass ratio of 1:0.1 by the mass ratio of 1:0.5, boehmite and red fuming nitric acid (RFNA), ball milling 48 hours.Vacuum coating method is adopted to be coated on cordierite honeycomb ceramic by slurry, after coating, with the raffinate in pressure-air blowout ceramic honey comb duct, the ceramic honey comb applied is put 48 hours in ambient temperatare, then at 120 DEG C dry 6 hours, roasting 6 hours at 600 DEG C.The manganese nitrate aqueous solution of chloroplatinic acid, palladium bichloride, six nitric hydrate zirconiums and mass ratio 50% is mixed with homogeneous phase solution (the unit catalyst load capacity that the proportionate relationship of four kinds of materials sees below), adopt equi-volume impregnating load on ceramic honey comb, load capacity is: Pt:400g/m
3, Pd:100g/m
3, Mn:30kg/m
3, Ce:10kg/m
3, after load at 120 DEG C dry 6 hours, at 350 DEG C, roasting 6 hours, was designated as catalyst I II.Catalyst is placed in carclazyte calciner tail end, temperature 200 DEG C, air speed 20000h
-1under carry out catalytic combustion, change into water and carbon dioxide, purification after discharge.
Clean-up effect: PX clearance is 99%, toluene removal rate 99%.
Catalyst I is placed in carclazyte calciner tail end by embodiment 4, reclaims PX in carclazyte tail gas and toluene temperature 200 DEG C, air speed 20000h
-1under carry out catalytic combustion, change into water and carbon dioxide, purification after discharge.
Clean-up effect: PX clearance is 95%, toluene removal rate 95%.
Embodiment 5
Catalyst I I is placed in carclazyte calciner tail end, reclaims PX in carclazyte tail gas and toluene temperature 200 DEG C, air speed 20000h
-1under carry out catalytic combustion, change into water and carbon dioxide, purification after discharge.
Clean-up effect: PX clearance is 99%, toluene removal rate 99%.
Embodiment 6
Catalyst I II is placed in carclazyte calciner tail end, reclaims PX in carclazyte tail gas and toluene temperature 150 DEG C, air speed 20000h
-1under carry out catalytic combustion, change into water and carbon dioxide, purification after discharge.
Clean-up effect: PX clearance is 95%, toluene removal rate 95%.
Embodiment 7
Catalyst I II is placed in carclazyte calciner tail end, reclaims PX in carclazyte tail gas and toluene temperature 180 DEG C, air speed 20000h
-1under carry out catalytic combustion, change into water and carbon dioxide, purification after discharge.
Clean-up effect: PX clearance is 99%, toluene removal rate 99%.
Table 1 catalyst coat intensity effect list
Known by the result of the test data of sequence number in table 11, the waste gas that the catalyst adopting this method to prepare produces for the treatment of absorption PX medium sulphide content clay powder recycling technique, even if at lower noble-metal-supported amount (Pt:200g/m
3, Pd:50g/m
3, Mn:20kg/m
3, Ce:5kg/m
3) time, as long as air speed is not too high, also good effect can be obtained.
In contrast table 1, the result of the test data of sequence number 1,3 and 7 are known, the waste gas that the catalyst adopting this method to prepare produces for the treatment of absorption PX medium sulphide content clay powder recycling technique, at air speed 5000-4000h
-1, under the service condition of temperature 150-200 DEG C, there is good result of use.
In contrast table 1, the result of the test data of sequence number 2 and 7 are known, the waste gas that the catalyst adopting this method to prepare produces for the treatment of absorption PX medium sulphide content clay powder recycling technique, are 20000h in air speed
-1there is better result of use.
In contrast table 1, the result of the test data of sequence number 2,6 and 7 are known, the waste gas that the catalyst adopting this method to prepare produces for the treatment of absorption PX medium sulphide content clay powder recycling technique, under the service condition of temperature 180-200 DEG C, and the better result of use of tool.
Although be described in detail the specific embodiment of the present invention above in conjunction with the embodiments, it is pointed out that protection scope of the present invention not by the restriction of these detailed description of the invention, but determined by claims.Those skilled in the art can carry out suitable change to these embodiments in the scope not departing from technological thought of the present invention and purport, and the embodiment after these changes is obviously also included within protection scope of the present invention.
Claims (3)
1. a support type Pt-Pd-Mn-Ce catalyst, is characterized in that: described catalyst adopts and cordierite applies activated alumina is carrier, and by load while of noble metal platinum, palladium and zirconia and manganese nitrate thereon, load capacity is respectively: Pt:200 ~ 600g/m
3, Pd:50 ~ 200g/m
3, Mn:20 ~ 40kg/m
3, Ce:5 ~ 15kg/m
3.
2. a preparation method for support type Pt-Pd-Mn-Ce catalyst according to claim 1, is characterized in that comprising the following steps:
By boehmite: water: urea: red fuming nitric acid (RFNA) presses the mass ratio mixing of 1:1:0.5:0.1, ball milling 48 hours; Vacuum coating method is adopted to be coated on cordierite honeycomb ceramic by slurry, after coating, with the raffinate in pressure-air blowout ceramic honey comb duct, the ceramic honey comb applied is put 48 hours in ambient temperatare, then at 120 DEG C dry 6 hours, roasting 6 hours at 600 DEG C;
The manganese nitrate aqueous solution of chloroplatinic acid, palladium bichloride, six nitric hydrate zirconiums and mass ratio 50% is become homogeneous phase solution by load capacity proportions, and adopt equi-volume impregnating load on ceramic honey comb, load capacity is: Pt:200 ~ 600g/m
3, Pd:50 ~ 200g/m
3, Mn:20 ~ 40kg/m
3, Ce:5 ~ 15kg/m
3, after load at 120 DEG C dry 6 hours, roasting 6 hours at 350 DEG C, obtained support type Pt-Pd-Mn-Ce catalyst.
3. one kind according to claim 1 support type Pt-Pd-Mn-Ce catalyst apply in process absorption PX medium sulphide content clay powder recycling technique, it is characterized in that comprising the following steps: support type Pt-Pd-Mn-Ce catalyst is placed in carclazyte calciner tail end, the PX in recovery carclazyte tail gas and toluene are at 5000 ~ 40000h
-1air speed under, carry out catalytic combustion at the temperature of 150 ~ 200 DEG C, change into water and carbon dioxide, purification after discharge.
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| CN201410365912.9A CN105312053B (en) | 2014-07-29 | 2014-07-29 | Support type Pt-Pd-Mn-Ce catalyst, preparation method and the application in processing absorption PX in sulfide clay powder recycling technique |
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Cited By (4)
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| CN107344098A (en) * | 2016-05-06 | 2017-11-14 | 中国石化扬子石油化工有限公司 | A kind of preparation method of catalyst for PTA vent gas treatments |
| CN109261151A (en) * | 2018-10-29 | 2019-01-25 | 天津科技大学 | A kind of bimetallic catalyst of preparing propylene by dehydrogenating propane as well as preparation method and application thereof |
| CN112547112A (en) * | 2020-12-31 | 2021-03-26 | 河南神马催化科技股份有限公司 | Palladium catalyst for removing trace sulfide in benzene |
| CN113277473A (en) * | 2021-05-13 | 2021-08-20 | 万华化学（宁波）有限公司 | Process for decomposing residual chlorine in hydrochloric acid |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107344098A (en) * | 2016-05-06 | 2017-11-14 | 中国石化扬子石油化工有限公司 | A kind of preparation method of catalyst for PTA vent gas treatments |
| CN107344098B (en) * | 2016-05-06 | 2020-11-10 | 中国石化扬子石油化工有限公司 | Preparation method of catalyst for PTA tail gas treatment |
| CN109261151A (en) * | 2018-10-29 | 2019-01-25 | 天津科技大学 | A kind of bimetallic catalyst of preparing propylene by dehydrogenating propane as well as preparation method and application thereof |
| CN112547112A (en) * | 2020-12-31 | 2021-03-26 | 河南神马催化科技股份有限公司 | Palladium catalyst for removing trace sulfide in benzene |
| CN113277473A (en) * | 2021-05-13 | 2021-08-20 | 万华化学（宁波）有限公司 | Process for decomposing residual chlorine in hydrochloric acid |
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