CN101722020A - Eutectic zeolite catalyst containing EUO structure and preparation method and application thereof - Google Patents
Eutectic zeolite catalyst containing EUO structure and preparation method and application thereof Download PDFInfo
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- CN101722020A CN101722020A CN200810224438A CN200810224438A CN101722020A CN 101722020 A CN101722020 A CN 101722020A CN 200810224438 A CN200810224438 A CN 200810224438A CN 200810224438 A CN200810224438 A CN 200810224438A CN 101722020 A CN101722020 A CN 101722020A
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Abstract
The invention relates to an eutectic zeolite catalyst containing an EUO structure and a preparation method and application thereof, wherein the eutectic zeolite catalyst comprises hydrogen type zeolite containing the EUO structure, an adhesive and a VIII family element in an element period table; the zeolite contains silicon and aluminum and/or an element T of magnesium, and the atomic ratio of Si/T is 8-100; the content of the hydrogen type zeolite containing the EUO structure is 1-90wt%; the bearing capacity of a VIII family metal is 0.01-2.0wt%; the adhesive accounts for the rest quality; the gross weight is 100 percent; and in an isomerization reaction of C8 aromatics, the reactive activity can be greatly improved, the transforming quantity of ethylbenzene to xylene as a target product is improved; meanwhile, the side reaction in the isomerization process can be effectively inhabited.
Description
Technical field
The present invention relates to a kind of adopt solid-phase synthesis synthetic the eutectic zeolite isomerization of C-8 aromatics catalyst and preparation and the application that contain the EUO structure.
Technical background
At present, the industrial isomerization of C-8 aromatics catalyst that uses has ethylbenzene conversion to take off the technology that ethyl is converted into benzene as the technology and the ethylbenzene of dimethylbenzene.Used metal constituent element is noble metal platinum basically in the catalyst, though on the content and mode of loading on different, but do not have big difference, the used acidic zeolite constituent element of each catalyst is then had any different: be the technology of dimethylbenzene for ethylbenzene conversion, the I-400 catalyst of UOP is a UZM series, the OPARIS catalyst of IFP is an EUO series, and the SKI-400 catalyst of SINOPEC-RIPP is a MOR series; Take off the technology that ethyl is converted into benzene for ethylbenzene, the SKI-100 catalyst of the I-300 catalyst of UOP, the EB-4500 catalyst of EXXON-MOBIL and SINOPEC-RIPP is ZSM-5 series, but has nothing in common with each other on the catalyst performance.
Patent ZL89100145X discloses the noble metal support type isomerization catalyst that contains MOR, and its used molecular sieve is MOR, and catalyst performance is isomerization activity PX/ ∑ X 〉=21.5%, conversion of ethylbenzene EBc 〉=25%, carbon eight hydrocarbon yield C
8Y 〉=96.5%.In other similar patent ZL95116456.2, ZL95116460.0, ZL95116461.9, be based on the catalyst that MOR is a main body equally, added a small amount of other acid active components, to improve catalyst performance.
Patent US6,723,301B2, US6,616,910, US6,514,479B1, US6,147,269 grades disclose molecular sieve EUO and have been used for C
8The technology of aromatics isomerization reaction.Patent has also related to the modification processing method of catalyst simultaneously, as ammonia passivation, presulfurization etc.
By using concrete processing and/or prescription optimization, can slacken the shortcoming of MOR poor selectivity, described in FR-A-2691914.This technology can reduce the disproportionation side reaction.
US5,908,967 disclose a kind of by isomerization catalyst is carried out the method that modification reduces side reaction, in catalyst manufacturing process,, suppress part highly acid center to molecular sieve MOR metallic cerium modification, reduce the degree of disproportionation side reaction, improve the yield of dimethylbenzene.
For the isomerization of C-8 aromatics catalyst, the index that characterizes its performance mainly is isomerization activity PX/ ∑ X, conversion of ethylbenzene EBc, carbon eight hydrocarbon yield (C
8Index such as Y).Present industrial operation catalyst still exists activity and selectivity defective on the low side.Selection of catalysts (C
8Y) reason on the low side is mainly caused by side reaction, produces C as cracking
7Following non-aromatics, disproportionation and transalkylation produce benzene, toluene and C
9Above heavy aromatics.Therefore, the new catalyst that exploitation activity and selectivity are higher is particularly important.
Summary of the invention
The purpose of this invention is to provide a kind of adopt synthetic catalyst that contains the EUO structural zeolite of solid-phase synthesis and the application in isomerization of C-8 aromatics thereof.Specifically, with at least a zeolite and binding agent (as the aluminium oxide) moulding that contains the EU-1 structure, prepare catalyst through processes such as roasting, ion-exchange, modification processing, metal depositions.With C8 aronmatic mixture or monomer whose hydrocarbon is that raw material and above-mentioned catalyst are in the appropriate processing condition haptoreaction, can obtain isomerization activity than the higher and better reaction effect of selectivity, improve the selective conversion of ethylbenzene to dimethylbenzene, reduce disproportionation and transalkylation reaction significantly, the simultaneous isomerization activity remains on high level.
Catalyst of the present invention is a kind of zeolite catalyst of containing metal active component, and wherein each component and character thereof are:
Adopt the synthetic h-type zeolite that contains the EUO structure of solid-phase synthesis, for example EU-1/MOR eutectic zeolite partly or entirely is a Hydrogen; The element T that contains silicon and aluminium and/or magnesium, total Si/T atomic ratio are greater than 8, preferably in 8 to 100 scope;
Adhesive, preferred aluminium oxide;
Periodic table of elements group VIII element, preferred platinum or palladium.
Described catalyst is characterised in that:
By chemisorbed, H for example
2-O
2The decentralization of one or more metals of the described group VIII that titration or carbon monoxide chemisorbed are measured, it is in 50%～100% scope;
Macroscopical breadth coefficient of described one or more metals is in 0.1～1.0 scope, and is preferred 0.2 to 0.6, and described macroscopical breadth coefficient is defined as the ratio of concentration of metal described in the particle cores and grain edges concentration;
With the conventional catalyst strength measurement method measure with the radially crushing strength of the catalyst of extrudate form (as the cylinder bar shaped) greater than 80N/cm, it characterizes catalyst mechanical strength.
This catalyst is used for the hydrocarbon conversion such as C8 aronmatic cut, promptly by dimethylbenzene and ethylbenzene and/or contain the alkane of eight carbon and during the isomerization of the mixed material that the mixture of cycloalkane constitutes, fabulous catalytic performance is arranged.
Adhesive is by being selected from natural clay (as kaolin, attapulgite, bentonite etc.), synthesis of clay, magnesia, aluminium oxide, silica, silica-alumina, titanium oxide, boron oxide, oxygen
The mixture of one or more in change zirconium, aluminum phosphate, the titanium phosphate, preferred aluminium oxide.
The zeolite that EUO type structure is arranged that the employing solid-phase synthesis that is comprised in the catalyst of the present invention is synthetic, preferred EU-1/MOR eutectic zeolite, its be to small part, preferred almost all be Hydrogen.
Each weight percentages of components of catalyst of the present invention is:
The h-type zeolite that contains the EUO structure of (1) 1～90wt%;
The group VIII element of (2) 0.01～2.00wt%;
(3) surplus is an adhesive.
The present invention relates to this Preparation of catalysts method is: (1) is at first with well known to a person skilled in the art that any method processing has the zeolite of EUO type structure (for example preferably adopting the synthetic EU-1/MOR eutectic zeolite of solid-phase synthesis), for example roasting in dry air, roasting under the preferred low oxygen concentration nitrogen atmosphere is to remove the organic template agent that exists in the building-up process mesolite micropore; (2) then, the zeolite of preferred matrix binder (as aluminium oxide) and above-mentioned preparation is evenly mixed, moulding, preferred extruded moulding is more preferably made the cylinder bar shaped; During moulding, for every kind of matrix, by well known to a person skilled in the art principle, determine condition of molding, choice of base, optional matrix peptization medium and content, interpolation pore former, hybrid mode and time, extrusion pressure, baking temperature and the duration of zeolite, to obtain catalyst base; (3) then, preferably dry in advance at 200～600 ℃ roasting temperature, ℃ following oven dry a few hours in room temperature～200 for example are slowly to remove institute's water content.Drying steps preferably carries out before carrying out the required intensification of roasting, optionally carries out as hothouse or the vertical activation furnace of taking care of health with specific installation; (4) use at least a NH then
4The Cl aqueous solution carries out primary ions exchange step at least, give-and-take conditions are controlled at 60～90 ℃ of temperature, preferred 2～4 hours of swap time,, preferably remove nearly all alkali metal cation to remove at least some alkali metal cations (particularly sodium ion) that zeolite cation position exists; (5) the catalyst granules carrier after the exchange needs roasting and preliminary treatment, and the preferred pretreatment step is carried out after roasting, 200～600 ℃ of general sintering temperatures; The preferred water heat treatment method, temperature is at 200～500 ℃.(6) pretreated carrier is in room temperature～95 ℃, under liquid-solid ratio 1.2～2.0 conditions, flood (preferred 2～24 hours) or exchange (preferred 2～12 hours) with platinum acid chloride solution, palladium chloride solution or platinum ammonium complex ion, to deposit needed metallic element, preferable alloy platinum.And optionally carrying out after the zeolite preliminary treatment, carrying out after the ammonium exchange step, carrying out after the carrier preliminary treatment with the step of exchanged form plated metal.At last, after filtration, after the drying, 200～550 ℃ of activation are 2～8 hours under air atmosphere, can be prepared into catalyst of the present invention.
The invention still further relates to the isomerization method of C8 aronmatic.
The operating condition of this method is generally as follows:
Temperature is in 300～500 ℃ scope;
Hydrogen partial pressure is in the scope of 0.3～1.5MPa;
Charging air speed (representing with charging (kg)/catalyst (kg)/h) is at 0.25～20h
-1Scope in;
Hydrogen to oil volume ratio is in the scope of 600～1500/v/v.
Catalyst preparation process of the present invention is simple, except that having fabulous mechanical crushing strength, transform as C8 aronmatic for hydrocarbon,, fabulous catalytic performance is arranged promptly by dimethylbenzene and ethylbenzene and/or contain the alkane of eight carbon and the isomerization of the mixed material that the mixture of cycloalkane constitutes.
The specific embodiment
Following example explanation the present invention, and the scope that does not limit the present invention in any way.
Embodiment 1
The Si/Al that contains 35.0wt% is than the preparation that is the catalyst C1 of 30 EU-1/MOR eutectic zeolite, 64.65% aluminium oxide and 0.35% platinum.
Synthetic Si/Al is fully mixed than the EU-1/MOR eutectic zeolite and the aluminium-hydroxide powder that are 30,3% aqueous solution of nitric acid for preparing is joined in the mixture of powders mix, then with the mixture extruded moulding.The bar shaped mixture at room temperature left standstill 4 hours, and drying is after 6 hours down at 120 ℃ again, and with the strip pelletizing, length is 3～8 millimeters (wherein 4～6 millimeters particle accounts for more than 80%), makes carrier in 4 hours in 500 ℃ of roastings under air atmosphere.Press zeolite: NH
4Cl=1: 0.26 ratio is prepared the aqueous solution of 3% ammonium chloride, under 90 ℃ of water bath condition made carrier and aqueous ammonium chloride solution is carried out ion-exchange 2 hours then, washs to mother liquor and does not have chlorion.The gained carrier flooded 12 hours at normal temperatures with chloroplatinic acid in the presence of competitive adsorbate (trichloroacetic acid).Make wet solid 60 ℃ of diffusions 1 hour then, 140 ℃ of dryings 2 hours.Catalyst after 2 hours, is used hydrogen reducing 4 hours in 1 hour, 370 ℃ following 2 hours, 500 ℃ following roastings of 200 ℃ of dryings, make the catalyst C1 of platiniferous 0.35wt%.
Embodiment 2
The Si/Al that contains 35.00wt% is than the preparation that is the catalyst C2 of 60 EU-1/MOR eutectic zeolite, 64.65% aluminium oxide and 0.35% platinum.
After 350 ℃ of roastings were handled in 4 hours in the nitrogen of 5% oxygen concentration than the EU-1/MOR eutectic zeolite that is 60 with synthetic Si/Al, fully mix with aluminium-hydroxide powder, 3% aqueous solution of nitric acid for preparing joined in the mixture of powders mix, then with the mixture extruded moulding.The bar shaped mixture at room temperature left standstill 4 hours, and drying is after 6 hours down at 120 ℃ again, and with the strip pelletizing, length is 3～8 millimeters (wherein 4～6 millimeters particle accounts for more than 80%), makes carrier in 4 hours in 500 ℃ of roastings under air atmosphere.Press zeolite: NH
4Cl=1: 0.26 ratio is prepared the aqueous solution of 3% ammonium chloride, under 90 ℃ of water bath condition made carrier and aqueous ammonium chloride solution is carried out ion-exchange 2 hours then, washs to mother liquor and does not have chlorion.With after the catalyst base roasting after the ammonium exchange 450 ℃ of following hydrothermal treatment consists 4 hours, the gained carrier in the presence of competitive adsorbate (trichloroacetic acid) and chloroplatinic acid flooded at normal temperatures 12 hours.Make wet solid 60 ℃ of diffusions 1 hour then, 140 ℃ of dryings 2 hours.Catalyst after 2 hours, is used hydrogen reducing 4 hours in 1 hour, 370 ℃ following 2 hours, 500 ℃ following roastings of 200 ℃ of dryings, make the catalyst C2 of platiniferous 0.35% (weight).
Embodiment 3 (not being catalyst of the present invention)
The Si/Al that contains 45.00wt% is than the preparation that is the catalyst C3 of 12 modenite, 54.65% aluminium oxide and 0.35% platinum.
Synthetic Si/Al is fully mixed than the modenite and the aluminium-hydroxide powder that are 12,3% aqueous solution of nitric acid for preparing is joined in the mixture of powders mix, then with the mixture extruded moulding.The bar shaped mixture at room temperature left standstill 4 hours, and drying is after 6 hours down at 120 ℃ again, and with the strip pelletizing, length is 3～8 millimeters (wherein 4～6 millimeters particle accounts for more than 80%), makes carrier in 4 hours in 500 ℃ of roastings under air atmosphere.Press zeolite: NH
4Cl=1: 0.26 ratio is prepared the aqueous solution of 3% ammonium chloride, under 90 ℃ of water bath condition made carrier and aqueous ammonium chloride solution is carried out ion-exchange 2 hours then, washs to mother liquor and does not have chlorion.The gained carrier flooded 12 hours at normal temperatures with chloroplatinic acid in the presence of competitive adsorbate (trichloroacetic acid).Make wet solid 60 ℃ of diffusions 1 hour then, 140 ℃ of dryings 2 hours.Catalyst after 2 hours, is used hydrogen reducing 4 hours in 1 hour, 370 ℃ following 2 hours, 500 ℃ following roastings of 200 ℃ of dryings, make the catalyst C3 of platiniferous 0.35% (weight).
Embodiment 4
With the performance of 15 gram evaluating catalyst C1～C3, described aromatic fraction mainly contains alkane and cycloalkane, meta-xylene, ortho-xylene and the ethylbenzene of eight carbon.Estimating under the optimal operation conditions separately:
According to active (concentration PX/ ∑ X and the conversion of ethylbenzene EBc of paraxylene in dimethylbenzene in the product) and selectivity (carbon eight hydrocarbon yield C
8Y) evaluate catalysts performance.
∑X＝PX+MX+OX
C
8＝EB+∑X+C
8 N+P
Table 1 catalyst performance index
Table 1 presentation of results, activity and the selectivity of the activity of catalyst C1 of the present invention, C2 and selectivity ratios catalyst C3 are much higher, compare with C1, and zeolite among the C2 and catalyst have all passed through preliminary treatment, and selectivity has raising.
Claims (7)
1. eutectic zeolite catalyst that contains the EUO structure, it is characterized in that: this catalyst is to be made of the h-type zeolite that contains the EUO structure, adhesive and periodic table of elements group VIII element; The element T that contains silicon and aluminium and/or magnesium in the zeolite, Si/T atomic ratio 8～100;
The h-type zeolite content that contains the EUO structure is 1～90wt%;
The load capacity of group VIII metal is 0.01～2.0wt%;
Its surplus is an adhesive; Gross weight is 100%.
2. according to the described eutectic zeolite catalyst that contains the EUO structure of claim 1, it is characterized in that: the zeolite that wherein contains the EUO structure is EU-1/MOR eutectic zeolite, EU-1/ZSM-50 eutectic zeolite, EU-1/ZSM-5 eutectic zeolite or EU-1/NES eutectic zeolite.
3. according to the described eutectic zeolite catalyst that contains the EUO structure of claim 2, it is characterized in that: the composite construction that the crystal grain of EU-1/MOR eutectic zeolite has EUO type and MOR type simultaneously, wherein the quality of MOR type structure accounts for 1%～80%.
4. according to the described eutectic zeolite catalyst that contains the EUO structure of claim 1, it is characterized in that: adhesive is one or more the mixture in natural clay, synthesis of clay, magnesia, aluminium oxide, silica, silica-alumina, titanium oxide, boron oxide, zirconia, aluminum phosphate, the titanium phosphate.
5. according to the described eutectic zeolite catalyst that contains the EUO structure of claim 1, it is characterized in that: the group VIII metal is platinum or palladium.
6. according to the described preparation method who contains the eutectic zeolite catalyst of EUO structure of claim 1, it is characterized in that:
(1) at first with the roasting under low oxygen concentration atmosphere of EUO structural zeolite, sintering temperature is 200～600 ℃;
(2) adhesive and zeolite evenly mix, moulding;
(3) then at 200～600 ℃ roasting temperature;
(4) and NH
4The Cl aqueous solution carries out ion-exchange, 60～90 ℃ of temperature, 2～4 hours time;
(5) hydrothermal treatment consists, temperature is at 200～500 ℃; Then in 200～600 ℃ of roastings of temperature;
(6) pretreated carrier is in room temperature～95 ℃, under liquid-solid ratio 1.2～2.0 conditions, flooded 2～24 hours or exchange 2～12 hours with platinum acid chloride solution, palladium chloride solution or platinum ammonium complex ion, after filtration, after the drying, 200～550 ℃ of activation are 2～8 hours under air atmosphere.
7. according to the described purposes that contains the eutectic zeolite catalyst of EUO structure of claim 1, it is characterized in that: the catalyst that is used as isomerization of C-8 aromatics;
300～500 ℃ of temperature, hydrogen dividing potential drop 0.30～1.5MPa, hydrogen to oil volume ratio 600～1500v/v,
Feed weight air speed 0.25～20h
-1
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| CN102416345A (en) * | 2010-09-27 | 2012-04-18 | 中国石油化工股份有限公司 | Mixed crystal material containing EUO zeolite and preparation method thereof |
| CN103803575A (en) * | 2012-11-08 | 2014-05-21 | 中国石油化工股份有限公司 | Synthetic method for EU-1/MOR symbiotic molecular sieve |
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| CN104353487A (en) * | 2014-11-20 | 2015-02-18 | 西安元创化工科技股份有限公司 | C8 aromatics isomerization catalyst and application thereof |
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| CN105080600B (en) * | 2014-05-14 | 2018-06-08 | 中国石油化工股份有限公司 | Application in whole EUO zeolite catalysts and Alleyl aromatics isomerizating |
| CN104353487A (en) * | 2014-11-20 | 2015-02-18 | 西安元创化工科技股份有限公司 | C8 aromatics isomerization catalyst and application thereof |
| CN104353487B (en) * | 2014-11-20 | 2017-08-29 | 西北化工研究院 | A kind of C8 arene isomerization catalysts and its application |
| CN106311320A (en) * | 2015-07-03 | 2017-01-11 | 中国石油天然气股份有限公司 | Catalyst containing EU-1/MOR eutectic zeolite as well as preparation method and application thereof |
| CN106311321A (en) * | 2015-07-03 | 2017-01-11 | 中国石油天然气股份有限公司 | Catalyst containing EU-1/ZSM-5 eutectic zeolite as well as preparation method and application thereof |
| CN106311320B (en) * | 2015-07-03 | 2018-09-04 | 中国石油天然气股份有限公司 | A kind of catalyst and its preparation method and application of the zeolite of eutectic containing EU-1/MOR |
| CN106311321B (en) * | 2015-07-03 | 2019-08-02 | 中国石油天然气股份有限公司 | A kind of catalyst and preparation method and application of the zeolite of eutectic containing EU-1/ZSM-5 |
| CN107297221A (en) * | 2017-07-11 | 2017-10-27 | 太原大成环能化工技术有限公司 | A kind of ethylbenzene dealkylation catalyst and preparation method thereof |
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Application publication date: 20100609 |