Paraffin hydrocarbon dehydrogenation catalyst

FIELD: hydrogenation-dehydrogenation catalysts.

SUBSTANCE: invention concerns catalysts for dehydrogenation of C2-C5-alkanes into corresponding olefin hydrocarbons. Alumina-supported catalyst of invention contains 10-20% chromium oxide, 1-2% alkali metal compound, 0.5-2% zirconium oxide, and 0.03-2% promoter oxide selected from zinc, copper, and iron. Precursor of alumina support is aluminum oxide hydrate of formula Al2O3·nH2O, where n varies from 0.3 to 1.5.

EFFECT: increased mechanical strength and stability in paraffin dehydrogenation process.

9 cl, 1 dwg, 3 tbl, 7 ex

 

The invention relates to methods for preparing catalysts for dehydrogenation of paraffin hydrocarbons, C2-C5alkanes to the corresponding olefinic hydrocarbons.

Olefinic hydrocarbons are the most important products of organic synthesis, used in the synthetic rubber industry for the production of basic monomers butadiene, isoprene, isobutylene, as well as in the production of polymers, high-octane components of motor fuels (MTBE).

Technology dehydrogenation of paraffin hydrocarbons in olefin is based on the use of a reactor with a fixed bed of granular catalyst or reactor fluidized bed microspherical catalyst circulating in the reactor - regenerator. The process is carried out continuously at a temperature of 540-650°C. the Catalysts for these processes must have high mechanical abrasion resistance, high temperature resistance in variable environments and stability.

Effective and affordable are the catalysts for the dehydrogenation of hydrocarbons, which contain oxides of chromium in the amount of 9-17% and aluminum oxide. As promoters use compounds of alkali and alkaline earth metals in an amount up to 5% (isoprene Production / Scholarone.com, Gaselys. - L.: Chemistry, 1973. - s.112-118). In the ides of known harmful chromium compounds there is a problem of strong fastening of chromium in the catalyst, as well as increasing its activity and operational stability. Operational stability depends on the ability of the catalyst to store in variables of the process conditions (temperature 540-650°, oxidising and reducing environment, the mechanical effect) for a long time their catalytic and mechanical properties.

Known solutions to this problem in the preparation of chromium catalysts.

One of them is the complexity of the composition of the catalyst by introducing promoters or modifiers in the catalyst or carrier in the form of aluminum oxide.

A known catalyst which contains chromium oxide in the amount of 25%, the compound of alkaline and/or alkaline earth metal, preferably cesium in the amount of 0.7 to 4.5% and the promoter in the form of zirconium dioxide in the amount of 0.9% for medium - aluminium oxide (Patent USSR No. 1836140, CL. B 01 J 23/26, 1993).

The catalyst has high activity but low mechanical strength and stability.

Known catalyst for dehydrogenation of paraffin hydrocarbons (RF Patent No. 2167709, CL. B 01 J 23/26, 2001), which is obtained by applying chromium compounds in amounts of 10-25%, potassium compounds in the amount of 0.5-2% on the media in the form of aluminum oxide modified with compounds of zirconium (0,5-2%), boron (0,5-2%) and silicon (0.5 to 1.5%).

This catalyst has insufficient is th selectivity and stability, and low mechanical strength.

To solve the problem of improving the efficiency of used catalysts, which as the carrier contain aluminium spinel, which is applied to compounds of chromium, tin and platinum.

Known catalyst containing chromium oxide 10-30%, and optionally, tin oxide in an amount of 0.1-3% on a carrier of aluminum oxide and zinc oxide in the amount of 30-45% (RF Patent No. 2177827, CL. B 01 J 23/26, 2002).

Known catalyst containing chromium oxide 10-30%, tin oxide in an amount of 0.1-3% and additionally platinum in the amount of 0.005-2% on the media, aluminum oxide and zinc oxide (Patent RF №2183988, CL. B 01 J 23/26, 2002).

These catalysts, in spite of the complex composition and multi-stage method of production, do not reach a stable activity and selectivity. Bad to consolidate the strength of the active components in the medium leads to their entrainment in the process of operation and the reduction of the initial activity of the catalysts. Low and the mechanical strength of such catalysts.

Known catalyst for dehydrogenation of paraffin hydrocarbons (RF Patent No. 2148430, CL. B 01 J 23/26, 2000), which contains the oxides of chromium 12-23%, the compound of alkaline and/or alkaline earth metal in the amount of 0.5-3.5% and the connection of non-metal: boron and/or silicon in an amount of 0.1-10%. The catalyst contains also the least one connection of the modifying metal (Ti, Zr, Sn, Fe, Ga, Co, Mn, Mo) in an amount of 0.5 to 1.5%. The catalyst formed by heat treatment of aluminum compounds of the formula Al2About3·nH2O, where n=0,3-1,5, x-ray amorphous structure together with other compounds.

The catalyst has high activity and selectivity, but the lack of operational stability. The chemical composition is complex, which creates certain difficulties when playing its properties during preparation.

The closest technical solution is the catalyst contains chromium oxide in the amount of 12-23%, the compound of alkaline and/or alkaline earth metal in an amount of 0.5-3.5%, zirconium dioxide in an amount of 0.1-5% and at least one oxide promoter from the group of niobium, tantalum, hafnium in an amount of 0.001-2% aluminum oxide (Patent RF №2200143, CL. 07 With 5/333, 2003). The catalyst formed during the heat treatment of aluminum compounds of the formula Al2O3·nH2O. Where n=0,3-1,5, x-ray amorphous structure together with the compounds of the above elements.

The disadvantage of this catalyst is that it has no practical application because of the scarcity and high cost of the used compounds of hafnium, niobium, tantalum. In addition, this catalyst does not solve problemsability.

The objective of the invention is to develop a catalyst for dehydrogenation of paraffin hydrocarbons having high mechanical strength, catalytic activity and stability.

The problem is solved by using a catalyst for dehydrogenation of paraffin hydrocarbons containing chromium oxide compound of alkali metal, Zirconia, promoter and aluminum oxide, the precursor medium - compound of aluminium of the formula Al2O3·nH2Oh, where n=0,3-1,5, ingenuitea patterns. The catalyst contains as a promoter, at least one compound of a metal selected from the group of zinc, copper, iron in an amount of 0.03-2.0 wt.% and the catalyst has the following composition, wt.% (in terms of oxide):

The chromium oxide10-20
Connection alkaline metal1-2
Zirconium oxide0,5-2
The oxide promoter group:
zinc, copper, iron0,03-2
Aluminium oxiderest

The catalyst preferably formed during the heat treatment of the carrier - aluminum compounds of the formula Al2About3·nH2Oh, where n=,3-1,5, x-ray amorphous structure, together with compounds of chromium, zirconium, alkali metal promoter from the group of zinc, copper, iron.

The carrier - connection of aluminium of the formula Al2About3·nH2Oh, where n=0.5 to 1.0, x-ray amorphous structure, preferably represents a spheroid particles consisting of hexagonal rods with the system planar, parallel pores, corresponding to the splitting faces (001), with a specific surface area 80-250 m2/g, pore volume of 0.1-0.3 cm3/g and the size of 20-250 μm.

The catalyst has a value of specific surface area preferably 80-200 m2/year

The catalyst contains an oxide of chromium (VI) is preferably not less than 0.13 wt.% before regeneration.

The catalyst contains an oxide of chromium (VI), preferably in a quantity of 0.8 to 1.2 wt.% after regeneration.

The catalyst is preferably a microspherical powder with a particle size of 70-250 μm.

The catalyst is preferably a microspherical powder with a particle size of 20 to 250 μm.

The catalyst may be present in the form of granules with a diameter of 3-5 mm

The difference between the claimed catalyst from the prototype is that the composition of the catalyst as a promoter enter at least one compound of a metal from the group of zinc, copper, iron.

The use of the proposed promoters together the other components of the catalyst and aluminum compounds of the formula Al 2O3·nH2O, where n=0,3-1,5, x-ray amorphous structure obtained fast partial dehydration of hydrargillite, allowed to obtain a catalyst having high activity, strength, stability.

Under the connection Al2O3·nH2Oh, where n=0,3-1,5, x-ray amorphous structure is understood in this connection, x-ray analysis does not detect any lines, characteristic of any crystalline phase. This compound has high reactivity, which becomes possible intercalate compounds of the catalyst components in the interlayer space between alyumogidroksidnykh packages.

The carrier - connection of aluminium of the formula Al2O3·nH2Oh, where n=0.5 to 1.0, x-ray amorphous structure may contain as impurities compounds of silicon, iron, sodium amount, wt.% (in terms of oxides):

silicon oxide- not more than 0,03
iron oxide- not more than 0.05
sodium oxide- not more than 0.3

These impurities do not adversely affect the properties of the media.

We have found that the heat treatment of the carrier - aluminum compounds of the formula Al2O3·nH2the, where n=0,3-1,5, x-ray amorphous structure, together with compounds of chromium, zirconium, alkali metal and promoter from the group of zinc or copper, or iron, a catalyst which has high activity, high strength, and high stability in the operating mode of action of the catalyst at dehydrogenation.

This high stability of the catalyst in the process of dehydrogenation of paraffin hydrocarbons (reduction - oxidation) can be explained by the formation of active centers in the form of solid solutions of chromium and chromite zinc or copper, or iron, in which the oxide of chromium (VI), then Cr6+is in the active form.

When the heat treatment leads to the formation of highly dispersed x-ray amorphous solid solutions of chromium and chromite zinc, copper, iron, strongly related to the structure of the formed aluminum oxide. The catalyst after heat treatment has a specific surface area of 80-200 m2/g, high mechanical strength.

Stabilization of chromium compounds in solid solutions with zinc, copper and iron prevents the formation of solid solutions of chromium with aluminum, which increases the activity and stability of the catalyst, increasing its service life.

To obtain highly active and stable catalyst with high mechanical strength, nope this low erosive effects on the equipment it is proposed to use preferably the carrier is a compound of aluminium of the formula Al2O3·nH2Oh, where n=0.5 to 1.0, x-ray amorphous structure consisting of spheroidal particles with a size of 20 to 250 μm. The particles consist of hexagonal rods with the system planar, parallel pores, corresponding to cleavage at the faces (001) with a specific surface area 80-250 m2/g and a pore volume of 0.1 - specific surface 80-250 m2/g and a pore volume of 0.1-0.3 cm3/, figure 1 shows the carrier: (a) diagram of the hexagonal core particles of the carrier by splitting the faces (001) in pores; b) hexagonal core particles of the carrier by splitting the faces (001) parallel pores.

In the process of getting the media by dehydration hydrargillite system is formed flat and parallel pores about the face (001) in the hexagonal structure of rods hydrargillite (see drawing). Character (001) is the designation of the faces with the largest number of positive indices (fundamentals of Mineralogy and crystallography / Vppndrv. - M.: Higher school, 1978. - p.59).

It is known that the dehydrogenation catalysts containing chromium oxide in the form of a mixture of oxides of Cr3+and Cr6+(Production of isoprene / Scholarone.com, Gaselys. - L.: Chemistry, 1973. - s.112-118). The content of Cr6+in the proposed catalyst does not exceed 4 wt.%.

In desktop mode the action of the known catalysts for the dehydrogenation is reduced Cr 6+below 0.1%, while the catalyst is deactivated. In the proposed catalyst for reducing the content of Cr6+below 0,13% not observed, and the catalyst for a long time does not lose activity.

During regeneration of the catalyst is burning coke and oxidation of Cr3+to Cr6+. The content of Cr6+from the minimum content of 0.13% before regeneration is increased to 0,8-1,2% after regeneration in contrast to the known catalysts. This ensures stable operation of the catalyst in the dehydrogenation reaction.

The proposed catalyst in contrast to the known has the property to stabilize the content of Cr6+in the operating mode of action of the catalyst to the amount at which the catalyst retains its activity. Thus, the proposed catalyst is a stabilizer Cr6+in the process of dehydrogenation of paraffin hydrocarbons.

We have also found that the addition of the proposed catalyst for use in the industry quickly detectiveromance chromium catalysts increases their lifespan due to the stabilization of Cr6+.

The particle size of the catalyst is determined by the process conditions. For fluidized bed use a catalyst with a particle size of 70-250 μm. The particle size of the catalyst, which is used as an additive to know who Tim chromium catalysts for the stabilization of chromium, is 20-250 μm. The catalyst for stationary layer can be prepared in the form of granules with a diameter of 3-5 mm

Thus, the proposed set of features has led to a new technical result is to obtain a highly active, stable in variable process conditions of the dehydrogenation catalyst having a high mechanical strength.

Determination of the phase composition of the materials used in the technology of preparation of the catalyst dehydrogenation, conduct radiographic technique based on x-ray diffraction. Survey samples is carried out in Cu-K-α-radiation using a differential discrimination of the monochromator. The interval of angles on a scale of 2θ from 10 to 75°, the angular velocity detector 1/60°.

Specific surface area determined by BET method, the volume of pore - water adsorption, particle size - sieve method.

The abrasion resistance is determined by the mass fraction of the loss in catalyst attrition. The method is based on the destruction of the catalyst particles in the fluidized layer and measuring the mass of particles carried by the air flow rate is stable.

The crushing strength is determined by the force on the destruction of the granules between two planes.

The outer shape of the catalyst particles was determined using a scanning microscope.

The following examples illustrate the proposed solution.

Example 1

Media microspherical AOK-1 connection of aluminium of the formula Al2O3·nH2Oh, where n=0,5, ingenuitea structure, with properties presented in table 1, are loaded into propitiating. There also fill in an impregnating solution containing the catalytic components in the quantities necessary for preparation of the catalyst composition, wt.% (in terms of oxides):

the chromium oxide- 10,
including chromium oxide (Cr6+)to 3.8
oxide potassium- 2,0
zirconium oxide- 2,0
zinc oxide- 2,0
aluminium oxide- the rest.

The catalyst after drying, calcined at 700°C. the Catalyst has the composition shown in table No. 2, and operational characteristics are presented in table No. 3.

Examples 2-5

The catalysts are prepared analogously to example 1. Different applied by the media, the composition of the active components and the resulting properties. Data carriers are presented in table 1, the composition of the catalyst (table 2, performance characteristics, in table No. 3.

Example 6

The catalyst is similar to the use of the 1, different properties of the media. The composition of the catalyst (table No. 1, 2). After calcination of the microspherical catalyst with a particle size of 20 to 250 μm preparing a mixture capable of forming. The mixture is formed into pellets with a diameter of 3-5 mm and calcined at a temperature of 750°C. Receive the catalyst with the properties presented in table 3. Strength is determined by the crushing of the granules by forming in MPa.

Example 7 (prototype)

Media microspherical AOK-4 - connection of aluminium of the formula Al2O3·nH2Oh, where n=1.5, x-ray amorphous structure, with properties presented in table 1, are loaded into the mixer, there is poured a solution containing compounds of chromium, potassium, zirconium, niobium in amounts necessary to obtain a catalyst composition, % wt. (in terms of oxides):

the chromium oxide- 16,
including chromium oxide (Cr6+)- 2,9
the potassium oxide + lithium oxide- 2,1
zirconium oxide- a 0.1
the oxide of niobium- 2,0
aluminium oxide- the rest.

Obtained after drying and calcination at 750°the catalyst has the composition shown in table No. 2, and properties, represented the military in table No. 3.

As seen from the examples, the catalyst of the proposed structure has high mechanical strength, stability in the operating mode of action of the catalyst in the dehydrogenation of paraffin hydrocarbons.

Table No. 1.
Properties media - aluminum compounds of the formula Al2O3·nH2About x-ray amorphous structure
Media

AOK-1AOK-2AOK-3AOK-4AOK-5
1. The value "n" in the formula Al2O3·nH2About0,51,00,71,50,3
2. The shape of the particlesSpheroidal particles consisting of hexagonal rods with the size of the sides of the hexagon 1-10 μm with a system of flat parallel pores, corresponding to the splitting faces (001)Similarly, the KLA-1Similarly, the KLA-1Spheroidal solid particlesSimilarly, the KLA-4
3. Particle size, microns70-25020-25070-25040-20070-250
4. Specific surface area, m2/g14580 250145200
5. Pore volume, cm3/g0,180,10,30,130.25
6. The degree of rehydration to pseudoboehmite, %4535413330

14
Table No. 2.
The composition of the catalysts for the dehydrogenation of paraffin hydrocarbons
Example1234567 prototype
1. The carrier-connection of aluminium of the formula Al2O3·nH2About x-ray amorphous structure of tables No. 1AOK-1AOK-2AOK-3AOK-4AOK-5AOK-1AOK-4
2. Composition, wt.%:
oxide of chromium, including:101620152016
oxide chromium (VI)the 3.83,44,03,53,03,02,9
the connection of an alkali metal (K2O)21,511,521 (Na2O)2 (K2O)0,1 (Li2O)
- zirconium oxide210,51,5110,1
oxide promoter group:
zinc2-0,07-1,8--
copper--0,031---
iron-0,03--0,20,03-
the oxide of niobium------2
- aluminium oxiderestOST the aspects restrestrestrestrest

Table No. 3.
The properties of the catalysts for the dehydrogenation of paraffin hydrocarbons
Example

1234567 prototype
1. The particle size of the catalyst:
- microspheric, mcm70-25020-25070-25040-20070-25040-200
- granulated, mm3-5
2. Specific surface area, m2/g138802001109010085
3. Operational properties of the catalyst dehydrogenation:
activity, EAP, %54535652536052
- selectivity, BP90919489909488,7
- mechanical strength (weight loss during abrasion), wt.%1,53,22,04,0the 3.84,6
mechanical crushing strength, MPa12
4. The content of the oxide of chromium (VI) in the operating mode of action of the catalyst, wt.%:
before regeneration0,200,150,30,130,140,250,08
after regeneration1,00,881,20,80,850,90,5

1. Catalyst for dehydrogenation of paraffin hydrocarbons, vkljuchajuwih the oxide of chromium, the connection of an alkali metal, zirconium dioxide, the promoter and the aluminum oxide, the precursor medium - compound of aluminium of the formula Al2O3·nH2Oh, where n=0,3-1,5, x-ray amorphous structure, characterized in that it contains as a promoter, at least one compound of a metal selected from the group of zinc, copper, iron, in the amount of 0.03-2.0 wt.% and the catalyst has the following composition, wt.% in terms of the oxide:

The chromium oxide10-20
Connection alkaline metal1-2
Zirconium oxide0,5-2
The oxide promoter group:
zinc, copper, iron0,03-2
Aluminium oxideRest

2. The catalyst according to claim 1, characterized in that it is formed during the heat treatment of the carrier - aluminum compounds of the formula Al2About3·nH2O, where n=0,3-1,5, x-ray amorphous structure together with compounds of chromium, zirconium, alkali metal promoter from the group of zinc, copper, iron.

3. The catalyst according to claim 1, characterized in that the carrier - connection of aluminium of the formula Al2About3·nH2Oh, where n=0.5 to 1.0, x-ray amorphous structure represents the way the th spheroid particles, consisting of hexagonal rods with the system planar, parallel pores, corresponding to the splitting faces (001), with a specific surface area 80-250 m2/g, pore volume of 0.1-0.3 cm3/g and the size of 20-250 μm.

4. The catalyst according to claim 1, characterized in that it has a value of specific surface area of 80-200 m2/year

5. The catalyst according to claim 1, characterized in that it contains chromium oxide (VI) not less than 0.13 wt.% before regeneration.

6. The catalyst according to claim 1, characterized in that it contains an oxide of chromium (VI) in an amount of 0.8-1.2 wt.% after regeneration.

7. The catalyst according to claim 1, characterized in that it is a microspherical powder with a particle size of 70-250 μm.

8. The catalyst according to claim 1, characterized in that it is a microspherical powder with a particle size of 20 to 250 μm.

9. The catalyst according to claim 1, characterized in that it is a pellet with a diameter of 3-5 mm



 

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