CN1895766A - Catalytic selective hydrogenation - Google Patents
Catalytic selective hydrogenation Download PDFInfo
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- CN1895766A CN1895766A CN 200510083850 CN200510083850A CN1895766A CN 1895766 A CN1895766 A CN 1895766A CN 200510083850 CN200510083850 CN 200510083850 CN 200510083850 A CN200510083850 A CN 200510083850A CN 1895766 A CN1895766 A CN 1895766A
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Abstract
A selective catalytic hydrogenation process able the control the hydroselectivity includes such steps as fixing the selective hydrocatalyst to the rotator of a super-gravitational rotary-bed reactor, rotating to form a rotating catalyst bed, and making the hydrocarbon material and H2 pass through the rotating catalyst bed in parallel mode or opposite mode. Controlling the rotation speed and radial thickness of rotator can control the hydroselectivity.
Description
Technical field
The present invention relates to a kind of method of catalytic reaction, specifically, relate to and utilize rotating packed bed reactor to carry out the method for catalytic selectivity hydrogenation.
Background technology
The hydro carbons selective hydrogenation reaction generally carries out in fixed bed reactors at present, connects with one or several reactors and realizes.Material and hydrogen are so that also stream or reflux type are realized selectable hydrogenation reaction by the fixed beds layer according to the different rate of adsorption of each component of material.The fixed bed hydrogenation reaction process has advantages such as simple in structure, that back-mixing is little; Shortcomings such as but the fixed bed reactors hydrogenation also exists, and heat transfer is poor, residence time of material is long.For example: when in fixed bed reactors, carrying out exothermic reaction, because heat transfer property is poor, when the exothermic heat of reaction amount is big, even adopt shell and tube reactor also may produce the temperature runaway phenomenon.Material passes through beds with drip or immersion way in the fixed-bed process, material and catalyst are long time of contact, side reaction and excessive hydrogenation easily take place, cause that the purpose product selectivity is poor, diene polymerization covers catalyst surface, thereby reduced catalytic active center, influenced life of catalyst.
Rotating packed bed reactor is proposed by Britain Imperial Chemical Industries (ICI) the earliest.The EP0023745A3 proposition is high-gravity rotating bed can be used for processes such as absorption, desorb, distillation, but laboratory data is only arranged, and discloses the application technology of industrially scalable.Chinese patent CN1064338A, CN1116146A, CN1116185A are successfully with the hypergravity field swinging bed preparation process that is applied to plant-scale oil-field flooding deoxidation process and calcium carbonate superfine powder.Chinese patent CN1507940A proposes to carry out catalytic reaction in super gravity field, and discloses the method for carrying out the full hydrogenation of hydro carbons in the super gravity field reactor.
Summary of the invention
The method that the purpose of this invention is to provide a kind of catalysis selective hydrogenation specifically, just provides a kind of method of carrying out the catalytic selectivity hydrogenation in rotating bed super gravity field.Method of the present invention is to carry out hydrogenation reaction in the mode that is different from fixed bed reactors fully, is a kind of method of new catalysis selective hydrogenation.
Method of the present invention, be that the deimpurity selective hydrogenation reaction of hydrocarbon material is carried out in rotating bed super gravity field, selective hydrocatalyst is fixed on the rotor of rotating packed bed reactor, the catalytic bed that formation is being rotated, material and hydrogen with and stream or the mode of adverse current by the catalytic bed of rotation at a high speed.
Method of the present invention is regulated the time of staying of hydrocarbon material in catalytic bed by rotor speed and the rotor radial thickness of regulating rotating packed bed reactor, controls the degree of depth of hydrogenation, thereby improves the selectivity of selective hydrogenation reaction.
Preferably regulate hydrocarbon material in the time of staying of catalytic bed according to formula (1) and formula (2),
u
l＝0.021L
0.25(ω
2R)
0.61 (2)
Wherein, τ represents the time of staying of hydrocarbon material in hypergravity field swinging bed reactor catalysis bed, s;
R
2, R
1External diameter and the internal diameter of representing hypergravity field swinging bed reactor rotor, m;
u
lThe expression hydrocarbon material is by the flow velocity of catalytic bed, m/s;
L represents the flow of hydrocarbon material, m
3/ h;
ω represents hypergravity field swinging bed reactor rotor speed, l/s;
R represents catalytic bed geometrical mean radius, m.
Described catalyst is put into and is supported internals, is fixed on the rotor of rotating packed bed reactor, and described support internals are selected from mesh-supported internals, ring-type and support a kind of in internals and the annular porous material.Wherein, when described support internals are annular porous material, described activity of such catalysts component directly can be coated in porous material surface,, make foamed aluminium, after surface treatment, Al as can aluminium being base material
2O
3Adhere to from the teeth outwards, will select on the active constituent such as the surface of Pd of hydrogenation with infusion process then attached to porous material.
Described hydrocarbon material comprises at least a monoolefine and impurity, and wherein said impurity is alkynes compounds, alkadiene compound or their mixture.
Comprise the compound that contains two keys at least in the described hydrocarbon material, wherein said impurity is alkynes.
Comprise the compound that contains two keys at least in the described hydrocarbon material, wherein said impurity is alkynes class and a kind of compound that contains adjacent double bonds.
Described hydrocarbon material comprises a kind of pair of key by the separated compound of at least one singly-bound, and wherein said impurity is alkynes.
The process conditions that described hydrocarbon material carries out selective hydrogenation reaction are: the rotating speed of hypergravity field swinging bed reactor is 100-10000rpm; Reaction temperature is 20-200 ℃; Reaction pressure is normal pressure-4.0MPa; Gas space velocity is 2000-10000h
-1The liquid air speed is 5-200h
-1
The described hypergravity field swinging bed reactor of method of the present invention can use existing hypergravity device in the prior art, preferably uses the present invention's rotating packed bed reactor shown in the drawings.
The detailed process of method of the present invention is as follows:
Select hydrogenation catalyst to be installed in the revolving bed rotor that is rotating at a high speed, hydrocarbon material enters from the import of rotating packed bed reactor liquid phase after metering, evenly is sprayed at by liquid distribution trough on the beds of rotation at a high speed.Hydrogen through metering is entered by the import of rotating packed bed reactor gas phase, with hydrocarbon material in beds with adverse current or and the abundant haptoreaction of mode of stream after, remaining hydrogen is discharged by gaseous phase outlet, hydrocarbon material is discharged by liquid phase outlet.Under air speed one stable condition, can control the time of staying of material by the rotating speed of regulating rotor; Can control the degree of depth of hydrogenation by the radial thickness that changes catalyst filling in the rotor; Can control hydrogen/hydrocarbon by the feed rate that changes hydrocarbon material and hydrogen.
In the method for the present invention, the control of material time of staying in catalytic bed can realize in the following manner.As the formula (1), the time of staying of hydrocarbon material in catalytic bed and the radial thickness R of catalytic bed
2-R
1And material is relevant by the flow velocity of catalytic bed, and the catalytic bed radial thickness is more little, and material is fast more by the flow velocity of catalytic bed, and the time of staying is short more.
The flow of the flow velocity of material by catalytic bed and material and the rotating speed of hypergravity field swinging bed reactor rotor are relevant, as the formula (2), the flow velocity of hydrocarbon material is directly proportional with the flow of hydrocarbon material and rotor speed, mass flow and rotor speed are big more, and material is fast more by the flow velocity of catalytic bed.Under the constant prerequisite of mass flow, regulating material is the rotating speed that changes hypergravity field swinging bed reactor rotor in the most effective means of beds flow velocity.From formula (1) and formula (2) as can be known, regulating material means of the time of staying in beds has two, and the one, the radial thickness (R of catalytic bed
2-R
1), the 2nd, the rotational speed omega of hypergravity field swinging bed reactor rotor.Under the situation that equipment has been finalized the design in actual production, regulating material the most effective means of the time of staying in beds is exactly the rotating speed that changes hypergravity field swinging bed reactor rotor.Mainly be to change the time of staying of hydrocarbon material in catalytic bed among the present invention,, realize the purpose of selective hydrogenation so that reach the control hydrogenation degree of depth by the rotating speed of regulating hypergravity field swinging bed reactor rotor.
The present invention utilizes hypergravity field swinging bed reactor to carry out catalysis selective hydrogenation reaction, it is the relative compound with a triple bond of compound with two keys that the hydrogenation target is specifically related to mixture, the relative compound of compound with two two keys with a triple bond, has the relative compound that wherein contains the two keys of iterate of compound that the relative compound with a triple bond of the compound of any two keys and two key are separated by one or more singly-bounds, method by hydrogenation strongly becomes two keys with three, or the two keys of iterate are become two keys, to remove these impurity.Selective hydrogenation reaction comprises: C
2Selection hydrogenation in the material removes acetylene; C
3Selection hydrogenation in the material removes propine and allene; C
4Selection hydrogenation in the material removes 1,2-butadiene and 1,3-butadiene; C
4Selection hydrogenation in the material removes ethyl acetylene and vinylacetylene, C
5And C
6Selection acetylene hydrogenation hydrocarbon in the material and alkadienes, 1, the selection in the 4-butanediol preparation process removes butynediols hydrogenation or the like.
In petrochemical industry, all contain one or more alkynes classes or dienes compound in the hydrocarbon raw material of producing as steam cracking, catalytic cracking.Acetylene compound comprises acetylene, propine, ethyl acetylene, vinylacetylene and diacetylene etc.; The dienes compound comprises allene, 1,2-butadiene, 1,3-butadiene or the like.Acetylene compound and dienes compound influence the stability of the further process catalyst system therefor of alkene as the impurity of olefin feedstock, and industrial common employing fixed bed reactors are selected this class impurity of hydrogenation and removing.
Because hypergravity field swinging bed reactor has following three features:
The one, there is not back-mixing fully.Hydrocarbon material that is to say under the powerful action of centrifugal force at hypergravity, moment the catalytic bed by rotating at a high speed, material mobile in catalytic bed approaches desirable laminar flow, material has the time of staying much at one.By the radial thickness that rotating speed, feed rate, the catalyst of regulating rotor loads, can control and select the hydrogenation degree of depth, suppress the generation of side reaction, thereby effectively improve the selectivity of target product.Hypergravity field swinging bed reactor does not have the characteristics of back-mixing, make its have other form reactors such as fixed bed, fluid bed, tubular reactor incomparable advantage.
The 2nd, strengthen mass transfer.Hydrocarbon material is sprayed on the catalytic bed of rotation at a high speed by liquid distribution trough, mass transport process between hydrocarbon material and the hydrogen, between hydrocarbon material, hydrogen and the catalyst, between hydrogenation products and the catalyst is reinforced under the effect of hypergravity, effectively reduced or eliminated the influence of diffusion process to hydrogenation reaction, make the hydrogenation products reaction environment that speeded away, impel reactant to accelerate to move to the product direction, thereby shorten the reaction time, make the disposal ability of per volume of catalyst in the unit interval improve tens times and even hundreds of times.In addition, owing to strengthened the mass transport process of gas-liquid phase, hydrogen is easier to be dissolved in the hydrocarbon material, so reaction pressure also can obviously reduce.Under the identical prerequisite of disposal ability, can significantly reduce catalyst consumption, reduce equipment volume greatly, investment cost and energy consumption also reduce thereupon greatly.This also is that traditional hydrogenation mode is incomparable.
The 3rd, heat-transfer effect is good.The hydro carbons selective hydrogenation reaction is generally exothermic reaction.In exothermal reaction process, it is vital in time getting rid of reaction heat.When carrying out exothermic reaction in traditional fixed bed reactors, if heat can not in time be taken out of, the lighter's reaction temperature is out of control, and " temperature runaway " phenomenon then takes place weight person.And in hypergravity field swinging bed reactor, because hydrocarbon material passes through catalytic bed rapidly under the effect of hypergravity, and from liquid phase outlet eliminating, exothermic heat of reaction does not also make catalytic bed significantly heat up and is taken out of conversion zone rapidly, therefore reaction temperature steadily, be easy to control, be applicable to the hydrogenation reaction that thermal discharge is big.In addition, when in traditional fixed bed reactors, carrying out selective hydrogenation reaction, consider exothermic heat of reaction, the concentration that needs impurity such as limited reactions inlet alkynes, must dilute hydrogenating materials with the partial hydrogenation product, reach the purpose that reduces impurity content in the raw material, therefore handle the limited ability system of fresh material.And in hypergravity field swinging bed reactor hydrogenation process,, therefore needn't consider the trouble that exothermic heat of reaction is brought because exothermic heat of reaction is taken out of conversion zone rapidly by reaction mass, select the disposal ability of hydrogenation also to improve greatly thus.This also is that tradition selects the hydrogenation mode not available.
Therefore, the present invention utilizes hypergravity field swinging bed reactor to carry out the method that catalysis selective hydrogenation removes impurity in the hydrocarbon material, is a kind of new method that tradition is selected hydrogenation technique that is different from fully.
Method of the present invention has that equipment volume is little, investment cost is low, disposal ability is big, the advantage of purpose selectivity of product height, mass transfer, good heat-transfer.This method has changed the way of contact of hydrocarbon material and catalyst, hydrocarbon material is sprayed on the catalytic bed that is in the hypergravity rotation by liquid distribution trough, material moment is passed through catalytic bed, material and catalyst are short time of contact, and do not have air-teturning mixed phenomenon fully, and suppress the generation of hydrogenation side reaction, avoid diene polymerization, purpose selectivity of product height, catalyst life is long.
Description of drawings
Fig. 1 is the schematic diagram of the used rotating packed bed reactor of method of the present invention.
This reactor comprises: can high speed rotor rotated 2, rotary-catalytic bed 7, liquid phase import 6 and export 5, gas phase import 1 and export 4 and liquid distribution trough 3 etc.
Below, the flow process of the method for accompanying drawings catalysis selective hydrogenation of the present invention:
As shown in Figure 1, hydrogen tangentially enters hypergravity field swinging bed reactor by gas phase import 1, the rotor that is fixed with catalytic bed 2 that under action of pressure, passes at a high speed rotation with by hydrocarbon material (liquid phase or the gas phase) adverse current of liquid distribution trough 3 ejections of hypergravity field swinging bed reactor center/and flow and contact, gas-liquid (or gas gas) two-phase is mixed in the catalytic bed of rotation at a high speed strongly, mass transfer and reaction are carried out in turbulence, reacted remaining hydrogen is drawn by the gaseous phase outlet 4 of hypergravity field swinging bed reactor, reacted liquid phase throws away through liquid phase outlet 5, and gas-liquid two-phase enters after-treatment system separately or does him and use.
The specific embodiment
Utilizing hypergravity field swinging bed reactor to carry out catalysis selective hydrogenation reaction, can be the gas phase selective hydrogenation reaction, as removes C
2Acetylene impurity in the material; Can be selective hydrogenation reaction in liquid phase also, as remove C
4Ethyl acetylene, vinylacetylene and 1,3-butadiene in the material; Reaction mass can all be fresh hydro carbons, also can the fresh hydro carbons of part and the mixed material of part circulation products, and recycle ratio can be adjusted arbitrarily according to reaction needed; Hydrocarbon material and hydrogen can adverse current mode carry out selective hydrogenation reaction by catalytic bed, also can and the mode of stream carry out hydrogenation reaction by catalytic bed, hydrogen/hydrocarbon can be adjusted arbitrarily according to reaction needed.
Method of the present invention is not defined as any concrete selective hydrogenation reaction, but below the selection method of hydrotreating put up with alkynes at least a hydrocarbon material and diene impurity the present invention is described specifically.But, can not limit scope of the present invention with this.Scope of the present invention is as the criterion with the content of determining in claims.
Embodiment 1
Utilize hypergravity field swinging bed reactor to carry out C
2Cut removes the selective hydrogenation reaction of acetylene impurity.C
2Acetylene content is 1.0% in the cut, with commercially available C
2Select hydrogenation catalyst (BC-H-21B) to put into mesh-supported internals (catalyst being divided into the little lattice of 15 centimetres of about 15 cm x, 15 cm x at rotor with 40 purpose stainless steel cloths), be fixed on the rotor of hypergravity field swinging bed reactor.C2 cut and hydrogen pass through catalytic bed in the mode that also flows.
The process conditions of carrying out selective hydrogenation reaction are as follows:
Gas space velocity: 10000h
-1, reaction temperature: 70 ℃, reaction pressure: 2.0MPa
Hydrogen/alkynes: 1.1mol/mol,
Rotor speed: 1250-1500rpm, catalytic bed radial thickness: 135mm
Select the hydrogenation result:
Remain acetylene content: 1000ppm in the hydrogenation products, ethylene selectivity: 95%
Embodiment 2
Utilize hypergravity field swinging bed reactor to carry out C
4Raffinate removes the selective hydrogenation reaction of butadiene.C
4Raffinate carbon containing four alkane: 10-20%, carbon four monoolefines: 80-90%; Carbon four diolefin 0.5-2%.C
4Select hydrogenation catalyst (to contain 0.2%Pd/Al
2O
3) according to the preparation of CN1321544A disclosed method, catalyst is put into ring-type support internals, be fixed on the rotor of hypergravity field swinging bed reactor.It is to make two annulus with 4 millimeters corrosion resistant plate that described ring-type supports internals, stainless steel column with 6 millimeters between two annulus supports, the circular support internals that form, wherein cylindrical is with 10,8 of interior circles, seal with stainless steel cloth in the slit that forms between the stainless steel pillar of inside and outside circle, makes a call to the aperture of 25 millimeters of 4 diameters on the corrosion resistant plate of last circle, is used for loading catalyst.C4 raffinate and hydrogen pass through catalytic bed in the mode of adverse current.
Select the hydrogenation technique condition:
Liquid air speed: 40h
-1, reaction temperature: 30 ℃, reaction pressure: 1.2MPa
Hydrogen/alkadienes: 1.10mol/mol
Rotor speed: 1850-2000rpm, the radial thickness of the catalyst layer that is rotating: 150mm
Select the hydrogenation result:
Remain butadiene content:＜10ppm in the hydrogenation products, butylene selectivity: 95%.
Claims (8)
1. the method for a catalysis selective hydrogenation, it is characterized in that, to select hydrogenation catalyst to be fixed on the rotor of rotating packed bed reactor, the catalytic bed that formation is being rotated, hydrocarbon material and hydrogen with adverse current or and stream the catalytic bed of mode by rotating, the deimpurity selective hydrogenation reaction of hydrocarbon material is carried out in super gravity field.
2. method according to claim 1 is characterized in that, regulates the time of staying of hydrocarbon material in catalytic bed by rotating speed and the rotor radial thickness of regulating the rotating packed bed reactor rotor.
3. method according to claim 2 is characterized in that, regulates hydrocarbon material in the time of staying of catalytic bed according to formula (1) and formula (2),
u
l＝0.021L
0.25(ω
2R)
0.61 (2)
Wherein, τ represents the time of staying of hydrocarbon material in hypergravity field swinging bed reactor catalysis bed, s;
R
2, R
1External diameter and the internal diameter of representing hypergravity field swinging bed reactor rotor, m;
u
lThe expression hydrocarbon material is by the flow velocity of catalytic bed, m/s;
L represents the flow of hydrocarbon material, m
3/ h;
ω represents hypergravity field swinging bed reactor rotor speed, 1/s;
R represents catalytic bed geometrical mean radius, m.
4. method according to claim 1, it is characterized in that described catalyst is put into supports internals, be fixed on the rotor of rotating packed bed reactor, described support internals are selected from mesh-supported internals, ring-type and support a kind of in internals and the annular porous material.
5. method according to claim 1 is characterized in that described hydrocarbon material comprises at least a monoolefine and impurity, and wherein said impurity is alkynes compounds, alkadiene compound or their mixture.
6. method according to claim 1 is characterized in that described hydrocarbon material comprises the compound that contains two keys at least, and wherein said impurity is alkynes.
7. method according to claim 1 is characterized in that comprising in the described hydrocarbon material compound that contains two keys at least, and wherein said impurity is alkynes class and a kind of compound that contains adjacent double bonds.
8. method according to claim 1 is characterized in that described hydrocarbon material comprises a kind of pair of key by the separated compound of at least one singly-bound, and wherein said impurity is alkynes.
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