CN105879792B - It is a kind of using prepared in slurry bed reactor for the reaction system and method for ethylene - Google Patents
It is a kind of using prepared in slurry bed reactor for the reaction system and method for ethylene Download PDFInfo
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- CN105879792B CN105879792B CN201610424136.4A CN201610424136A CN105879792B CN 105879792 B CN105879792 B CN 105879792B CN 201610424136 A CN201610424136 A CN 201610424136A CN 105879792 B CN105879792 B CN 105879792B
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- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000005977 Ethylene Substances 0.000 title claims abstract description 45
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000002002 slurry Substances 0.000 title claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 79
- 239000002904 solvent Substances 0.000 claims abstract description 65
- 239000003054 catalyst Substances 0.000 claims abstract description 64
- 239000007789 gas Substances 0.000 claims abstract description 43
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims abstract description 37
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims abstract description 35
- 230000004907 flux Effects 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 238000009833 condensation Methods 0.000 claims abstract description 17
- 230000005494 condensation Effects 0.000 claims abstract description 17
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- 230000009467 reduction Effects 0.000 claims abstract description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012495 reaction gas Substances 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000008246 gaseous mixture Substances 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 230000005587 bubbling Effects 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000011148 porous material Substances 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 4
- 239000003921 oil Substances 0.000 description 28
- 238000005984 hydrogenation reaction Methods 0.000 description 19
- 230000000694 effects Effects 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 239000012071 phase Substances 0.000 description 6
- 230000008929 regeneration Effects 0.000 description 6
- 238000011069 regeneration method Methods 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000003245 coal Substances 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 230000002411 adverse Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000005997 Calcium carbide Substances 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- AMXBISSOONGENB-UHFFFAOYSA-N acetylene;ethene Chemical group C=C.C#C AMXBISSOONGENB-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 carbonyl sulfur Chemical compound 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- CLZWAWBPWVRRGI-UHFFFAOYSA-N tert-butyl 2-[2-[2-[2-[bis[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]amino]-5-bromophenoxy]ethoxy]-4-methyl-n-[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]anilino]acetate Chemical compound CC1=CC=C(N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)C(OCCOC=2C(=CC=C(Br)C=2)N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)=C1 CLZWAWBPWVRRGI-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Classifications
-
- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C5/00—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
- C07C5/02—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation
- C07C5/08—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation of carbon-to-carbon triple bonds
- C07C5/09—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation of carbon-to-carbon triple bonds to carbon-to-carbon double bonds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The present invention relates to it is a kind of using prepared in slurry bed reactor for the reaction system and method for ethylene.System includes：Paste state bed reactor, condenser, condensation separator, condensate tank, solvent pump, bottom of towe solvent tank, filter plant, green oil removing system, high-temperature heating equipment and catalyst reduction device；Paste state bed reactor includes housing, heater and sieve plate；The lower part of housing is equipped with reaction gas inlet, liquid flux entrance, liquid outlet；The top of housing is equipped with gas vent and liquid inlet；Heater is arranged on the lower part in housing；Sieve plate is located in housing, is fixed in inner walls.The present invention also provides the method that ethylene is prepared using above system, including：The gaseous mixture of acetylene and hydrogen is sent into paste state bed reactor and is reacted；The gas after reaction is made to pass through condensation separation and obtains ethylene；The recyclable utilization of catalyst being obtained by filtration.The present invention can effectively solve the problems, such as prior art preparation ethylene so that internal heat be not easy to spread out of, catalyst utilization it is low.
Description
Technical field
Present invention relates generally to the preparation fields of ethylene, and in particular to it is a kind of using prepared in slurry bed reactor for the anti-of ethylene
Answer system and method.
Background technology
Ethylene is one of a kind of important basic material and the chemicals of world wide production maximum in modern industry, production
Product are widely used in the fields such as national economy, people's lives, national defence, are " mothers of organic synthesis ".In face of the shortage of petroleum resources
With riseing for international oil price, raw material sources are asked as what the bottleneck and pendulum of development ethylene industry must solve in face of people
Topic.Therefore, a kind of new technology is researched and developed to prepare ethylene, it, can be allowed to substitute oil as industrial raw materials
Alleviate dependence of the modern industry to oil.
In coal chemical technology, Non-catalytic partial is passed through as raw material by calcium carbide technique or by raw material of natural gas using coal
Oxidation technology produces acetylene, it has also become maturation process.Again using acetylene as raw material, under the action of selective hydrocatalyst, lead to
It crosses hydrogenation process and obtains ethylene product, can further expand Coal Chemical Industry Route.Therefore, the new process of producing ethylene with acetylene hydrogenation is developed
Technology has broad application prospects.
Low concentration acetylene gas and solid phase catalyzing hydrogen addition technology is highly developed in the oil industry, is mainly used for removing in ethylene
Acetylene impurities, the reactor used are fixed bed reactors, load solid-phase catalyst in the reactor and carry out gas-solid phase reaction.But
Due to ethyne reactive height, hydrogenation reaction thermal discharge is big, even there are a small amount of acetylene in cracking gas, traditional gas is solid phase fixed bed
There are still green oil generating amount is big, the catalyst circulation period is short, reactor easily serious problems such as " temperature runaway " for hydrogenation reactor.
The prior art one is the fluidized-bed process and device of a kind of producing ethylene with acetylene hydrogenation.The technique includes the following steps：
Catalyst and diluent are added in fluidized-bed reactor；Heating reduction is carried out to catalyst；Acetylene and hydrogen mixture are led to
Fluidized bed reactor；Selective hydrogenation of acetylene generates ethylene；Cooling medium is passed through reactor heat exchange component to remove reaction
Heat；Isolated ethylene product.The technology has the following disadvantages：
Preparing ethylene by selective hydrogenation of acetylene is strong exothermal reaction, although cooling medium is to remove reaction in the process
The a large amount of heat released, but be still difficult to completely eliminate the hidden danger that part gas temperature is excessively high when reacting；
Because of the fluid bed that the technique uses, it is just difficult to avoid that the mutual sharp impacts of catalyst particles intergranular, this can bring catalysis
The loss of agent, increases the problems such as abrasion of heat exchange component and reactor at the difficulty for increasing dedusting.
The prior art two continuously detaches production line for a kind of ethylene, including oxygen hydrogenation reactor, the second drier of cracking gas,
Removal of mercaptans/carbonyl sulfur reactor, dearsenification reactor, acetylene hydrogenation reactor.Used by its acetylene hydrogenation reactor used
Reactor is fixed bed reactors.The acetylene of processing low concentration is merely able to, and treating capacity is smaller；If acetylene content increases,
A large amount of green oils can be generated, the catalyst circulation period is caused to shorten, even will appear the problem of reactor " temperature runaway ".
Therefore, in order to enable reactor adapts to larger amount of reaction acetylene gas, will not cause catalyst utilization it is low,
The problem of reactor " temperature runaway ", fundamentally improves gas-liquid flow field distribution, improves the quality fluidized in reactor, it is necessary to propose
A kind of new reaction system and method that prepare ethylene.
Invention content
The purpose of the present invention is to provide it is a kind of using prepared in slurry bed reactor for the reaction system and method for ethylene, with solution
The problem of certainly prior art preparation ethylene causes internal heat to be not easy to spread out of, catalyst utilization is low.
The present invention provide it is a kind of using prepared in slurry bed reactor for the reaction system of ethylene, including：Paste state bed reactor,
Condenser, condensation separator, condensate tank, solvent pump, bottom of towe solvent tank, filter plant, green oil removing system, high temperature add
Thermal and catalyst reduction device；Wherein described paste state bed reactor includes housing, heater and sieve plate；Under the housing
Portion is equipped with reaction gas inlet, liquid flux entrance, liquid outlet；The top of the housing is equipped with gas vent and liquid enters
Mouthful；The heater is arranged on the lower part in the housing；The sieve plate is located in the housing, is fixed on the inner walls
On, under the liquid inlet, on the reaction gas inlet, the liquid flux entrance；The green oil removing system
System is connected by the liquid flux entrance with the paste state bed reactor, and the bottom of towe solvent tank passes through the liquid outlet
It is connected with the paste state bed reactor, the condenser is connected by the gas vent with the paste state bed reactor, described
Solvent pump is connected by the liquid inlet with the paste state bed reactor；It is the condenser, the condensation separator, described cold
Lime set storage tank and the solvent pump are sequentially communicated；The bottom of towe solvent tank, the filter plant, the high-temperature heating equipment,
The catalyst reduction device and the condensate tank are sequentially communicated；The filter plant connects with green oil removing system
It is logical.
Above-mentioned system is equipped with agitating device in the condensate tank.
Above-mentioned system, the condensation separator connect ethylene collection device.
Above-mentioned system is dispersed with the sieve plate that multilayer is mutually parallel, the sieve plate of adjacent layer inside the paste state bed reactor
Between it is spaced, the interval of each layer sieve plate is equal.
Above-mentioned system, every layer of sieve plate include seal pot, bubbling area, downflow weir and downspout；Wherein, the sieve plate
Part edge fixed with the inner walls；The fixed part edge is by liquid with the part that the downflow weir fences up
Disk；For holding the liquid flowed down from downspout described in upper strata；Sieve pore is distributed in the centre of the seal pot, forms bubbling
Area, the bubbling area are the main regions of gas liquid reaction；The downflow weir is located at revocable edge of the sieve plate, described to overflow
Seal pot of the weir higher than place layer is flowed, for keeping the height of liquid on every layer of sieve plate；The downspout is used to make liquid
The seal pot of sieve plate described in lower floor is flow to from the downflow weir of sieve plate described in upper strata, positioned at the side of the downflow weir.
Above-mentioned system, the sieve pore are equally distributed circular aperture, and the centre-to-centre spacing of the aperture is the 1-5 in aperture
Times, a diameter of 5-20mm of the aperture.
Above-mentioned system, the sieve pore of the sieve plate are equipped with float valve or bubble-cap.
Above-mentioned system, the bottom end of the downspout of sieve plate described in upper strata are not higher than the height of sieve plate downflow weir described in lower floor.
The present invention provides a kind of method that ethylene is prepared using above system, the method includes：
The gaseous mixture of acetylene and hydrogen is sent into the paste state bed reactor；Using the solvent pump by the condensate liquid
Liquid flux and catalyst in storage tank are sent into the paste state bed reactor；Make the liquid flux with catalyst in the slurry
The bottom of the paste state bed reactor is flow in state bed reactor through the sieve plate；Utilize the institute of the paste state bed reactor bottom
It states heater and the liquid flux is evaporated to solvent vapo(u)r；The gaseous mixture of the acetylene and hydrogen is made to be carried out by catalyst anti-
It should；The gas after the acetylene and hydrogen reaction is made to circulate from the paste state bed reactor into the condenser, then by described
Condensation separator condenses out the solvent in the gas after the reaction；The solvent condensed out is made to enter the condensation
Condensed gas is obtained ethylene by liquid storage tank through refrigerated separation again；The partially liq for making the paste state bed reactor bottom is molten
Agent and catalyst enter the bottom of towe solvent tank, then pass through the filter plant；The partially liq being obtained by filtration is molten
The bottom of the paste state bed reactor is returned again to after the agent feeding green oil removing system；The partially catalyzed that will be obtained by filtration
Agent is sequentially sent to the high-temperature heating equipment, catalyst reduction device and condensate tank.
Above-mentioned method is mixed the catalyst and the liquid flux by the agitating device in the condensate tank
After closing uniformly, then will the mixed catalyst and the liquid flux feeding slurry bed system by the solvent pump
In reactor.
The beneficial effects of the present invention are, the present invention propose it is a kind of it is new using prepared in slurry bed reactor for the anti-of ethylene
System and method is answered, the reaction system and method are simple to operation, and reaction process is easily achieved shifting heat, and catalyst is recycled profit
With green oil can be removed in time so that carrying out high concentration selective hydrogenation of acetylene using paste state bed reactor becomes a kind of important
Alkene processed production ways.
Description of the drawings
Fig. 1 is the structure diagram for the paste state bed reactor that technical solution of the present invention prepares ethylene；
Fig. 2 is the overlooking the structure diagram of sieve plate in technical solution of the present invention；And
Fig. 3 is the system structure flow diagram that technical solution of the present invention embodiment prepares ethylene.
Specific embodiment
Below in conjunction with drawings and examples, the specific embodiment of the present invention is described in more details, so as to energy
The advantages of enough more fully understanding the solution of the present invention and its various aspects.However, specific embodiments described below and reality
Example is applied to be for illustrative purposes only rather than limitation of the present invention.
If Fig. 1 is the structure chart of the paste state bed reactor in the present invention.Wherein：1st, reaction gas inlet；2nd, liquid outlet；
3rd, gas vent；4th, liquid inlet；5th, sieve plate；6th, downspout；7th, heater；8th, solvent liquid entrance.
The principle of paste state bed reactor be gas in the form of bubbling by being suspended with liquid (slurries) layer of solid fine grain, with
Realize the reactor of gas-liquid solid phase reaction process.This kind is used for the paste state bed reactor of preparing ethylene by selective hydrogenation of acetylene, described
Paste state bed reactor includes reactor shell, heater 7 and sieve plate 5.
Reactor shell lower part is provided with reaction gas inlet 1, solvent liquid entrance 8 and liquid outlet 2, reactor shell
Gas vent 3 is arranged at top.
In the bottom having heaters 7 of reactor, penetrate in reactor enclosure body.Wherein, heater 7 can steam solvent
Hair, provides the steam air-flow continuously risen, while provide heat source for entire reactor.
The sieve plate 5 is located in the housing, is fixed in the inner walls, under the liquid inlet 4, institute
State reaction gas inlet 1, on the liquid flux entrance 8.
Middle part in reactor enclosure body is evenly distributed sieve plate 5.Have on every layer of sieve plate 5 seal pot, downflow weir,
Downspout 6 and bubbling area.Part edge and the inner walls of sieve plate are fixed, and revocable edge is equipped with downflow weir.Fixed portion
Point edge is seal pot with the part that the downflow weir fences up, for holding the liquid flowed down from upper strata downspout.
The vertical view of sieve plate 5 is as shown in Figure 2.Being to maintain on every layer of sieve plate in the effect of the downflow weir of one end of sieve plate 5 has
The liquid of certain altitude.Downspout 6 is next in downflow weir.Specifically, the downflow weir and institute that downspout can be by the sieve plate
The gap for stating reactor wall is formed.It is such as pipeline configuration that certain downspout 6, which may also be other structure,.The effect of downspout 6
It is the seal pot that liquid is allowed to flow to lower floor's sieve plate at the downflow weir of upper sieve plate.The bottom end of the downspout 6 of upper sieve plate 5 is not high
In the height of 5 downflow weir of lower floor's sieve plate.Design is to realize fluid-tight in this way, that is, preventing gas from rising at downspout 6 causes
Each layer gas connects and short-circuit.Central region on sieve plate 5 is bubbling area, is uniform-distribution with circular aperture thereon.Aperture is
The main thoroughfare that gas rises, enables to gas uniformly to be contacted with liquid.
The downspout 6 of reactor adjacent layer is in being projected on circumferential angle on the direction of the seal pot
It is staggeredly arranged.Facilitate in this way and realize that the liquid that upper sieve plate 5 flows down is stored in 5 upper certain time of adjacent lower sieve plate, until liquid
Body is higher by the downflow weir of the lower floor and flows out to again the sieve plate 5 of lower floor.
The flow direction of aperture and liquid can keep fork row pattern state, and the arrangement mode of aperture can be positive triangle formula.Small hole center away from
It it is 1-5 times of aperture, the centre-to-centre spacing between preferred hole is 1.5 times；A diameter of 5-20mm in hole, preferred hole it is a diameter of
10mm。
Float valve or bubble-cap can be also equipped on the sieve pore of sieve plate.Float valve can float on sieve plate, with gas flow
Change and change its open degree.There is riser in bubble-cap, rotary space is formed between bubble-cap and riser.Riser is fixed on
On sieve plate, gas phase enters rotary space by riser, is sprayed with certain spouting velocity by slot, with the liquid shape on sieve plate
It is contacted into bubbling.
The reaction system for ethylene using prepared in slurry bed reactor is illustrated in figure 3, including what is mentioned in above description
Paste state bed reactor 10, condenser 30, condensation separator 40, condensate tank 50, solvent pump 60, bottom of towe solvent tank 70, mistake
Filter equipment 80, green oil removing system 90, high-temperature heating equipment 100 and catalyst reduction device 110.Green oil removing system 90 passes through
The liquid flux entrance is connected with the paste state bed reactor 10, the bottom of towe solvent tank 70 by the liquid outlet with
The paste state bed reactor 10 connects, and the condenser 30 is connected by the gas vent with the paste state bed reactor 10,
The solvent pump 60 is connected by the liquid inlet with the paste state bed reactor 10；The condenser 30, the condensation point
It is sequentially communicated from device 40, the condensate tank 50 and the solvent pump 60；The bottom of towe solvent tank 70, the filter plant
80th, the high-temperature heating equipment 100, the catalyst reduction device 110 and the condensate tank 50 are sequentially communicated, catalyst
Pass sequentially through above equipment；The paste state bed reactor 10, the bottom of towe solvent tank 70, the filter plant 80 with it is described green
Oily removing system 90 connects, and solvent passes sequentially through above equipment.
Above-mentioned system is equipped with agitating device in the condensate tank 50, for solvent in condensate tank 50 with urging
The stirring of agent.
When preparing ethylene, the gaseous mixture of acetylene and hydrogen by the reaction gas inlet 1 of 10 bottom of paste state bed reactor into
Enter into reactor；Reaction gas with solvent vapo(u)r together by the aperture on the sieve plate of inside reactor enter liquid phase it
In.Wherein solvent vapo(u)r generates liquid flux heating evaporation by the heater 7 of reactor bottom.Catalyst and carrier solvent
It is flowed into the liquid inlet 4 on autoreactor top.Because aperture is equally distributed on sieve plate 5, so reaction gas is also therewith
It evenly spreads in liquid.In a liquid, reaction gas occurs instead under the catalytic action of the catalyst in being suspended in liquid
It should.Gas after reaction is detached from this layer of sieve plate 5, then is entered in supernatant liquid by the aperture of upper sieve plate 5.So repeatedly
Until by the sieve plate 5 of reactor the top, go out from the gas vent 3 of reactor top.
In the reactor, gas be to it is lower and on flow direction, liquid is flow direction from top to down, and gas phase and liquid phase are in integrally
Reveal the direction of adverse current, increase the effect of mass transfer and heat transfer.Due to having multiple sieve plate in reactor, that is, mean to react
There is multiple small paste state bed reactors in device, increase the contact area that gas-liquid-solid three-phase comes into full contact with, improve gas-liquid
Flow Field Distribution avoids short circuit, but also can strengthen turbulence and gas-liquid mass transfer, improves the quality fluidized in reactor.
The reaction gas come out from reactor top, then gas temperature is cooled down by the cooling of condenser 30.Then,
The solvent in gas is condensed out by condensation separator 40 again.The solvent condensed out enters condensate tank 50, gas
Body can obtain product ethylene using depth refrigerated separation.
Bottom of towe solvent tank 70 is entered by liquid outlet in the solvent of reactor bottom, then by filter plant 80,
After calcining of the catalyst using high-temperature heating equipment 100 after filtering, can effectively Removal of catalyst surface attachment green oil
With the impurity such as solvent, the regeneration of catalyst is realized.But the catalyst after calcination is oxidation state, therefore to pass through catalyst reduction and fill
110 are put to realize the reduction of catalyst.Catalyst after reducing/regenerating is added in condensate tank 50 again.And it filters out
Solvent is then entered in green oil removing system 90.System 90 is removed by green oil to detach green oil with solvent, solvent passes through reaction
The liquid inlet of device bottom is returned to reactor, and green oil is then preserved into green oil storage tank.
In condensate tank 50, by agitating device by catalysts and solvents after mixing, then pass through solvent pump 60
Mixed liquid is sent in reactor.The process can realize recycling for catalyst.
In the present embodiment, the solvent used is distilled water (5 μm/cm of conductivity ＜).Rise from reactor bottom
Steam is the heat source of entire reactor, keeps stablizing relatively for system temperature.When starting selective hydrogenation of acetylene reaction, release
A large amount of heat can be shifted by the evaporation of solvent, avoid and occur the phenomenon that local temperature is excessively high in reactor.
Heater in the present invention can be come using the mode of electrical heating, steam heating, flue gas or heat-conducting oil heating
It realizes.
High-temperature heating equipment in the present invention can be realized using heating units such as electrical heating, revolving bed, fluid beds.
Compared with the technology of acetylene hydrogenation a small amount of in current ethylene, this technology can be realized to be added by high concentration selective acetylene
Hydrogen ethylene has further expanded the technology path of coal chemical industry.
Further, in the technical solution of the present invention, gas be to it is lower and on flow direction, liquid is stream from top to down
The direction of adverse current is integrally showed to, gas phase and liquid phase, increases the effect of mass transfer and heat transfer.
Further, there is multiple sieve plate in the reactor of technical scheme of the present invention, that is, mean to deposit in reactor
In multiple small paste state bed reactors, the area that gas-liquid-solid three-phase comes into full contact with is increased, improves gas-liquid flow field distribution, it can
Short circuit is avoided, but also turbulence and gas-liquid mass transfer can be strengthened, improves the quality fluidized in reactor.
Further, green oil removing system and catalyst regeneration system is provided in system, significantly reduce green oil and
Catalyst activity reduces the influence to reaction, realizes the smooth long term running of device；The system and method for the present invention makes simultaneously
Obtaining catalyst can recycle, and improve the utilization ratio of catalyst.
Using the sensible heat of liquid phase solvent, (sensible heat refers to, when the addition of this heat or after remove, to lead technical scheme of the present invention
The variation of mass temperature is caused, without phase transformation), heat-sinking capability significantly improves, and can be quickly moved out because of selective hydrogenation of acetylene
The heat for generating ethylene and generating, reduces the temperature of reaction bed, improves the conversion ratio of acetylene and the selectivity of ethylene.
In addition, the heating system of the technical program is simple, the heater for only relying on reactor bottom can be realized as heat supply.
In short, reaction system provided by the invention and method, when carrying out selective hydrogenation of acetylene reaction, can be effectively prevented from
" temperature runaway " phenomenon occurs, can preferably inhibit the preparation of ethylene through selective hydrogenation of acetylene catalyst bed because of caused by exothermic reaction in the process
The appearance of hot spot, can remove green oil, avoid catalyst inactivation, improve the stability of catalyst in time in layer.The present invention proposes
Equipment using having well solved the problem of catalyst use efficiency is low by the way of catalyst recycling.
Embodiment 1
It is as shown in Figure 3 using the system for preparing ethylene by selective hydrogenation of acetylene in embodiment.System structure is as above
State the form described in embodiment.The operating pressure of the system is 0.25MPa, and temperature is 130 DEG C.
Can first by the use of nitrogen as air source, with paste state bed reactor 10 in the solvent containing catalyst establish gas-liquid flow direction；
Then, then gradually the heater of bottom is opened, establishes steam ascending air.When steam rises to reactor head cooling for reflux,
And after temperature is stablized, can nitrogen be gradually converted to hydrogen and the gaseous mixture of acetylene gas is passed into reactor.
In the reactor, acetylene and hydrogen generate ethylene under the catalytic action of catalyst；Gas after reaction passes through again
Condenser 30 and condensation separator 40 after the solvent in gas is condensed out, then send out reaction system battery limit (BL).Condensation separator
40 can further connect ethylene collection device, such as cryogenic separation device, to obtain ethylene product.
The catalyst of reactor bottom is flow to solvent from reactor head, then is filtered out by filter plant 80；When
It was found that when catalyst activity reduces, catalyst is passed sequentially through into 110 groups of high-temperature heating equipment 100 and catalyst reduction device
Into catalyst regeneration system, realize the regeneration of catalyst；Then the catalyst after regeneration is transferred to condensate tank 50 again
In the middle；In condensate tank 50 after mixing, it is transported to reactor head using solvent pump 60.When in discovery solvent
Green oil amount increase, when reducing reactivity, the solvent filtered out from filter plant 80 can be passed into green oil removing system
In system 90, green oil therein is removed.Green oil removes system 90 and catalyst regeneration system significantly reduces green oil and catalyst
Activity reduces the influence to reaction, realizes the smooth long term running of device.
In the present embodiment, the solvent used is distilled water (5 μm/cm of conductivity ＜), the steaming risen from reactor bottom
Vapour is the heat source of entire reactor, keeps stablizing relatively for system temperature.When starting selective hydrogenation of acetylene reaction, releasing
A large amount of heat, can be shifted by the evaporation of solvent, it is excessively high to avoid local temperature.The grain size of the catalyst used is 40-
150 μm, the filtering accuracy of the filter plant used is 1 μm.
Finally it should be noted that：Obviously, the above embodiment is merely an example for clearly illustrating the present invention, and simultaneously
The non-restriction to embodiment.For those of ordinary skill in the art, it can also do on the basis of the above description
Go out other various forms of variations or variation.There is no necessity and possibility to exhaust all the enbodiments.And thus drawn
The obvious changes or variations that Shen goes out are still in the protection scope of this invention.
Claims (10)
1. it is a kind of using prepared in slurry bed reactor for the reaction system of ethylene, including：Paste state bed reactor, condenser, condensation
Separator, condensate tank, solvent pump, bottom of towe solvent tank, filter plant, green oil remove system, high-temperature heating equipment and urge
Agent reduction apparatus；
Wherein described paste state bed reactor includes housing, heater and sieve plate,
The lower part of the housing is equipped with reaction gas inlet, liquid flux entrance, liquid outlet；The top of the housing is equipped with gas
Body exports and liquid inlet；
The heater is arranged on the lower part in the housing, penetrates in reactor enclosure body, for making evaporation of the solvent, provides continuous
The steam air-flow of rising, while provide heat source for entire reactor；
The sieve plate is located in the housing, is fixed in the inner walls, under the liquid inlet, the reaction
On gas access, the liquid flux entrance；
The green oil removing system is connected by the liquid flux entrance with the paste state bed reactor, the bottom of towe solvent storage
Tank is connected by the liquid outlet with the paste state bed reactor, and the condenser passes through the gas vent and the slurry
Bed reactor connection, the solvent pump are connected by the liquid inlet with the paste state bed reactor；
The condenser, the condensation separator, the condensate tank and the solvent pump are sequentially communicated；The bottom of towe solvent
Storage tank, the filter plant, the high-temperature heating equipment, the catalyst reduction device and the condensate tank connect successively
It is logical；The filter plant removes system connectivity with the green oil.
2. system according to claim 1, which is characterized in that agitating device is equipped in the condensate tank.
3. system according to claim 1, which is characterized in that the condensation separator connects ethylene collection device.
4. system according to claim 1, which is characterized in that it is mutually flat that multilayer is dispersed with inside the paste state bed reactor
Capable sieve plate, spaced between the sieve plate of adjacent layer, the interval of each layer sieve plate is equal.
5. system according to claim 1, which is characterized in that every layer of sieve plate includes seal pot, bubbling area, downflow weir
And downspout；Wherein, the part edge of the sieve plate is fixed with the inner walls；
The fixed part edge is seal pot with the part that the downflow weir fences up, for holding from descending liquid described in upper strata
The liquid that pipe flows down；
Sieve pore is distributed in the centre of the seal pot, forms bubbling area, the bubbling area is the main region of gas liquid reaction；
The downflow weir is located at revocable edge of the sieve plate, and the downflow weir is higher than the seal pot of place layer, for keeping every
The height of liquid on the layer sieve plate；
The downspout is for making the downflow weir of sieve plate described in liquid from upper strata flow to the seal pot of sieve plate described in lower floor, positioned at institute
State the side of downflow weir.
6. system according to claim 5, which is characterized in that the sieve pore is equally distributed circular aperture, described small
The centre-to-centre spacing in hole is 1-5 times of aperture, a diameter of 5-20mm of the aperture.
7. system according to claim 5, which is characterized in that the sieve pore of the sieve plate is equipped with float valve or bubble-cap.
8. system according to claim 5, which is characterized in that the bottom end of the downspout of sieve plate described in upper strata is not higher than lower floor
The height of the sieve plate downflow weir.
9. a kind of method for preparing ethylene using any one of claim 1 to 8 system, the method includes：
The gaseous mixture of acetylene and hydrogen is sent into the paste state bed reactor；
The liquid flux in the condensate tank and catalyst are sent into the paste state bed reactor using the solvent pump；
The liquid flux is made to flow to the paste state bed reactor through the sieve plate in the paste state bed reactor with catalyst
Bottom；
The liquid flux is evaporated to solvent vapo(u)r using the heater of the paste state bed reactor bottom；
The gaseous mixture of the acetylene and hydrogen is made to pass through catalyst to be reacted；
The gas after the acetylene and hydrogen reaction is made to circulate from the paste state bed reactor into the condenser, then by described
Condensation separator condenses out the solvent in the gas after the reaction；The solvent condensed out is made to enter the condensation
Condensed gas is obtained ethylene by liquid storage tank through refrigerated separation again；
The partially liq solvent and catalyst for making the paste state bed reactor bottom enter the bottom of towe solvent tank, then pass through institute
State filter plant；The slurry bed system is returned again to after the partially liq solvent being obtained by filtration is sent into the green oil removing system
The bottom of reactor；The partial catalyst being obtained by filtration is sequentially sent to the high-temperature heating equipment, catalyst reduction dress
It puts and condensate tank.
10. it according to the method described in claim 9, it is characterized in that, will be urged by the agitating device in the condensate tank
Agent and liquid flux are after mixing, then molten by the mixed catalyst and the liquid by the solvent pump
Agent is sent into the paste state bed reactor.
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| FR2817767B1 (en) * | 2000-12-07 | 2003-02-28 | Technip Cie | PROCESS AND PLANT FOR THE RECOVERY AND PURIFICATION OF ETHYLENE PRODUCED BY PYROLYSIS OF HYDROCARBONS, AND GASES OBTAINED BY PROCESS |
| US8471082B2 (en) * | 2008-03-14 | 2013-06-25 | Catalytic Distillation Technologies | Process for converting methane to ethylene |
| CN102489225B (en) * | 2011-12-10 | 2014-05-21 | 太原理工大学 | Slurry bubble column technology for preparing ethylene through acetylene hydrogenation and device thereof |
| CN103044179A (en) * | 2012-12-19 | 2013-04-17 | 清华大学 | Method for preparing ethylene through liquid-phase selective hydrogenation of acetylene in slurry reactor |
| CN104826558B (en) * | 2015-05-15 | 2016-10-12 | 北京神雾环境能源科技集团股份有限公司 | Paste state bed reactor and response system for preparing ethylene by selective hydrogenation of acetylene |
| CN105175208B (en) * | 2015-08-07 | 2017-11-14 | 北京华福工程有限公司 | Acetylene hydrogenation prepares the method for ethene and the reaction tower for this method |
| CN206045989U (en) * | 2016-06-14 | 2017-03-29 | 北京神雾环境能源科技集团股份有限公司 | A kind of response system of utilization prepared in slurry bed reactor for ethylene |
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