CN105418352A - Device and method for producing ethylene through hydrogenation of high concentration acetylene - Google Patents
Device and method for producing ethylene through hydrogenation of high concentration acetylene Download PDFInfo
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- CN105418352A CN105418352A CN201511019629.1A CN201511019629A CN105418352A CN 105418352 A CN105418352 A CN 105418352A CN 201511019629 A CN201511019629 A CN 201511019629A CN 105418352 A CN105418352 A CN 105418352A
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Abstract
The invention provides a device and method for producing ethylene through hydrogenation of high concentration acetylene. The device comprises an acetylene hydrogenation reactor, a solvent absorbing tower, and an ethylene condensing device. The structure of the device is simple. An acetylene feed pipeline is connected to the acetylene hydrogenation reactor through an acetylene solvent tank; acetylene is dissolved into a solvent and then introduced into the acetylene hydrogenation reactor; through liquid phase pressurization, the pressure limitation of acetylene is overcome, thus hydrogenation of acetylene can be carried out under a pressure of 1.5 MPaG or more; the acetylene hydrogenation reactor is connected to the solvent absorbing tower, after the acetylene hydrogenation, the obtained gas phase is absorbed by the solvent, the multi-tower rectification separation in the conventional technology is not needed therefore, and the energy consumption is low. The provided device and method can utilize the excess calcium carbide product, greatly relieves the demand on ethylene in our country, and has an important meaning for the sustainable development of acetylene industry of our country, energy saving, and emission reduction.
Description
Technical field
The present invention relates to technical field of petrochemical industry, in particular to a kind of device and method of high density producing ethylene with acetylene hydrogenation.
Background technology
Ethene is a kind of important basic material in modern industry, is also one of maximum chemical of world wide production.Ethylene yield has become the mark of a measurement national oil development of chemical industry level, and its throughput is counted as the embodiment of a national economic strength.
Ethene is mainly obtained by the method for cracking petroleum hydrocarbon, and oil is a kind of Nonrenewable resources in short supply, and its price with impact fluctuations such as international environment changes very greatly.Current China annual petroleum consumption rank the second in the world, within 2011, dependence on foreign countries for oil reaches 56.5%, and this defines serious strategy threat concerning China that oil reserve is not enriched.Therefore, the another kind of new source of searching and processing method prepare large basic organic chemical raw material-ethene, at field of industrial production petroleum replacing as raw material, can alleviate the dependency of China for oil to a great extent.
Not yet carry out the direct technique for producing ethylene of acetylene in the world to explore.The lower concentration acetylene gas solid catalysis hydrogen addition technology of current widespread use and high purity acetylene ethene have very large difference.
Lower concentration acetylene gas solid catalysis hydrogen addition technology is very ripe in the oil industry, is mainly used in removing acetylene impurities in ethene.The existence of acetylene, can reduce the activity of ethylene rolymerization catalyst, and polymerization is deteriorated, and therefore acetylene content should be controlled at below 1ppm.For the course of processing of some particular requirement, the production of such as low pressure polyethylene, in smart ethene, acetylene content requires to be less than 0.1ppm.Remove a small amount of (about 1%) acetylene in ethene in industry and adopt fixed-bed process, with Pd or Ni for catalyzer, react under 30 ~ 100 DEG C of conditions.But because ethyne reactive high hydrogenation reaction heat effect is large, even there is a small amount of acetylene in splitting gas, still there are the serious problems such as green oil generating amount is large, the catalyst recirculation cycle is short, reactor easy " temperature runaway " in traditional fixed bed hydrogenation reactor.Therefore, when removing acetylene in petroleum industry, while usually adopting millisecond pyrolyzer, original one-stage hydrogenation technique is changed into the multi-stek hydrogenation technique of three series connection, intersegmental cooling, reaction process is comparatively complicated.
In view of this, special proposition the present invention.
Summary of the invention
The first object of the present invention is the device providing a kind of high density producing ethylene with acetylene hydrogenation, the device of described high density producing ethylene with acetylene hydrogenation has structure simply, is pressurizeed by liquid phase, overcomes acetylene pressure restriction, acetylene hydrogenation can be made at more than 1.5MPaG pressure operation, low power consumption and other advantages.
The second object of the present invention is to provide a kind of method of carrying out producing ethylene with acetylene hydrogenation adopting the device of above-mentioned high density producing ethylene with acetylene hydrogenation, and the method technique is simple, overcomes acetylene pressure restriction, acetylene hydrogenation can be made at more than 1.5MPaG pressure operation; Meanwhile, after hydrogenation reaction, tail gas is by solvent absorbing, avoids multitower rectifying separation in traditional technology, reduces energy consumption, and technique is advanced.
In order to realize above-mentioned purpose of the present invention, spy by the following technical solutions:
A device for high density producing ethylene with acetylene hydrogenation, the device of described high density producing ethylene with acetylene hydrogenation comprises acetylene hydrogenation reactor, solvent absorbing tower and ethene concentration unit; Wherein, acetylene hydrogenation reactor, solvent absorbing tower are connected in turn with ethene concentration unit; Described acetylene hydrogenation reactor is connected with hydrogen feed pipeline with acetylene feeding pipe respectively; Described acetylene feeding pipe arranges solvents for ethyne tank; Described ethene concentration unit is connected with ethene discharging pipeline.
The apparatus structure of high density producing ethylene with acetylene hydrogenation of the present invention is simple, acetylene feeding pipe is connected with acetylene hydrogenation reactor by solvents for ethyne tank, acetylene is dissolved and passes into acetylene hydrogenation reactor more in a solvent, pressurizeed by liquid phase, overcome acetylene pressure restriction, acetylene hydrogenation can be made at more than 1.5MPaG pressure operation; Acetylene hydrogenation reactor is connected with solvent absorbing tower, and after acetylene hydrogenation reaction, gained gas phase is by solvent absorbing, and avoid multitower rectifying separation in traditional technology, energy consumption is low.
Described acetylene feeding pipe is preferably connected with bottom acetylene hydrogenation reactor respectively by venturi-type eductors with hydrogen feed pipeline.The solvent and the hydrogen that are dissolved with acetylene preferably mix in venturi-type eductors.
Acetylene feeding pipe between described solvents for ethyne tank and acetylene hydrogenation reactor preferably arranges interchanger.
Described acetylene hydrogenation reactor preferably adopts paste state bed reactor, in-built solvent.
Preferably be connected with catalyst filtration device, in order to reclaim spent catalyst bottom described acetylene hydrogenation reactor.Described catalyst filtration device preferably adopts one or more of plate and frame(type)filter press, chamber-type press filter, pressure leaf filter, Rotary Filter Press or belt filter press.
Described solvent absorbing tower bottom preferably sequentially passes through pump and is connected with solvent absorbing top of tower with interchanger.
Described solvent absorbing tower is connected with solvent treatment tower; Described solvent treatment tower is connected with acetylene hydrogenation reactor, and the solvent recuperation after refining uses.
Described solvent treatment top of tower is connected with light constituent discharging pipeline; Described solvent treatment tower bottom is connected with heavy constituent discharging pipeline.
Described solvent treatment top of tower sequentially passes through interchanger and is connected with light constituent discharging pipeline with return tank.
Described solvent treatment tower bottom is preferably connected with interchanger, forms circulation loop.
Each pipeline as required, preferably arranges corresponding valve, respectively in order to control the opening and closing of each pipeline; Each pipeline is preferably connected in parallel, in order to monitor each pipeline actual condition with one or more in corresponding pressure warning unit, under meter, controller as required respectively.
Adopt the device of above-mentioned a kind of high density producing ethylene with acetylene hydrogenation to carry out the method for producing ethylene with acetylene hydrogenation, comprise the steps:
Raw material acetylene and solvent, the solvent having dissolved acetylene enters acetylene hydrogenation reactor; Hydrogen directly enters acetylene hydrogenation reactor; Both generate ethene at reaction in acetylene hydrogenation reactor; Reaction gained gas phase is after solvent absorbing, and in gas phase, ethene and hydrogen are isolated to product ethene.
The method technique of producing ethylene with acetylene hydrogenation of the present invention is simple, and raw material acetylene adopts the mode of dissolution with solvents, can overcome acetylene pressure restriction, acetylene hydrogenation can be made at more than 1.5MPaG pressure operation; Meanwhile, after hydrogenation reaction, tail gas is by solvent absorbing, avoids multitower rectifying separation in traditional technology, reduces energy consumption, and technique is advanced.
The method of described a kind of producing ethylene with acetylene hydrogenation, comprises the steps:
(1) acetylene hydrogenation:
Acetylene enters solvents for ethyne tank, mixes be dissolved completely in solvent with solvents for ethyne tank internal solvent, and solvent carries acetylene and after interchanger heating, send into acetylene hydrogenation reactor after pump boosting; Hydrogen to mix with acetylene at reactor inlet together sends into hydrogenator; Unstripped gas passes into bottom acetylene hydrogenation reactor, by the bubbling of gas, catalyzer is suspended with slurry form in a solvent, reacts; Heat of reaction is removed preferably by built-in heat exchanger; After reaction, gained gas phase sends into solvent absorbing tower;
Principal reaction equation is as follows:
C
2H
2+H
2→C
2H
4(1)
C
2H
2+2H
2→C
2H
6(2)
2C
2H
2+2H
2→C
4H
8(3)
(2) solvent absorbing:
After acetylene hydrogenation reaction, gained gas phase enters bottom solvent absorption tower, and solvent enters interchanger after solvent pump boosting, enters top, absorption tower through the cooled solvent of interchanger; Gained gas phase counter current contact after solvent and acetylene hydrogenation react, absorbs the byproduct of reaction in gas phase;
(3) ethene concentrate:
From top, solvent absorption tower gas phase out after ethene concentration unit ethene concentrate is refining, obtain product ethene; Hydrogen (may contain micro-by product) returns acetylene hydrogenation reactor recycle;
(4) solvent treatment:
The by product that acetylene hydrogenation produces, delivers to solvent treatment tower through solvent absorbing tower bottom; Solvent treatment tower carries out rectifying cutting to solvent; According to the difference with solvent boiling point, be referred to as light constituent and heavy constituent; The light constituent, the heavy constituent impurity that contain in solvent is removed by rectifying cutting; Solvent treatment tower lateral line withdrawal function refine after solvent, be pumped to acetylene hydrogenation reactor recycling;
(5) catalyst recovery:
Through long-time running, acetylene hydrogenation catalyst inactivation; Inactivation rear catalyst delivers to catalyst filtration device after stopping, and reclaims spent catalyst.
The pressure that acetylene enters acetylene cylinder is 0.02 ~ 0.2MPaG, and be preferably 0.02-0.15MPaG, temperature is-20 ~ 40 DEG C, is preferably-10 DEG C.
Solvent and acetylene throughput ratio are 2 ~ 20:1 (mass ratio), are preferably 5 ~ 10:1.
Acetylene solution mixes with hydrogen through venturi mixer, and hydrogen and acetylene throughput ratio are 2 ~ 10:1 (mol ratio), is preferably 4 ~ 6:1.
Hydrogen feed temperature is 20 ~ 200 DEG C, and be preferably 40 DEG C, feed pressure is 0.2 ~ 2.0MPaG, is preferably 0.45 ~ 1.5MPaG.
Described solvent is one or more in N-Methyl pyrrolidone, dimethyl formamide, dimethyl sulfoxide (DMSO), Monomethylamine and acetone.
Used catalyst is palladium be main active ingredient, silver and ruthenium is auxiliary agent, aluminium sesquioxide is the catalyzer of carrier.Reaction pressure is 0.1 ~ 3.0MPaG, and be preferably 0.45 ~ 1.5MPaG, more preferably 0.8MPaG, temperature of reaction is 120 ~ 250 DEG C, is preferably 150 DEG C.
Described solvent absorbing tower service temperature is-40 DEG C ~ 60 DEG C, and be preferably-5 ~ 40 DEG C, working pressure is 0.2 ~ 1.0MPaG, is preferably 0.2 ~ 0.8MPaG.
Described solvent preferably adopts fresh solvent, sealing and circulating.The cold medium that interchanger adopts be preferably in recirculated water, refrigerated water, liquefied ammonia, propylene one or more.
Adopt ethene concentrating method to be preferably membrane sepn is separated with PSA one or both.
Solvent treatment tower is preferably rectifying tower, and service temperature is-60 DEG C ~ 150 DEG C, and be preferably-20 ~ 30 DEG C, more preferably 20 DEG C, working pressure is-0.2MPaA ~ 1.5MPaG, is preferably 0.5 ~ 1.5MPaG, more preferably 1.0PaG.
Described catalyst filtration device preferably adopts operate continuously or periodical operation, and working pressure is-0.2MPaA ~ 1.5MPaG, and be preferably 0.5MPaA, operation pressure reduction is 0.02MPa ~ 0.6MPa, and be preferably 0.2MPaA, service temperature is 20 ~ 150 DEG C, is preferably 50 DEG C.
Compared with prior art, beneficial effect of the present invention is:
The apparatus structure of high density producing ethylene with acetylene hydrogenation of the present invention is simple, acetylene feeding pipe is connected with acetylene hydrogenation reactor by solvents for ethyne tank, acetylene is dissolved and passes into acetylene hydrogenation reactor more in a solvent, pressurizeed by liquid phase, overcome acetylene pressure restriction, acetylene hydrogenation can be made at more than 1.5MPaG pressure operation; Acetylene hydrogenation reactor is connected with solvent absorbing tower, and after acetylene hydrogenation reaction, gained gas phase is by solvent absorbing, and avoid multitower rectifying separation in traditional technology, energy consumption is low.The method technique of producing ethylene with acetylene hydrogenation of the present invention is simple, and raw material acetylene adopts the mode of dissolution with solvents, adopts acetylene liquid phase positive delivery, safer compared with pressurizeing with traditional acetylene in gas phase; Acetylene pressure is high pressure acetylene higher than 0.15MPaG, risk of very easily blasting, and therefore traditional technology seldom has acetylene high pressure operating mode; The method of producing ethylene with acetylene hydrogenation of the present invention can overcome acetylene pressure restriction, and acetylene hydrogenation can be made at more than 1.5MPaG pressure operation; Meanwhile, after hydrogenation reaction, tail gas is by solvent absorbing, avoids multitower rectifying separation in traditional technology, reduces energy consumption, and technique is advanced.The present invention finds a way out not only to the calcium carbide production capacity of China's surplus, and greatly alleviates China's ethylene requirements, has great importance to promotion China acetylene chemical industry Green Sustainable, energy-saving and emission-reduction.
Accompanying drawing explanation
In order to be illustrated more clearly in the specific embodiment of the invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the apparatus structure schematic diagram of high density producing ethylene with acetylene hydrogenation of the present invention;
Reference numeral:
1-acetylene hydrogenation reactor; 2-solvent absorbing tower; 3-solvent treatment tower;
4-ethene concentration unit; 5-acetylene cylinder; 6-return tank;
7-catalyst filtration device; 8-interchanger; 9-pump;
10-venturi-type eductors; PC, LC, FC, TC-controller.
Embodiment
Below in conjunction with the drawings and specific embodiments, technical scheme of the present invention is clearly and completely described, but it will be understood to those of skill in the art that, following described embodiment is the present invention's part embodiment, instead of whole embodiments, only for illustration of the present invention, and should not be considered as limiting the scope of the invention.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.Unreceipted actual conditions person in embodiment, the condition of conveniently conditioned disjunction manufacturers suggestion is carried out.Agents useful for same or the unreceipted production firm person of instrument, be and can buy by commercially available the conventional products obtained.
In describing the invention, it should be noted that, orientation or the position relationship of the instruction such as term " " center ", " on ", D score, "left", "right", " vertically ", " level ", " interior ", " outward " they be based on orientation shown in the drawings or position relationship; be only the present invention for convenience of description and simplified characterization; instead of instruction or imply the device of indication or element must have specific orientation, with specific azimuth configuration and operation, therefore can not be interpreted as limitation of the present invention.In addition, term " first ", " second ", " the 3rd " only for describing object, and can not be interpreted as instruction or hint relative importance.
In describing the invention, it should be noted that, unless otherwise clearly defined and limited, term " installation ", " being connected ", " connection " should be interpreted broadly, and such as, can be fixedly connected with, also can be removably connect, or connect integratedly; Can be mechanical connection, also can be electrical connection; Can be directly be connected, also indirectly can be connected by intermediary, can be the connection of two element internals.For the ordinary skill in the art, particular case above-mentioned term concrete meaning in the present invention can be understood.
Embodiment 1
Enter acetylene cylinder from out-of-bounds acetylene, it is 0.02 ~ 0.2MPaG that acetylene enters acetylene cylinder pressure, and this example is preferably 0.15MPaG, and temperature be-20 ~ 40 DEG C, this example preferably 10 DEG C.Mixing with acetylene cylinder internal solvent is dissolved completely in solvent, and solvent is the one or more combination of N-Methyl pyrrolidone, dimethyl formamide, dimethyl sulfoxide (DMSO), Monomethylamine and acetone, and this example is preferably N-Methyl pyrrolidone.Solvent and acetylene throughput ratio 2 ~ 20:1 (mass ratio), this example is preferably 10:1.Solvent carries acetylene and after interchanger heating, send into acetylene hydrogenation reactor after pump boosting.Hydrogen to mix with acetylene at acetylene hydrogenation reactor entrance together sends into hydrogenator.Hydrogen feed temperature is 20 ~ 200 DEG C, and this example is preferably 40 DEG C.Feed pressure is 0.2 ~ 2.0MPaG, and this example is preferably 1.5MPaG.Acetylene solution mixes with hydrogen through venturi mixer, and hydrogen and acetylene throughput ratio are 2 ~ 10:1 (mol ratio), and this example is preferably 4:1.
Principal reaction equation is as follows:
C
2H
2+H
2→C
2H
4(1)
C
2H
2+2H
2→C
2H
6(2)
2C
2H
2+2H
2→C
4H
8(3)
Described acetylene hydrogenation reactor adopts paste state bed reactor, in-built solvent.Solvent is one or more of N-Methyl pyrrolidone, dimethyl formamide, dimethyl sulfoxide (DMSO), Monomethylamine and acetone.This example is preferably N-Methyl pyrrolidone.Used catalyst is palladium be main active ingredient, silver and ruthenium is auxiliary agent, aluminium sesquioxide is the catalyzer of carrier.Reaction pressure is 0.1 ~ 3.0MPaG, and temperature of reaction is 120 ~ 250 DEG C.It is 1.5MPaG that this example is preferably reaction pressure, and temperature of reaction is 150 DEG C.Gas passes into bottom acetylene hydrogenation reactor, by the bubbling of gas, catalyzer is suspended with slurry form in a solvent, reacts.Heat of reaction is removed by built-in heat exchanger.After reaction, gained gas phase sends into solvent absorbing tower.
After reaction, gained gas phase enters bottom solvent absorption tower, and solvent enters interchanger after solvent pump boosting, enters solvent absorbing top of tower through the cooled solvent of interchanger.Solvent and reaction gas counter current contact, absorb the byproduct of reaction in gas.Solvent is one or more of N-Methyl pyrrolidone, dimethyl formamide, dimethyl sulfoxide (DMSO), Monomethylamine and acetone.This example is preferably N-Methyl pyrrolidone.Absorption tower service temperature is-40 DEG C ~ 60 DEG C, and working pressure is 0.2 ~ 1.0MPaG.It is 40 DEG C that this example is preferably service temperature, and working pressure is 0.2MPaG.Solvent adopts fresh solvent, sealing and circulating.Interchanger adopts cold medium to be one or more in recirculated water, refrigerated water, liquefied ammonia, propylene, and this example is preferably recirculated water.
In the gas out of top, solvent absorption tower, main containing hydrogen and mixture of ethylene, after ethene concentrate is refining, obtain product ethene.Hydrogen and micro-by product return acetylene hydrogenation reactor recycle.Adopt the preferred PSA of concentrating method to be separated.
The by product that acetylene hydrogenation produces, delivers to solvent treatment tower through solvent absorbing tower bottom, carries out rectifying cutting to solvent.According to the difference with solvent boiling point, be referred to as light constituent and heavy constituent.The light constituent and heavy constituent impurity that contain in solvent is removed by rectifying cutting.Solvent treatment tower lateral line withdrawal function refine after solvent, be pumped to acetylene hydrogenation reactor recycling.Solvent treatment tower service temperature is-60 DEG C ~ 150 DEG C, and working pressure is-0.2MPaA ~ 1.5MPaG.This example is preferably service temperature 20 DEG C, working pressure 1.0MPaG.
Through long-time running, acetylene hydrogenation catalyst inactivation.Inactivation rear catalyst delivers to catalyst filtration device after stopping, and reclaims spent catalyst.Spent catalyst producer reclaims.The preferred pressure leaf filter of catalyst filtration device.Working pressure is preferably 0.5MPaG, and operation pressure reduction is preferably 0.2MPa, and service temperature is preferably 50 DEG C.
Embodiment 2
Enter acetylene cylinder from out-of-bounds acetylene, it is 0.02 ~ 0.2MPaG that acetylene enters acetylene cylinder pressure, and this example is preferably 0.15MPaG, and temperature be-20 ~ 40 DEG C, this example preferably-10 DEG C.Mixing with acetylene cylinder internal solvent is dissolved completely in solvent, and solvent is the one or more combination of N-Methyl pyrrolidone, dimethyl formamide, dimethyl sulfoxide (DMSO), Monomethylamine and acetone, and this example is preferably acetone.Solvent and acetylene throughput ratio 2 ~ 20:1 (mass ratio), this example is preferably 5:1.Solvent carries acetylene and after interchanger heating, send into acetylene hydrogenation reactor after pump boosting.Hydrogen to mix with acetylene at acetylene hydrogenation reactor entrance together sends into hydrogenator.Hydrogen feed temperature is 20 ~ 200 DEG C, and this example is preferably 40 DEG C.Feed pressure is 0.2 ~ 2.0MPaG, and this example is preferably 0.45MPaG.Acetylene solution mixes with hydrogen through venturi mixer, and hydrogen and acetylene throughput ratio are 2 ~ 10:1 (mol ratio), and this example is preferably 6:1.
Described acetylene hydrogenation reactor adopts paste state bed reactor, in-built solvent.Solvent is one or more of N-Methyl pyrrolidone, dimethyl formamide, dimethyl sulfoxide (DMSO), Monomethylamine and acetone.This example is preferably acetone.Used catalyst is palladium be main active ingredient, silver and ruthenium is auxiliary agent, aluminium sesquioxide is the catalyzer of carrier.Reaction pressure is 0.1 ~ 3.0MPaG, and temperature of reaction is 120 ~ 250 DEG C.It is 0.45MPaG that this example is preferably reaction pressure, and temperature of reaction is 150 DEG C.Gas passes into bottom acetylene hydrogenation reactor, by the bubbling of gas, catalyzer is suspended with slurry form in a solvent, reacts.Heat of reaction is removed by built-in heat exchanger.After reaction, gained gas phase sends into solvent absorbing tower.
After reaction, gained gas phase enters bottom solvent absorption tower, and solvent enters interchanger after solvent pump boosting, enters solvent absorbing top of tower through the cooled solvent of interchanger.Solvent and reaction gas counter current contact, absorb the byproduct of reaction in gas.Solvent is one or more of N-Methyl pyrrolidone, dimethyl formamide, dimethyl sulfoxide (DMSO), Monomethylamine and acetone.This example is preferably acetone.Absorption tower service temperature is-40 DEG C ~ 60 DEG C, and working pressure is 0.2 ~ 1.0MPaG.This example is preferably service temperature and is-5 DEG C, and working pressure is 0.2MPaG.Solvent adopts fresh solvent, sealing and circulating.Interchanger adopts cold medium to be one or more in recirculated water, refrigerated water, liquefied ammonia, propylene, and this example is preferably liquefied ammonia.
In the gas out of top, solvent absorption tower, main containing hydrogen and mixture of ethylene, after ethene concentrate is refining, obtain product ethene.Hydrogen and micro-by product return acetylene hydrogenation reactor recycle.Adopt the preferred PSA of concentrating method to be separated.
The by product that acetylene hydrogenation produces, delivers to solvent treatment tower through solvent absorbing tower bottom, carries out rectifying cutting to solvent.According to the difference with solvent boiling point, be referred to as light constituent and heavy constituent.The light constituent and heavy constituent impurity that contain in solvent is removed by rectifying cutting.Solvent treatment tower lateral line withdrawal function refine after solvent, be pumped to acetylene hydrogenation reactor recycling.Solvent treatment tower service temperature is-60 DEG C ~ 150 DEG C, and working pressure is-0.2MPaA ~ 1.5MPaG.This example is preferably service temperature 20 DEG C, working pressure 1.0MPaG.
Through long-time running, acetylene hydrogenation catalyst inactivation.Inactivation rear catalyst delivers to catalyst filtration device after stopping, and reclaims spent catalyst.Spent catalyst producer reclaims.The preferred pressure leaf filter of catalyst filtration device.Working pressure is preferably 0.5MPaG, and operation pressure reduction is preferably 0.2MPa, and service temperature is preferably 50 DEG C.
Embodiment 3
Enter acetylene cylinder from out-of-bounds acetylene, it is 0.02 ~ 0.2MPaG that acetylene enters acetylene cylinder pressure, and this example is preferably 0.15MPaG, and temperature be-20 ~ 40 DEG C, this example preferably-10 DEG C.Mixing with acetylene cylinder internal solvent is dissolved completely in solvent, and solvent is the one or more combination of N-Methyl pyrrolidone, dimethyl formamide, dimethyl sulfoxide (DMSO), Monomethylamine and acetone, and this example is preferably acetone.Solvent and acetylene throughput ratio 2 ~ 20:1 (mass ratio), this example is preferably 5:1.Solvent carries acetylene and after interchanger heating, send into acetylene hydrogenation reactor after pump boosting.Hydrogen to mix with acetylene at acetylene hydrogenation reactor entrance together sends into hydrogenator.Hydrogen feed temperature is 20 ~ 200 DEG C, and this example is preferably 40 DEG C.Feed pressure is 0.2 ~ 2.0MPaG, and this example is preferably 0.45MPaG.Acetylene solution mixes with hydrogen through venturi mixer, and hydrogen and acetylene throughput ratio are 2 ~ 10:1 (mol ratio), and this example is preferably 6:1.
Described acetylene hydrogenation reactor adopts paste state bed reactor, in-built solvent.Solvent is one or more of N-Methyl pyrrolidone, dimethyl formamide, dimethyl sulfoxide (DMSO), Monomethylamine and acetone.This example is preferably acetone.Used catalyst is palladium be main active ingredient, silver and ruthenium is auxiliary agent, aluminium sesquioxide is the catalyzer of carrier.Reaction pressure is 0.1 ~ 3.0MPaG, and temperature of reaction is 120 ~ 250 DEG C.It is 0.45MPaG that this example is preferably reaction pressure, and temperature of reaction is 150 DEG C.Gas passes into bottom acetylene hydrogenation reactor, by the bubbling of gas, catalyzer is suspended with slurry form in a solvent, reacts.Heat of reaction is removed by built-in heat exchanger.After reaction, gained gas phase sends into solvent absorbing tower.
After reaction, gained gas phase enters bottom solvent absorption tower, and solvent enters interchanger after solvent pump boosting, enters solvent absorbing top of tower through the cooled solvent of interchanger.Solvent and reaction gas counter current contact, absorb the byproduct of reaction in gas.Solvent is one or more of N-Methyl pyrrolidone, dimethyl formamide, dimethyl sulfoxide (DMSO), Monomethylamine and acetone.This example is preferably acetone.Absorption tower service temperature is-40 DEG C ~ 60 DEG C, and working pressure is 0.2 ~ 1.0MPaG.This example is preferably service temperature and is-5 DEG C, and working pressure is 0.2MPaG.Solvent adopts fresh solvent, sealing and circulating.Interchanger adopts cold medium to be one or more in recirculated water, refrigerated water, liquefied ammonia, propylene, and this example is preferably liquefied ammonia.
In the gas out of top, solvent absorption tower, main containing hydrogen and mixture of ethylene, after ethene concentrate is refining, obtain product ethene.Hydrogen and micro-by product return acetylene hydrogenation reactor recycle.Adopt the preferred PSA of concentrating method to be separated.
The by product that acetylene hydrogenation produces, delivers to solvent treatment tower through solvent absorbing tower bottom, carries out rectifying cutting to solvent.According to the difference with solvent boiling point, be referred to as light constituent and heavy constituent.The light constituent and heavy constituent impurity that contain in solvent is removed by rectifying cutting.Solvent treatment tower lateral line withdrawal function refine after solvent, be pumped to acetylene hydrogenation reactor recycling.Solvent treatment tower service temperature is-60 DEG C ~ 150 DEG C, and working pressure is-0.2MPaA ~ 1.5MPaG.This example is preferably service temperature 30 DEG C, working pressure 1.5MPaG.
Through long-time running, acetylene hydrogenation catalyst inactivation.Inactivation rear catalyst delivers to catalyst filtration device after stopping, and reclaims spent catalyst.Spent catalyst producer reclaims.The preferred pressure leaf filter of catalyst filtration device.Working pressure is preferably 0.5MPaG, and operation pressure reduction is preferably 0.2MPa, and service temperature is preferably 50 DEG C.
Embodiment 4
Enter acetylene cylinder from out-of-bounds acetylene, it is 0.02 ~ 0.2MPaG that acetylene enters acetylene cylinder pressure, and this example is preferably 0.15MPaG, and temperature be-20 ~ 40 DEG C, this example preferably-10 DEG C.Mixing with acetylene cylinder internal solvent is dissolved completely in solvent, and solvent is the one or more combination of N-Methyl pyrrolidone, dimethyl formamide, dimethyl sulfoxide (DMSO), Monomethylamine and acetone, and this example is preferably acetone.Solvent and acetylene throughput ratio 2 ~ 20:1 (mass ratio), this example is preferably 5:1.Solvent carries acetylene and after interchanger heating, send into acetylene hydrogenation reactor after pump boosting.Hydrogen to mix with acetylene at acetylene hydrogenation reactor entrance together sends into hydrogenator.Hydrogen feed temperature is 20 ~ 200 DEG C, and this example is preferably 40 DEG C.Feed pressure is 0.2 ~ 2.0MPaG, and this example is preferably 0.45MPaG.Acetylene solution mixes with hydrogen through venturi mixer, and hydrogen and acetylene throughput ratio are 2 ~ 10:1 (mol ratio), and this example is preferably 6:1.
Described acetylene hydrogenation reactor adopts paste state bed reactor, in-built solvent.Solvent is one or more of N-Methyl pyrrolidone, dimethyl formamide, dimethyl sulfoxide (DMSO), Monomethylamine and acetone.This example is preferably acetone.Used catalyst is palladium be main active ingredient, silver and ruthenium is auxiliary agent, aluminium sesquioxide is the catalyzer of carrier.Reaction pressure is 0.1 ~ 3.0MPaG, and temperature of reaction is 120 ~ 250 DEG C.It is 0.8MPaG that this example is preferably reaction pressure, and temperature of reaction is 150 DEG C.Gas passes into bottom acetylene hydrogenation reactor, by the bubbling of gas, catalyzer is suspended with slurry form in a solvent, reacts.Heat of reaction is removed by built-in heat exchanger.After reaction, gained gas phase sends into solvent absorbing tower.
After reaction, gained gas phase enters bottom solvent absorption tower, and solvent enters interchanger after solvent pump boosting, enters solvent absorbing top of tower through the cooled solvent of interchanger.Solvent and reaction gas counter current contact, absorb the byproduct of reaction in gas.Solvent is one or more of N-Methyl pyrrolidone, dimethyl formamide, dimethyl sulfoxide (DMSO), Monomethylamine and acetone.This example is preferably acetone.Absorption tower service temperature is-40 DEG C ~ 60 DEG C, and working pressure is 0.2 ~ 1.0MPaG.This example is preferably service temperature and is-5 DEG C, and working pressure is 0.8MPaG.Solvent adopts fresh solvent, sealing and circulating.Interchanger adopts cold medium to be one or more in recirculated water, refrigerated water, liquefied ammonia, propylene, and this example is preferably liquefied ammonia.
In the gas out of top, solvent absorption tower, main containing hydrogen and mixture of ethylene, after ethene concentrate is refining, obtain product ethene.Hydrogen and micro-by product return acetylene hydrogenation reactor recycle.Adopt the preferred PSA of concentrating method to be separated.
The by product that acetylene hydrogenation produces, delivers to solvent treatment tower through solvent absorbing tower bottom, carries out rectifying cutting to solvent.According to the difference with solvent boiling point, be referred to as light constituent and heavy constituent.The light constituent and heavy constituent impurity that contain in solvent is removed by rectifying cutting.Solvent treatment tower lateral line withdrawal function refine after solvent, be pumped to acetylene hydrogenation reactor recycling.Solvent treatment tower service temperature is-60 DEG C ~ 150 DEG C, and working pressure is-0.2MPaA ~ 1.5MPaG.This example is preferably service temperature-20 DEG C, working pressure 0.5MPaG.
Through long-time running, acetylene hydrogenation catalyst inactivation.Inactivation rear catalyst delivers to catalyst filtration device after stopping, and reclaims spent catalyst.Spent catalyst producer reclaims.The preferred pressure leaf filter of catalyst filtration device.Working pressure is preferably 0.5MPaG, and operation pressure reduction is preferably 0.2MPa, and service temperature is preferably 50 DEG C.
The apparatus structure of high density producing ethylene with acetylene hydrogenation of the present invention is simple, acetylene feeding pipe is connected with acetylene hydrogenation reactor by solvents for ethyne tank, acetylene is dissolved and passes into acetylene hydrogenation reactor more in a solvent, pressurizeed by liquid phase, overcome acetylene pressure restriction, acetylene hydrogenation can be made at more than 1.5MPaG pressure operation; Acetylene hydrogenation reactor is connected with solvent absorbing tower, and after acetylene hydrogenation reaction, gained gas phase is by solvent absorbing, and avoid multitower rectifying separation in traditional technology, energy consumption is low.The method technique of producing ethylene with acetylene hydrogenation of the present invention is simple, and raw material acetylene adopts the mode of dissolution with solvents, adopts acetylene liquid phase positive delivery, safer compared with pressurizeing with traditional acetylene in gas phase; Acetylene pressure is high pressure acetylene higher than 0.15MPaG, risk of very easily blasting, and therefore traditional technology seldom has acetylene high pressure operating mode; The method of producing ethylene with acetylene hydrogenation of the present invention can overcome acetylene pressure restriction, and acetylene hydrogenation can be made at more than 1.5MPaG pressure operation; Meanwhile, after hydrogenation reaction, tail gas is by solvent absorbing, avoids multitower rectifying separation in traditional technology, reduces energy consumption, and technique is advanced.The present invention finds a way out not only to the calcium carbide production capacity of China's surplus, and greatly alleviates China's ethylene requirements, has great importance to promotion China acetylene chemical industry Green Sustainable, energy-saving and emission-reduction.
Although illustrate and describe the present invention with specific embodiment, however it will be appreciated that can to make when not deviating from the spirit and scope of the present invention many other change and amendment.Therefore, this means to comprise all such changes and modifications belonged in the scope of the invention in the following claims.
Claims (10)
1. a device for high density producing ethylene with acetylene hydrogenation, is characterized in that, the device of described high density producing ethylene with acetylene hydrogenation comprises acetylene hydrogenation reactor, solvent absorbing tower and ethene concentration unit; Wherein, acetylene hydrogenation reactor, solvent absorbing tower are connected in turn with ethene concentration unit; Described acetylene hydrogenation reactor is connected with hydrogen feed pipeline with acetylene feeding pipe respectively; Described acetylene feeding pipe arranges solvents for ethyne tank; Described ethene concentration unit is connected with ethene discharging pipeline.
2. the device of a kind of high density producing ethylene with acetylene hydrogenation according to claim 1, is characterized in that, described acetylene feeding pipe is connected with bottom acetylene hydrogenation reactor respectively by venturi-type eductors with hydrogen feed pipeline.
3. the device of a kind of high density producing ethylene with acetylene hydrogenation according to claim 1, is characterized in that, the acetylene feeding pipe between described solvents for ethyne tank and acetylene hydrogenation reactor arranges interchanger.
4. the device of a kind of high density producing ethylene with acetylene hydrogenation according to claim 1, it is characterized in that, described acetylene hydrogenation reactor is connected with catalyst filtration device.
5. the device of a kind of high density producing ethylene with acetylene hydrogenation according to claim 1, is characterized in that, described solvent absorbing tower bottom sequentially passes through pump and is connected with solvent absorbing top of tower with interchanger.
6. the device of a kind of high density producing ethylene with acetylene hydrogenation according to claim 1, is characterized in that, described solvent absorbing tower is connected with solvent treatment tower; Described solvent treatment tower is connected with acetylene hydrogenation reactor.
7. the device of a kind of high density producing ethylene with acetylene hydrogenation according to claim 6, is characterized in that, described solvent treatment top of tower is connected with light constituent discharging pipeline; Described solvent treatment tower bottom is connected with heavy constituent discharging pipeline.
8. the device of a kind of high density producing ethylene with acetylene hydrogenation according to claim 7, is characterized in that, described solvent treatment top of tower sequentially passes through interchanger and is connected with light constituent discharging pipeline with return tank.
9. adopt the device of the arbitrary described a kind of high density producing ethylene with acetylene hydrogenation of claim 1-8 to carry out the method for producing ethylene with acetylene hydrogenation, it is characterized in that, comprise the steps:
Raw material acetylene and solvent, the solvent having dissolved acetylene enters acetylene hydrogenation reactor; Hydrogen directly enters acetylene hydrogenation reactor; Both generate ethene at reaction in acetylene hydrogenation reactor; Reaction gained gas phase is after solvent absorbing, and in gas phase, ethene and hydrogen are isolated to product ethene.
10. the method for a kind of producing ethylene with acetylene hydrogenation according to claim 9, is characterized in that, comprise the steps:
(1) acetylene hydrogenation:
Acetylene enters solvents for ethyne tank, mixes be dissolved completely in solvent with solvents for ethyne tank internal solvent, and solvent carries acetylene and after interchanger heating, send into acetylene hydrogenation reactor after pump boosting; Hydrogen to mix with acetylene at reactor inlet together sends into hydrogenator; After reaction, gained gas phase sends into solvent absorbing tower;
(2) solvent absorbing:
After acetylene hydrogenation reaction, gained gas phase enters bottom solvent absorption tower, and solvent enters interchanger after solvent pump boosting, enters top, absorption tower through the cooled solvent of interchanger; Gained gas phase counter current contact after solvent and acetylene hydrogenation react, absorbs the byproduct of reaction in gas phase;
(3) ethene concentrate:
From top, solvent absorption tower gas phase out after ethene concentration unit ethene concentrate is refining, obtain product ethene; Hydrogen returns acetylene hydrogenation reactor recycle;
(4) solvent treatment:
The by product that acetylene hydrogenation produces, delivers to solvent treatment tower through solvent absorbing tower bottom; Solvent treatment tower carries out rectifying cutting to solvent; According to the difference with solvent boiling point, be referred to as light constituent and heavy constituent; The light constituent, the heavy constituent impurity that contain in solvent is removed by rectifying cutting; Solvent treatment tower lateral line withdrawal function refine after solvent, be pumped to acetylene hydrogenation reactor recycling;
(5) catalyst recovery:
Through long-time running, acetylene hydrogenation catalyst inactivation; Inactivation rear catalyst delivers to catalyst filtration device after stopping, and reclaims spent catalyst.
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| CN105859498A (en) * | 2016-06-08 | 2016-08-17 | 北京神雾环境能源科技集团股份有限公司 | Reaction system and method for producing ethylene through catalyst regeneration |
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| CN105859500A (en) * | 2016-06-08 | 2016-08-17 | 北京神雾环境能源科技集团股份有限公司 | Ethylene preparation reaction system and method with vacuum solvent regeneration |
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| CN105906468A (en) * | 2016-06-08 | 2016-08-31 | 北京神雾环境能源科技集团股份有限公司 | Reaction system and method for preparing ethylene through regeneration of super gravity solvent |
| CN105859499B (en) * | 2016-06-08 | 2019-02-12 | 霍尔果斯道科特环能科技有限公司 | A kind of reaction system and method for producing ethylene with acetylene hydrogenation |
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| CN106944070A (en) * | 2017-02-27 | 2017-07-14 | 北京神雾环境能源科技集团股份有限公司 | A kind of synthesis of non-precious metal catalyst of high concentration preparation of ethylene through selective hydrogenation of acetylene and application process |
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