CN102336626A - Utilization method of waste gas discharged from butadiene extracting apparatus - Google Patents
Utilization method of waste gas discharged from butadiene extracting apparatus Download PDFInfo
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- CN102336626A CN102336626A CN2010102388615A CN201010238861A CN102336626A CN 102336626 A CN102336626 A CN 102336626A CN 2010102388615 A CN2010102388615 A CN 2010102388615A CN 201010238861 A CN201010238861 A CN 201010238861A CN 102336626 A CN102336626 A CN 102336626A
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Abstract
The invention discloses a utilization method of waste gas discharged from a butadiene extracting apparatus. According to the method, waste gas is subject to a reaction with hydrogen; alkyne in the waste gas is subject to a selective hydrogenation reaction, such that diolefins is produced; the reaction product is delivered back to the butadiene extracting apparatus, and 1,3-butadiene can be recovered. According to the invention, a compressor technology and a cold box technology are adopted, such that a problem of butadiene tail gas utilization difficulty is solved.
Description
Technical field
The present invention relates to a kind of petrochemical complex waste gas and recycle the field, particularly relate to the method that a kind of BEU is rich in the exhaust gas utilization of alkynes.
Background technology
When ethylene cracker coproduction carbon four hydrocarbon, the 1,3-butadiene in the cracking c_4 hydrocarbon is generally made with extra care through the method for direct rectifying through two sections SX rectifying again, and the residual gas that this refining plant produces is commonly called as divinyl tail gas.Extracting rectifying is also named extracting, and the retrieving arrangement of divinyl generally is BEU.Alkynes concentration is higher in the divinyl tail gas, generally greater than 20 weight %, and the highest 40 weight % that surpass.These waste gas that are rich in alkynes still do not have industrial utilization at present and are worth, and can only send torch burning to handle.Because high density alkynes is prone to the polymerization blast, just can send torch burning after therefore must diluting with the raffinate that contains butane, butylene earlier, so just cause the very big wasting of resources.Along with the increasing of hydrocarbon vapours cracking severity in recent years, alkynes content is in rising trend in the cracking c_4, and the tail gas amount that is rich in alkynes that BEU produces also increases considerably.If with the tail gas recycle utilization of being rich in alkynes in these waste gas, will improve the economic benefit of ethylene cracker greatly.
At present, method commonly used comprises following several kinds in the prior art:
A kind of method is before cracking c_4 gets into BEU, it to be selected hydrogenation, and alkynes content is reduced, and contains the alkynes exhaust gas discharging with minimizing.
Another kind method is that the described divinyl tail gas that is rich in the alkynes cut is selected hydrogenation, and alkynes is converted into divinyl and monoolefine, sends BEU again back to, to reclaim divinyl wherein.CN101434508 discloses the selection method of hydrotreating of the height unsaturated hydrocarbons in a kind of C-4-fraction; With the salvage stores that is rich in alkynes that obtains after the divinyl extracting is raw material; In the presence of catalyzer, adopt fixed-bed reactor, select hydrogenation to obtain 1; The 3-divinyl sends back to extraction plant with reaction product again.The operational condition that hydrogenation technique adopts is: temperature of reaction is 30～9 ℃, and reaction pressure is 1.0～4.0MPa, and the liquid air speed is 7～20h
-1Catalyzer is the palladium series catalyst of carrier with the aluminum oxide, and specific surface area is 50～150m
2/ g, specific pore volume are 0.25～1.0ml/g.Adopt the method for this invention effectively to utilize, reduce the wasting of resources for the rich alkynes salvage stores after the divinyl extracting.But the defective of above-mentioned prior art is:
1. this method does not solve the charging problem of reactor drum.Because hydrogenation reaction is liquid phase reaction, pressure is between 1.5～4.0MPa, and divinyl tail gas is gas phase, and pressure is near normal pressure, and how the raw material of gas phase being boosted, to send into reactor drum be a technical barrier;
2 owing to the concentration of alkynes in the material and divinyl is high, and polymerization is blasted easily, and how under the premise that security is guaranteed material to be boosted is the key of dealing with problems.
Summary of the invention
For solving the divinyl tail gas difficulty liquefaction that exists in the prior art, the problem that difficulty is boosted, the invention provides a kind of method of utilizing of BEU waste gas, through adopting the technology of compressor and ice chest, solved the difficult problem of divinyl waste gas utilization.
The method of utilizing that the purpose of this invention is to provide a kind of BEU waste gas; Adopt following technical scheme: the composition of described waste gas comprises butylene 0～10 weight %; Divinyl 30～70 weight %, ethylacetylene and vinylacetylene 20～50 weight %, this method reacts described extraction plant waste gas and hydrogen; Make the selective acetylene hydrocarbon hydrogenation in the described waste gas generate diolefin, its step comprises:
(1) boost, condensation: divinyl tail gas raw material boosts for one section through off-gas compressor, and the divinyl tail gas after boosting gets into ice chest as hot logistics, after heat exchange, is condensed into liquid phase carbon four;
(2) hydrogenation reaction: mix with recycle stream from reaction product from liquid phase carbon four logistics of step (1); After boosting pump boosts, allocate hydrogen into and be sent to hydrogenator, hydrogenation takes place in the reactor drum to select; Alkynes and hydrogen reaction generate diolefin; Be divided into two strands after hydrogenator outlet product is cooled to normal temperature, one is as recycle diffluence hydrogenator inlet, and one sees the battery limit (BL) off as reactor product;
(3) refrigeration system: adopt independent refrigeration system, provide the cryogen of specified temp to get into the ice chest heat exchange, for C 4 materials provides cold as cold logistics; Especially, two sections that have utilized off-gas compressor for cryogen boosts, cryogen recycle after compression, cooling, heat exchange.
In the concrete enforcement:
Off-gas compressor described in step (1), (3) adopts is with two sections compressor for compressing; Every section system that is respectively different boosts, and one section on compressor is for the waste gas raw material boosts, and two sections on compressor boosts for the cryogen of refrigeration system; Two systems are independent of each other, and have improved the safety of device operation.
The top hole pressure that off-gas compressor described in the step (1) is one section is 0.15～0.18MPa (absolute pressure, as follows), and temperature is 50～70 ℃.
Divinyl tail gas described in the step (1) is after the ice chest heat exchange, and temperature is 4～9 ℃, and divinyl tail gas all is condensed into liquid phase under this temperature.
In the described step (2), described hydrogenation reaction is a selective hydrogenation reaction, and carbon four alkynes and hydrogen reaction generate 1,3-butadiene, and reaction product is returned BEU again to reclaim 1,3-butadiene.
Mixture in the said step (2) adopts boosting pump to boost to 1.5～5.5MPa.
Said hydrogenator in the step (2) is one-stage hydrogenation or multistage hydrogenation.
Refrigeration system purpose described in the step (3) is that 0～4.0 ℃ cryogen is provided for divinyl tail gas; Cryogen can adopt any cryogens that are applicable to this operating mode such as propylene, carbon four components; Preferred carbon four components that adopt are the logistics of carbon four like any staples such as carbon four, cracking c_4 behind butane, butylene, the ether.
Especially, compressor described in the step (3) adopts two sections of off-gas compressor, promptly adopts a compressor, boosts for the waste gas raw material simultaneously and boosts for the cryogen of cooling system.The top hole pressure that compressor is two sections is 0.4～1.0MPa.
In claims and specification sheets, if do not particularly point out, unit " % " is meant weight percent content.
In concrete implementation process:
In the said step (1), off-gas compressor one section outlet pressure is in 0.15～0.2MPa (absolute pressure), and temperature gets into the ice chest heat exchange at 50～70 ℃, 4～9 ℃ of ice chest temperature outs, and waste gas all is condensed into liquid phase.This waste gas boosts, the operating parameters of process of cooling is all in the safety range that allows.
In described step (2), adopt and select hydrogenation technique, the carrier of catalyzer is an aluminum oxide; The main active ingredient of load is selected from one or both of Pt, Pd; Content is 0.01～1.0%, and the active ingredient that helps of load is Cu, and content is 0.01～5.0%; Be selected from least a among Ag, Mo, Ni, the Co simultaneously in addition, content is 0.01～5.0%.
In described step (2), reactor inlet temperature is 20～100 ℃, is preferably 20～6 ℃; Reaction pressure is 1.0～5.0MPa; The mol ratio of hydrogen and alkynes is generally 0.8～3.0, is preferably 1.2～2.5; The liquid phase volume air speed is 1～30h
-1, be preferably 10～25h
-1Recycle stream be 1～25: 1 from the liquid phase stream mass flux ratio of step (1), be preferably 5～15: 1.
Cryogen in the said step (3) preferably adopts carbon four components, and it mainly consists of butane and butylene, and butane content is 1～50%, butylene 10～90%, and both summations are not more than 100%; Compressor second stage exit pressure is 0.4～1.0MPa.
As required, moisture eliminator can be set to remove moisture wherein before the hydrogenator of described step (2); Described moisture eliminator adopts molecular sieve desiccant or alumina desiccant.Also can adopt coalescer to remove moisture, coalescer is a standard equipment, can select for use according to actual.
BEU waste gas of the present invention utilize method except the liquefaction that solved waste gas, the problem of boosting, also have following characteristics:
1. in the traditional technology, more the divinyl tail gas that is rich in alkynes of extraction plant acts as a fuel and burns, and the present invention generates 1,3-butadiene with the selective acetylene hydrocarbon hydrogenation in the waste gas, returns extraction plant again and reclaims divinyl wherein, has high economic benefit;
2. in the traditional technology, just can be sent to torch after needing one raffinate that the hydrocarbon mixture that is rich in alkynes is diluted, what the raw material among the present invention can directly adopt extraction plant contains alkynes waste gas, need not to have practiced thrift a large amount of butane, butylene with the raffinate dilution again;
3. only adopt a compressor, not only realized the waste gas raw material is boosted, and can save facility investment greatly simultaneously for the cryogen of cooling system boosts;
4. flow process of the present invention is simple, number of devices is few, adaptability to raw material is strong, less investment.
Description of drawings
Fig. 1 BEU waste gas of the present invention utilize the method process flow diagram.
Nomenclature:
1 waste gas, 2 compression back waste gas; 3 liquid phase carbon four; 4 reaction raw materials; 5 hydrogen; 6 reaction product; 7 recycle streams; 8 inlet cryogens; 9 outlet cryogens; 10 compressor outlets; Aforementioned 1～10 symbol also is used for representing the thing stream number of subordinate list;
11 compressors; 12 ice chests; 13 reactor drums.
Embodiment
Below in conjunction with embodiment, further specify the present invention.
Embodiment 1
1. boost: from the waste gas 1 of BEU (the main composition: butylene 7.82%, divinyl 43.76%, ethylacetylene and vinylacetylene 47.1% are the quality percentage composition), flow 1080kg/h, pressure 0.1MPa (absolute pressure, as follows).Waste gas gets into a section of compressor 11, and the pressure of compressor outlet exhaust gas stream 2 is 64.3 ℃ of 0.17MPa, temperature, and waste gas gets into the ice chest heat exchange and changes liquid phase into, and the pressure of ice chest outlet liquid phase carbon 43 is 5.1 ℃ of 0.14MPa, temperature;
2. reaction: liquid phase carbon 43 gets into mixing tank through dehydration back, mixes with recycle stream 7 from hydrogenation products, and the flow of recycle stream is 8640kg/h, after boosting pump boosts, allocates a certain amount of hydrogen 5 into, and entering reactor drum 13 reacts.Reaction conditions is: 40 ℃ of temperature, pressure 2.0MPa, hydrogen/alkynes mol ratio 1.5, liquid phase volume air speed 15h
-1, the intersegmental water recirculator of establishing is cooled to 40 ℃ with reactor outlet material, and reaction product is divided into two strands, and one returns mixing tank for recycle stream 7, and one sees the battery limit (BL) off as reaction product 6, and flow is 1108kg/h; The activity of such catalysts component is Pb, and content is 0.2%, and helping active ingredient is Cu2.1%, Ni0.15%.
3. refrigeration system: adopting carbon four components is cryogen, and it mainly consists of butane 90.7%, butylene 9.3%, boosts to 0.5MPa through two sections of off-gas compressor 11; The cooling of employing recirculated water; The 0.115MPa that reduces pressure, temperature is 2.2 ℃, gets into ice chest and the heat exchange of waste gas raw material as cold flow; The ice chest temperature out is 2.4 ℃, recycle after compressor boosts again.
The quality group of each main streams becomes to see the following form 1.
| The thing stream number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Temperature ℃ | 40 | 64.3 | 5.1 | 40 | 25 | 40 | 40 | 2.2 | 2.4 | 68.3 |
| Pressure MPa | 0.105 | 0.17 | 0.14 | 2 | 3 | 2 | 2 | 0.115 | 0.115 | 0.5 |
| Mass rate kg/h | 1080 | 1080 | 1080 | 9720 | 28 | 1108 | 8640 | 2994 | 2994 | 2002 |
| Mass fraction % | ||||||||||
| Hydrogen | 0 | 0 | 0 | 0 | 70 | 0 | 0 | 0 | 0 | 0 |
| Methane | 0 | 0 | 0 | 0.7 | 30 | 0.7 | 0.7 | 0 | 0 | 0 |
| Butane | 1.32 | 1.32 | 1.32 | 3.2 | 0 | 3.5 | 3.5 | 9.3 | 9.3 | 9.3 |
| Butylene | 7.82 | 7.82 | 7.82 | 59 | 0 | 61.4 | 61.4 | 90.7 | 90.7 | 90.7 |
| 1,3-butadiene | 41.8 | 41.8 | 41.8 | 31 | 0 | 31.3 | 31.3 | 0 | 0 | 0 |
| 1 | 1.92 | 1.92 | 1.92 | 2.2 | 0 | 2.2 | 2.2 | 0 | 0 | 0 |
| Ethylacetylene | 8.1 | 8.1 | 8.1 | 0.6 | 0 | 0 | 0 | 0 | 0 | 0 |
| Vinylacetylene | 37.9 | 37.9 | 37.9 | 2.4 | 0 | 0 | 0 | 0 | 0 | 0 |
| Carbon five | 1.14 | 1.14 | 1.14 | 0.6 | 0 | 0.6 | 0.6 | |||
| Carbon eight | 0.3 | 0 | 0.3 | 0.3 |
Claims (12)
- A BEU waste gas utilize method, comprise the steps:(1) boost, condensation: divinyl tail gas raw material boosts for one section through off-gas compressor, and the divinyl tail gas after boosting gets into ice chest as hot logistics, after heat exchange, is condensed into liquid phase carbon four;(2) hydrogenation reaction: mix with recycle stream from reaction product from liquid phase carbon four logistics of step (1); After boosting pump boosts, allocate hydrogen into and be sent to hydrogenator, hydrogenation takes place in the reactor drum to select; Alkynes and hydrogen reaction generate diolefin; Be divided into two strands after hydrogenator outlet product is cooled to normal temperature, one is as recycle diffluence hydrogenator inlet, and one sees the battery limit (BL) off as reactor product;(3) refrigeration system: provide cryogen to get into the ice chest heat exchange, for C 4 materials provides cold as cold logistics; Cryogen recycle after compression, cooling, heat exchange;Wherein off-gas compressor described in step (1), (3) adopts and to be with two sections compressor for compressing, and every section system that is respectively different boosts, and one section on compressor is for the waste gas raw material boosts, and two sections on compressor is for the cryogen of refrigeration system boosts, and two systems are independent of each other.
- 2. according to the method for utilizing of claim 1, wherein the top hole pressure of one section of off-gas compressor described in the step (1) is 0.15～0.18MPa, and temperature is 50～70 ℃.
- 3. according to the method for utilizing of claim 1, wherein the divinyl tail gas described in the step (1) is after the ice chest heat exchange, and temperature is 4～9 ℃.
- 4. according to the method for utilizing of claim 1, in the wherein said step (2), described hydrogenation reaction is a selective hydrogenation reaction, and carbon four alkynes and hydrogen reaction generate 1,3-butadiene, and reaction product is returned BEU again to reclaim 1,3-butadiene.
- 5. according to the method for utilizing of claim 1, the mixture in the wherein said step (2) adopts boosting pump to boost to 1.5～5.5MPa.
- 6. according to the method for utilizing of claim 1, wherein before the hydrogenator moisture eliminator is set described in the step (2), said moisture eliminator adopts molecular sieve desiccant or alumina desiccant, perhaps adopts coalescer.
- 7. according to the method for utilizing of claim 1, wherein the hydrogenator in the step (2) is one-stage hydrogenation or multistage hydrogenation.
- 8. according to the method for utilizing of claim 1, wherein cryogen adopts carbon four components in the step (3), is the logistics of carbon four like any staples such as carbon four, cracking c_4 behind butane, butylene, the ether.
- 9. according to the method for utilizing of claim 1, wherein two sections of the employing of the compressor described in the step (3) off-gas compressor, the top hole pressure that compressor is two sections is 0.4～1.0MPa.
- 10. according to the method for utilizing of claim 1, wherein in described step (2), reactor inlet temperature is 20～100 ℃, is preferably 20～6 ℃; Reaction pressure is 1.0～5.0MPa; The mol ratio of hydrogen and alkynes is generally 0.8～3.0, is preferably 1.2～2.5; The liquid phase volume air speed is 1～30h -1, be preferably 10～25h -1Recycle stream be 1～25: 1 from the liquid phase stream mass flux ratio of step (1), be preferably 5～15: 1.
- 11. according to the method for utilizing of claim 1, the cryogen in the wherein said step (3) adopts carbon four components, it mainly consists of butane and butylene, and butane content is 1～50%, butylene 10～90%, and both summations are not more than 100%; Compressor second stage exit pressure is 0.4～1.0MPa.
- 12. according to the method for utilizing of claim 1, the composition of wherein said waste gas comprises butylene 0～10 weight %, divinyl 30～70 weight %, ethylacetylene and vinylacetylene 20～50 weight %.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103787812A (en) * | 2012-10-30 | 2014-05-14 | 中国石油化工股份有限公司 | Butadiene tail gas hydrogenation system and hydrogenation method |
| US9566548B2 (en) | 2015-06-24 | 2017-02-14 | International Business Machines Corporation | Butadiene sequestration via sulfur dioxide charged zeolite beds |
| WO2022089250A1 (en) * | 2020-10-26 | 2022-05-05 | 中国石油化工股份有限公司 | Method for selective hydrogenation of butadiene extraction tail gas and selective hydrogenation apparatus |
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| CN1590513A (en) * | 2003-08-26 | 2005-03-09 | 中国石化集团齐鲁石油化工公司 | Selective hydrogenation technology of hydrocarbon material flow rich acetylene in hydrocarbon |
| WO2005037396A1 (en) * | 2003-10-20 | 2005-04-28 | Polski Koncern Natfowy Orlen Spolka Akcyjna | Butadiene recovery process |
| CN101189483A (en) * | 2005-03-04 | 2008-05-28 | 林德股份公司 | Method for liquefaction of a stream rich in hydrocarbons |
| CN101413749A (en) * | 2008-11-20 | 2009-04-22 | 成都赛普瑞兴科技有限公司 | Method and apparatus for single-stage mixing cryogen refrigerating cycle liquefied natural gas |
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2010
- 2010-07-28 CN CN201010238861.5A patent/CN102336626B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1590513A (en) * | 2003-08-26 | 2005-03-09 | 中国石化集团齐鲁石油化工公司 | Selective hydrogenation technology of hydrocarbon material flow rich acetylene in hydrocarbon |
| WO2005037396A1 (en) * | 2003-10-20 | 2005-04-28 | Polski Koncern Natfowy Orlen Spolka Akcyjna | Butadiene recovery process |
| CN101189483A (en) * | 2005-03-04 | 2008-05-28 | 林德股份公司 | Method for liquefaction of a stream rich in hydrocarbons |
| CN101413749A (en) * | 2008-11-20 | 2009-04-22 | 成都赛普瑞兴科技有限公司 | Method and apparatus for single-stage mixing cryogen refrigerating cycle liquefied natural gas |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103787812A (en) * | 2012-10-30 | 2014-05-14 | 中国石油化工股份有限公司 | Butadiene tail gas hydrogenation system and hydrogenation method |
| CN103787812B (en) * | 2012-10-30 | 2016-03-30 | 中国石油化工股份有限公司 | A kind of divinyl tail gas hydrogenation system and method for hydrotreating |
| US9566548B2 (en) | 2015-06-24 | 2017-02-14 | International Business Machines Corporation | Butadiene sequestration via sulfur dioxide charged zeolite beds |
| US9895656B2 (en) | 2015-06-24 | 2018-02-20 | International Business Machines Corporation | Butadiene sequestration via sulfur dioxide charged zeolite beds |
| US10105646B2 (en) | 2015-06-24 | 2018-10-23 | International Business Machines Corporation | Butadiene sequestration via sulfur dioxide charged zeolite beds |
| WO2022089250A1 (en) * | 2020-10-26 | 2022-05-05 | 中国石油化工股份有限公司 | Method for selective hydrogenation of butadiene extraction tail gas and selective hydrogenation apparatus |
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