CN104610007B - A kind of system and method for Oxidative Dehydrogenation of Butene into Butadiene - Google Patents
A kind of system and method for Oxidative Dehydrogenation of Butene into Butadiene Download PDFInfo
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- CN104610007B CN104610007B CN201310544346.3A CN201310544346A CN104610007B CN 104610007 B CN104610007 B CN 104610007B CN 201310544346 A CN201310544346 A CN 201310544346A CN 104610007 B CN104610007 B CN 104610007B
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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
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Abstract
The invention discloses the system and method for a kind of Oxidative Dehydrogenation of Butene into Butadiene.System arranges butylene vapourizing unit and reaction gas preheating device, and butylene vapourizing unit includes: butylene evaporator and butylene vaporizer, and reaction gas preheating device includes butylene heater and air heater；After air cushioning tank connects air heater, pipeline is divided into three, connects I section reactor, II section reactor, the entrance of III section reactor respectively；After butylene evaporator connects butylene heater, pipeline is divided into three, connects I section reactor, II section reactor, the entrance of III section reactor respectively.Make C4It is mixed into reactor with water vapour or generation gas again after being first preheating to certain temperature with air, restrained effectively aldehydes Organic substance and polycondensation reaction occurs because of Quench, reduce coking and the occurrence probability of carbon distribution of catalyst, thus extend regeneration period and the service life of catalyst, and then reduce running cost, improve economic benefit.
Description
Technical field
The present invention relates to butadiene production field, furtherly, relate to a kind of Oxidative Dehydrogenation of Butene fourth
The system and method for diene.
Background technology
Butadiene is a kind of important basic petrochemical Organic Ingredients and synthetic rubber monomer, at petrochemical industry alkene
Status in hydrocarbon feed is only second to ethylene and propylene, the most industrial mainly by three kinds of solvent extraction rectification
Method, from the mixing C of preparing ethylene by steam cracking by-product4In fraction, extracting obtains product butadiene, and they divide
Not being acetonitrile method, DMF method and NMP method, these three method has low cost and pollutes little economic advantages,
But it is as light hydrocarbon cracking, ethane dehydrogenation, C1The research and development of the new Ethylene Technologies such as raw material ethylene and pushing away
Wide application, in ethylene production, the butadiene of by-product will be difficult to meet the market demand of sustainable growth.Meanwhile, for
Further to C after ether4In butylene be used and improve whole plant economic benefit, use butylene oxidation-dehydrogenation
The technology of method butadiene get further promotion and application, and obtain swift and violent development in the recent period, but
It is the feature that method has energy consumption height, pollution is heavy and the operation cycle is short of Oxidative Dehydrogenation of Butene into Butadiene, special
Be not regeneration period of catalyst in reactor be the system determining oxidative dehydrogenation butadiene product equipment cycle of operation
About factor, and also directly influence running cost and the economic benefit of device the service life of catalyst, and
The key factor of the regeneration period and service life that affect catalyst is to generate containing aldehydes Organic substance in gas, raw
When becoming gas to mix with air or butylene, owing to air or butylene temperature are relatively low, aldehydes Organic substance is because of Quench
Polycondensation reaction occurs, and it is long-pending that the product of polycondensation can be attached in catalyst surface or space cause catalyst to occur
Carbon or coking and blocking catalyst so that the specific surface area of catalyst is greatly reduced, thus causes catalyst
Activity or reaction selectivity are greatly reduced.The document investigated by reality and consult is found, actual fortune
The catalyst regeneration cycle that the oxidative dehydrogenation butadiene product equipment of row or patented invention are mentioned substantially can only maintain
About 3 months, some oxidative dehydrogenation butadiene product equipment catalyst regeneration cycle only had 45 days, even 1
The moon is less than.Have been reported that and claim and can extend to 6 months, but actually sacrifice reactivity and selection
Property, i.e. do not ensure that the activity and selectivity of 6 months rear catalysts is the most constant.Because the regeneration period is short,
Correspondingly catalyst service life also can only maintain one to two regeneration periods, the most only about 12 months.
Some device, in order to improve conversion ratio and the device yield of butylene, uses the butylene of high concentration to react, and
This high concentration butene reaction necessarily causes generating the too high polymer under the high temperature conditions of butadiene concentration in gas
Abruptly increase and cause catalyst generation carbon distribution to affect catalyst regeneration cycle and service life, also result in simultaneously
The amount of by-product and kind too much affect subsequent production system, and this catalyst regeneration cycle is short and uses
Life-span short critical defect directly affects the running cost of device, thus affects economic benefit.
Summary of the invention
For solving problems of the prior art, the invention provides a kind of Oxidative Dehydrogenation of Butene into Butadiene
System and method., by controlling to enter the C of reactor4In butene concentration, and the vaporization of butylene is set
Device so that containing the C of butylene4Enter reactor with gas phase state, a pre-hot charging of reaction gas is set simultaneously
Put so that C4It is mixed into reaction with water vapour or generation gas again after being first preheating to certain temperature with air
Device, controls to enter the water alkene ratio of reactor, oxygen alkene ratio and feeding temperature, restrained effectively aldehydes Organic substance
There is polycondensation reaction because of Quench, and be effectively reduced coking and the carbon distribution occurrence probability of catalyst, thus
Extend regeneration period and the service life of catalyst, and then reduce the behaviour of oxidative dehydrogenation butadiene systems
Make cost, and substantially increase the economic benefit of system.
An object of the present invention is to provide the system of a kind of Oxidative Dehydrogenation of Butene into Butadiene.
Including:
Described system arranges butylene vapourizing unit and reaction gas preheating device,
Butylene vapourizing unit includes: butylene evaporator and butylene vaporizer, and butylene vaporizer is arranged on butylene evaporation
Pot bottom；
Described reaction gas preheating device includes butylene heater and air heater；
After air cushioning tank connects air heater, pipeline is divided into three, connects I section reactor, II respectively
Section reactor, the entrance of III section reactor；
After butylene evaporator connects butylene heater, pipeline is divided into three, connects I section reactor, II respectively
Section reactor, the entrance of III section reactor.
The two of the purpose of the present invention are to provide a kind of method of Oxidative Dehydrogenation of Butene into Butadiene.
Including:
1) air is heated by the air device the most again and is preheating to temperature is 150～300 DEG C, liquid phase C4Charging
Being preheating to temperature through butylene heater again after vaporization is 150～300 DEG C；
2) air and C4Being respectively classified into three strands, one steams with the water after two-stage reaction outlet heat exchanger heat exchange
Vapour is mixed into I section reactor, and one is mixed into II section with I section outlet generation gas after heat exchange and reacts
Device, one is mixed into III section reactor with II section outlet generation gas after heat exchange；
3) water vapour sequentially passes through I section reacting replacing heat device and II section reacting replacing heat device, exports with two reactor
High temperature generate after gas carries out heat exchange, then entrance I section reactor after mix with the air after preheating and butylene；
Under the effect of catalyst, carry out oxidative dehydrogenation generate containing 1,3-butadiene, C4Alkynes and furan, aldehyde,
Acid, CO2, the generation gas of CO.
The present invention controls to enter the C of reactor4In butene concentration, and a butylene vapourizing unit is set, makes
Must be containing the C of butylene4Enter reactor with gas phase state, a reaction gas preheating device be set simultaneously so that
C4It is mixed into reactor, especially with water vapour or generation gas again after being first preheating to certain temperature with air
It is that II and III section reactor feed, butylene and air mix at the generation gas with I section and II section reactor outlet
Before, it is mixed into II section and III section reactor with generation gas again after being first preheating to certain temperature.
Specifically can be by the following technical solutions:
Air is heated by the air device again after compressor pressurizes and is preheating to certain temperature, and liquid phase butylene is through butylene vapour
It is preheating to certain temperature, air and butylene through butylene heater again after change be respectively classified into according to certain ratio
Three strands, one is mixed into I section reactor with the water vapour after two-stage reaction outlet heat exchanger heat exchange,
One is mixed into II section reactor with I section outlet generation gas after heat exchange, and one exports with II section
Generation gas after heat exchange is mixed into III section reactor, water vapour sequentially pass through I section reacting replacing heat device and
II section reacting replacing heat device, generates after gas carries out heat exchange with the high temperature of two reactor outlet, then with preheating after
Air and butylene enter I section reactor according to after certain ratio mixing.Oxygen is carried out under the effect of catalyst
Fluidized dehydrogenation reaction generates containing 1,3-butadiene, C4Alkynes and furan, aldehyde, acid, CO2, the by-product such as CO
Generate gas.
Described C4In charging, butene concentration is 60%～100% (percentage by weight), preferably 75%～90%；
The operation pressure of described butylene vaporizer and butylene evaporator is 0.2～0.35MPag, and operation temperature is
30～50 DEG C.
The described C containing butylene4Being preheated to temperature respectively with air is 150～300 DEG C, preferably
200～250 DEG C；
Described entrance I section reactor, II section reactor, the C of III section reactor4, air and water vapour
Charging, total water alkene mol ratio is 6～20, preferably 10～15, total oxygen alkene mol ratio 0.1～1, preferably 0.5～0.8；
Described C4Entrance I section reactor, II section reactor, III section reactor ratio are 3～2:2～1:
1～0.5,
Described air enters I section reactor, II section reactor, the ratio of III section reactor are
2～1:1.5～0.8:1～0.5；
Described I section reactor reaction gas entrance feeding temperature is 300～400 DEG C,
Described II section reactor reaction gas entrance feeding temperature is 300～400 DEG C,
Described III section reactor reaction gas entrance feeding temperature is 300～400 DEG C；
Described butylene carburetion system is set and reaction gas pre-heating system be equally applicable to use one section or two-stage nitration or
Multistage Oxidative Dehydrogenation of Butene into Butadiene device or technology.
The invention have the characteristics that
By controlling to enter the C of reactor4In butene concentration, and a butylene vapourizing unit is set so that
C containing butylene4Enter reactor with gas phase state, a reaction gas preheating device is set so that C simultaneously4
After being first preheating to certain temperature with air again with water vapour or generate gas be mixed into reactor, control into
Enter the water alkene ratio of reactor, oxygen alkene ratio and feeding temperature, restrained effectively aldehydes Organic substance because of Quench
There is polycondensation reaction, and be effectively reduced the coking of catalyst and the occurrence probability of carbon distribution, thus extend and urge
The regeneration period of agent and service life, and then reduce the running cost of oxidative dehydrogenation butadiene systems,
And substantially increase the economic benefit of system.
Accompanying drawing explanation
The system schematic of the Oxidative Dehydrogenation of Butene into Butadiene of Fig. 1 present invention
Description of reference numerals:
1-air, 2-compressor, 3-air cushioning tank, 4-air heater, 5-III section air feed, 6-II
Section air feed, 7-I section air feed, 8-I section reactor, 9-II section reactor, 10-III section reactor,
11-I section reactor outlet generates gas, 12-I section outlet heat exchanger, and 13-I section exports the generation gas after heat exchange,
14-II section reactor outlet generates gas, 15-II section outlet heat exchanger, and 16-II section exports the generation gas after heat exchange,
17-III section reactor outlet generates gas, 18-water vapour, the water vapour after the outlet heat exchange of 19-I section, 20-II section
Water vapour after outlet heat exchange, 21-liquid phase C4, 22-butylene evaporator, 23-gas phase butylene, 24-butylene steams
Sending out device, 25-butylene heater, 26-I section butene feed, 27-II section butene feed, 28-III section butylene enters
Material
Detailed description of the invention
Below in conjunction with embodiment, further illustrate the present invention.
Embodiment:
Example 1
As it is shown in figure 1, the system of 100,000 tons/year of Oxidative Dehydrogenation of Butene into Butadienes.
Described system arranges butylene vapourizing unit and reaction gas preheating device,
Butylene vapourizing unit includes: butylene evaporator and butylene vaporizer, and butylene vaporizer is arranged on butylene evaporation
Pot bottom；
Described reaction gas preheating device includes butylene heater and air heater；
After air cushioning tank connects air heater, pipeline is divided into three, connects I section reactor, II respectively
Section reactor, the entrance of III section reactor；
After butylene evaporator connects butylene heater, pipeline is divided into three, connects I section reactor, II respectively
Section reactor, the entrance of III section reactor.
Air is heated by the air device again after compressor pressurizes and is preheating to 230 DEG C, liquid phase C4After butylene vaporizes
Being preheating to 230 DEG C through butylene heater again, air and butylene are respectively classified into three strands according to certain ratio, C4
The ratio entering three sections of reactors is 2:1:1, and it is 1:1:1 that air enters the ratio of three sections of reactors；One
Stock is mixed into I section reactor, one and I with the water vapour after two-stage reaction outlet heat exchanger heat exchange
Section outlet generation gas after heat exchange is mixed into II section reactor, and one exports through heat exchange with II section
After generation gas be mixed into III section reactor, low pressure water vapor sequentially passes through I section reacting replacing heat device and II
Section reacting replacing heat device, generates after gas carries out heat exchange with the high temperature of two reactor outlet, then with preheating after sky
Gas and butylene enter I section reactor according to after certain ratio mixing.Aoxidize under the effect of catalyst
Dehydrogenation reaction generates containing 1,3-butadiene, C4Alkynes and furan, aldehyde, acid, CO2, the life of the by-product such as CO
Become gas.
Butene concentration in C4 charging is 85%wt,
The operation pressure of butylene vaporizer and butylene evaporator is 0.25MPag, and operation temperature is 35 DEG C,
Enter the C of three sections of reactors4, air and water vapour charging, total water alkene mol ratio is 10, total oxygen
Alkene mol ratio is 0.6,
I section reactor reaction gas entrance feeding temperature is 350 DEG C,
II section reactor reaction gas entrance feeding temperature is 355 DEG C,
III section reactor reaction gas entrance feeding temperature is 365 DEG C；
Reactor vapor consumption is: 45 ton hour
Example 2:
1. as flow process is with example 1；
2. enter the C of three sections of reactors4, air and water vapour charging, total water alkene mol ratio is 8, total
Oxygen alkene mol ratio is 0.40；
3.C4The ratio entering three sections of reactors is 1.5:1:1, and air enters the ratio of three sections of reactors and is
1.5:1:0.8；
4. as other operating conditions are substantially with example 1.
Example 3:
1. as flow process is with example 1；
2. enter the C of three sections of reactors4, air and water vapour charging, total water alkene mol ratio is 20, total
Oxygen alkene mol ratio is 1；
3.C4The ratio entering three sections of reactors is 3:1:1, and it is 2 that air enters the ratio of three sections of reactors:
1:0.5；
4. as other operating conditions are substantially with example 1.
The present embodiment is shown in Table 1. compared with the contrast of technology
Table 1
| Contrast effect | Existing technique | The present embodiment 1,2,3 |
| Reactor | Two sections or three sections | Three sections |
| Butylene heater | Nothing | Have |
| Air heater | Nothing | Have |
| C4Middle butene concentration | More than 93%wt | 85%wt |
| C4Charging phase | Liquid phase | Gas phase |
| C4Feeding temperature | 40～100 DEG C | 230℃ |
| Air feed temperature | Less than 150 DEG C | 230℃ |
| I section reactor feed temperature | 330～360 DEG C | 350℃ |
| II section reactor feed temperature | 330～370 DEG C | 355℃ |
| III section reactor feed temperature | 340～400 DEG C | 365℃ |
| Generate condensation polymer in gas | Many | Few |
| Catalyst regeneration cycle | 1～3 months | 6～9 months |
| Catalyst service life | 9～12 months | 18～24 months |
As it can be seen from table 1 compared to existing technology, invention increases butylene carburetion system and and air
With butylene heating system, although increased on one-time investment, but the regeneration period of the upper catalyst of operation
Having extended with service life, greatly reduced running cost, the economic benefit of device is substantially carried
Rise.
Claims (9)
1. the device of an Oxidative Dehydrogenation of Butene into Butadiene, it is characterised in that:
Described device arranges butylene vapourizing unit and reaction gas preheating device,
Butylene vapourizing unit includes: butylene evaporator and butylene vaporizer, and butylene vaporizer is arranged on butylene evaporation
Pot bottom；
Described reaction gas preheating device includes butylene heater and air heater；
After air cushioning tank connects air heater, pipeline is divided into three, connects I section reactor, II respectively
Section reactor, the entrance of III section reactor；
After butylene evaporator connects butylene heater, pipeline is divided into three, connects I section reactor, II respectively
Section reactor, the entrance of III section reactor；
Described I section reactor, II section reactor and III section reactor are sequentially connected in series.
2. the method using Oxidative Dehydrogenation of Butene into Butadiene device as claimed in claim 1, its feature
It is that described method includes:
1) air is heated by the air device the most again and is preheating to temperature is 150～300 DEG C, liquid phase C4Charging
Being preheating to temperature through butylene heater again after vaporization is 150～300 DEG C；
2) air and C4Being respectively classified into three strands, one steams with the water after two-stage reaction outlet heat exchanger heat exchange
Vapour is mixed into I section reactor, and one is mixed into II section with I section outlet generation gas after heat exchange and reacts
Device, one is mixed into III section reactor with II section outlet generation gas after heat exchange；
3) water vapour sequentially passes through I section reacting replacing heat device and II section reacting replacing heat device, exports with two reactor
High temperature generate after gas carries out heat exchange, then entrance I section reactor after mix with the air after preheating and butylene；
Under the effect of catalyst, carry out oxidative dehydrogenation generate containing 1,3-butadiene, C4Alkynes and furan, aldehyde,
Acid, CO2, the generation gas of CO.
3. the method for Oxidative Dehydrogenation of Butene into Butadiene as claimed in claim 2, it is characterised in that:
Air is heated by the air device the most again and is preheating to temperature is 200～250 DEG C；Liquid phase C4Charging is through vapour
Being preheating to temperature through butylene heater again after change is 200～250 DEG C.
4. the method for Oxidative Dehydrogenation of Butene into Butadiene as claimed in claim 2, it is characterised in that:
Enter the C of every first stage reactor4, air and water vapour charging, total water alkene mol ratio is 6～20；Always
Oxygen alkene mol ratio 0.1～1.
5. the method for Oxidative Dehydrogenation of Butene into Butadiene as claimed in claim 4, it is characterised in that:
Enter the C of every first stage reactor4, air and water vapour charging, total water alkene mol ratio is 10～15, always
Oxygen alkene mol ratio be 0.5～0.8.
6. the method for Oxidative Dehydrogenation of Butene into Butadiene as claimed in claim 2, it is characterised in that:
Described C4In charging, butene concentration is 60%～100%.
7. the method for Oxidative Dehydrogenation of Butene into Butadiene as claimed in claim 2, it is characterised in that:
Described C4In charging, butene concentration is 75%～90%.
8. the method for Oxidative Dehydrogenation of Butene into Butadiene as claimed in claim 2, it is characterised in that:
The operation pressure of described butylene vaporizer and butylene evaporator is 0.2～0.35MPag, and operation temperature is
30～50 DEG C.
9. the method for Oxidative Dehydrogenation of Butene into Butadiene as claimed in claim 2, it is characterised in that:
Described C4Entrance I section reactor, II section reactor, the ratio of III section reactor are 3～2:2～1:
1～0.5；
Described air enters I section reactor, II section reactor, the ratio of III section reactor are
2～1:1.5～0.8:1～0.5.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1004232A (en) * | 1971-12-30 | 1977-01-25 | The Standard Oil Company | Coproduction of methacrylonitrile and butadiene |
| CN202516539U (en) * | 2012-03-10 | 2012-11-07 | 中石油东北炼化工程有限公司锦州设计院 | Low-temperature heat utilization system of reaction gas waste heat from fluidized bed for preparing butadiene by oxidative dehydrogenation of butene |
| CN102826950A (en) * | 2012-09-06 | 2012-12-19 | 湖南百利工程科技股份有限公司 | Process method for circularly utilizing waste water produced by butadiene preparation through butene oxidative dehydrogenation |
| CN102875314A (en) * | 2012-06-20 | 2013-01-16 | 张守义 | Two-reaction system for preparing butadiene through oxidative dehydrogenation of butene and anti-carbon method |
| CN103086828A (en) * | 2013-01-30 | 2013-05-08 | 中国石油化工股份有限公司 | Method for realizing increase production of butadiene |
-
2013
- 2013-11-05 CN CN201310544346.3A patent/CN104610007B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1004232A (en) * | 1971-12-30 | 1977-01-25 | The Standard Oil Company | Coproduction of methacrylonitrile and butadiene |
| CN202516539U (en) * | 2012-03-10 | 2012-11-07 | 中石油东北炼化工程有限公司锦州设计院 | Low-temperature heat utilization system of reaction gas waste heat from fluidized bed for preparing butadiene by oxidative dehydrogenation of butene |
| CN102875314A (en) * | 2012-06-20 | 2013-01-16 | 张守义 | Two-reaction system for preparing butadiene through oxidative dehydrogenation of butene and anti-carbon method |
| CN102826950A (en) * | 2012-09-06 | 2012-12-19 | 湖南百利工程科技股份有限公司 | Process method for circularly utilizing waste water produced by butadiene preparation through butene oxidative dehydrogenation |
| CN103086828A (en) * | 2013-01-30 | 2013-05-08 | 中国石油化工股份有限公司 | Method for realizing increase production of butadiene |
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