CN106008134B - Cracking of ethylene C9Deviate from the method for lighter component in separating technology - Google Patents
Cracking of ethylene C9Deviate from the method for lighter component in separating technology Download PDFInfo
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- CN106008134B CN106008134B CN201610333632.9A CN201610333632A CN106008134B CN 106008134 B CN106008134 B CN 106008134B CN 201610333632 A CN201610333632 A CN 201610333632A CN 106008134 B CN106008134 B CN 106008134B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2/00—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms
- C07C2/02—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by addition between unsaturated hydrocarbons
- C07C2/50—Diels-Alder conversion
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/148—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound
- C07C7/177—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound by selective oligomerisation or polymerisation of at least one compound of the mixture
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Abstract
The invention discloses a kind of cracking of ethylene C9Deviate from the method for lighter component in separating technology, solve cracking of ethylene C9Rectifying tower top cyclopentadiene and methyl cyclopentadiene excessive concentration during separation lighter component, influence the problem of device is stablized.Specifically from cracking of ethylene C9Second distillation column top is isolated the lighter components such as cyclopentadiene, methyl cyclopentadiene and is back to after dimerization reaction in Second distillation column in separating technology, reduce the content of cyclopentadiene and methyl cyclopentadiene in the lighter component of Second distillation column top, so that Second distillation column system vacuum pump no longer band liquid, system vacuum are stably controlled；Meanwhile add Second distillation column side line and kettle material produced quantity and optimize each section of material composition, improve the produced quantity and C of high-quality Petropols raw material9The comprehensive utilization ratio of fraction.
Description
Technical field
The invention belongs to petrochemical industry, removed in more particularly to a kind of by-product C 9 distillate from petroleum cracking ethene
The method of lighter component.
Background technology
Crack C9Fraction mostlys come from the accessory substance of naphtha or Pyrolysis Reaction of Gas Oil, accounts for the 10%-20% of ethylene yield.
Crack C9Fractional composition is complicated, there are about 190 Multicomponents, it is known that about nearly 30 kinds of materials, content accounts for 65%, remaining
The then unknown heavy component containing the more cyclenes of 16% C10~C12 and 19% or so.
Cracking C at present9The higher technique of fraction utilization rate is by C9Fraction carries out separation utilization, can be higher with separation purity
Cyclopentadiene, methyl cyclopentadiene, styrene, methyl styrene, dicyclopentadiene, the product such as indenes be used to produce Petropols
And other Application in Chemical Engineering.
In cracking C9In fraction separation process, since dicyclopentadiene content is higher in raw material, dicyclopentadiene is heated easily
Cyclopentadiene is resolved into, cyclopentadiene will be polymerized to dicyclopentadiene and heat release again at normal temperatures, and dicyclopentadiene is in essence
Evaporate to be heated in tower and be decomposed into cyclopentadiene, cause during rectifying column deviates from lighter component, the cyclopentadiene and methyl ring that are rich in
The lighter components such as pentadiene, are gathered since rectifying tower top flows back in rectifying tower top, easily make rectifying tower system vacuum pump band liquid, efficiency
Decline, make rectifying tower system vacuum relatively low and can not stability contorting, while the lighter hydrocarbons such as cyclopentadiene, methyl cyclopentadiene enter
Polymerization exotherm again after product storage tank, causes tank temperature to raise, there are security risk during storage.
In order to avoid the appearance of above-mentioned phenomenon, it is ensured that the steady production of device, usual way is will to deviate from cyclopentadiene
Rectifying column tower top extraction lighter component in the control of the sum of concentration of cyclopentadiene and methyl cyclopentadiene in 35% (WT) below, this
It is exactly substantial amounts of C that kind, which takes the mode of quiet run,9Component and dicyclopentadiene fraction are from this overhead extraction, to reduce tower top
Cyclopentadiene and methyl cyclopentadiene concentration, and then stablize the vacuum of rectifying column, the steady production of promote device is such a
Mode is actually a kind of mode of sacrificial resin raw material.
Due to substantial amounts of C9Component and dicyclopentadiene component are cut in lighter component, and this not only reduces C9Separation
Be used for produce the raw material of resin, and this strand of material can only be used as oil product to sell, and price is low compared with resin raw material, certainly will so drop
Low C9Fraction efficiently uses, and then influences the economic benefit of device.
Therefore, cracking of ethylene C can preferably be solved by being badly in need of one kind at present9In separating technology rectifying tower top cyclopentadiene and
Methyl cyclopentadiene excessive concentration, influences the method for device steady production.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of cracking of ethylene C9Deviate from the side of lighter component in separating technology
Method, adopting said method can reduce the pumped vacuum systems that the lighter hydrocarbons such as cyclopentadiene and methyl cyclopentadiene enter rectifying column, make tower true
Sky control is stablized, while obtains more, good Petropols raw material, improves C9Fraction comprehensive utilization ratio.
For achieving the above object, the technical solution adopted in the present invention is to provide a kind of cracking of ethylene C9Separating technology
The method of middle abjection lighter component, specifically includes following steps：
（1）Cracking of ethylene C9Raw material enters first rectifying column, and first rectifying column tower top lighter component enters Second distillation column, the
Sent after the heavy component cooling of one tower bottom of rectifying tower extraction to tank field；
（2）The tower top light component of first rectifying column carries out rectification under vacuum in Second distillation column, Second distillation column tower top
Contain cyclopentadiene, methyl cyclopentadiene and part C9The lighter component of component etc. enters dipolymer reactor；From Second distillation column
Fraction oil of the side take-off as high-quality Petropols raw materials for production is taken out below the packing section of top, tower reactor extraction material is used to give birth to
Produce Petropols or further separation utilization；
（3）Cyclopentadiene and methyl cyclopentadiene in Second distillation column tower top lighter component carry out two in dipolymer reactor
Poly- reaction, dimers enter third distillation column；
（4）Above-mentioned dimers are separated in third distillation column, and third distillation column tower top is separated containing not
The lighter component of the cyclopentadiene of dimerization, methyl cyclopentadiene etc. returns to dipolymer reactor and carries out dimerization reaction, third distillation column tower
The material rich in styrene, methyl styrene and dicyclopentadiene of kettle extraction is all back in Second distillation column or has part
Send outside to storage tank.
The bottom temperature of the first rectifying column is 190-230 DEG C, and tower top temperature is 100-140 DEG C, reflux ratio 0.1-
1.0, tower top pressure is -65~-80KPaG.
The bottom temperature of the Second distillation column is 120-170 DEG C, and tower top temperature is 60-110 DEG C, and reflux ratio is whole for 1-
Reflux, tower top pressure is -55~-80 KPaG.
The dipolymer reactor can be the series connection of one or more reactor, and reaction temperature is 100-160 DEG C, reaction pressure
For 1000~1500 KPaG.
The bottom temperature of the third distillation column is 110-160 DEG C, and tower top temperature is 40-80 DEG C, reflux ratio 1-8,
Tower top pressure is -10~-70 KPaG.
It is preferred that the bottom temperature of Second distillation column is 130-160 DEG C, tower top temperature is 60-90 DEG C, reflux ratio 2-5, tower
Pressure on top surface is -60~-75 KPaG.
It is preferred that dipolymer reactor reaction temperature is 110-140 DEG C, reaction pressure is 900~1200 KPaG.
It is preferred that the bottom temperature of third distillation column is 120-150 DEG C, tower top temperature is 40-70 DEG C, reflux ratio 1-5, tower
Pressure on top surface is -20~-50 KPaG.
Beneficial effect
1st, after using the method for the present invention, light group of the cyclopentadiene isolated from Second distillation column top, methyl cyclopentadiene etc.
Part is back in Second distillation column after dimerization reaction, makes Second distillation column top reflux material middle ring pentadiene and methyl ring penta
The sum of content of diene substantially reduces, and avoids the lighter components such as cyclopentadiene and methyl cyclopentadiene and is accumulated on Second distillation column top
It is poly-, the sum of content of cyclopentadiene and methyl cyclopentadiene in the lighter component of Second distillation column top is substantially reduced, so as to ensure the
Two rectifying tower system vacuum pumps no longer band liquid, distillation system vacuum are stably controlled；Avoid and adopted outside Second distillation column top gently
Since cyclopentadiene and methyl cyclopentadiene too high levels enter the generation of polymerization exotherm phenomenon behind tank field in component；
2nd, after adding Second distillation column top lighter component dipolymer reactor and the further piece-rate system of third distillation column, the second essence
Total reflux operation can be realized by evaporating tower, so as to increase Second distillation column side line and kettle material produced quantity and optimize each section of material group
Into, so, the method for the present invention has the cut quality of optimization Petropols raw material, improves the produced quantity of high-quality Petropols raw material
Effect, for improve C9The comprehensive utilization ratio of fraction provides safeguard.
Brief description of the drawings
Fig. 1 is the process flow diagram of the present invention.
In figure：1- first rectifying columns；2- Second distillation columns；3- dipolymer reactors；4- third distillation columns；W1- cracking of ethylene
C9Raw material；W2- first rectifying columns tower reactor produces heavy constituent；W3- first rectifying column overhead extraction fractions；W4- Second distillation columns top
Discharging（Dipolymer reactor is fed）；W5- dipolymer reactors discharge（Third distillation column is fed）；W6- third distillation columns top production
Material；Second distillation column reflux material is removed in the extraction of W7- third distillation columns kettle；Adopted outside W8- third distillation columns kettle to storage tank material；W9-
Adopt material in Second distillation column side；W10- Second distillation columns tower reactor produces material.
Embodiment
Below in conjunction with the accompanying drawings and specific embodiment, comparative example, the present invention is further explained.It is to be understood that embodiment is only used
In the explanation present invention rather than limit the scope of the invention.In addition, it should also be understood that, after present disclosure has been read, this area
Technical staff can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims
Limited range.
Embodiment 1
The technological process of the present embodiment and embodiment 2 is as shown in Figure 1, concrete technology step is as follows：
（1）Cracking of ethylene C9Raw material fraction enters first rectifying column with the speed of 12500kg/h, and tower top lighter component enters the
Two rectifying columns, send to tank field after the heavy component cooling of first rectifying column tower reactor extraction；
（2）First rectifying column tower top lighter component carries out rectification under vacuum in Second distillation column, and Second distillation column tower top contains
There are cyclopentadiene, methyl cyclopentadiene and part C9The lighter component of component etc. enters dipolymer reactor；From Second distillation column tower
Side take-off part fraction oil, the raw materials for production as high-quality Petropols are taken out below the packing section of top；Tower reactor produces material
It is directly used in production Petropols or further separation utilization；
（3）Cyclopentadiene and methyl cyclopentadiene in Second distillation column tower top lighter component carry out two in dipolymer reactor
Poly- reaction, dimers enter third distillation column；
（4）Dimers are separated by third distillation column, and third distillation column tower top is separated to contain non-dimerization
Cyclopentadiene, the lighter component of methyl cyclopentadiene etc. return to dipolymer reactor and carry out dimerization reaction, third distillation column tower reactor is adopted
The material rich in styrene, methyl styrene and dicyclopentadiene gone out is all back in Second distillation column or has part to send outside
To storage tank.
Technological parameter involved by the present embodiment, as shown in table 1 and table 2：
1 cracking of ethylene C of table9Separator operating condition table
2 cracking of ethylene C of table9Raw material is formed with separated each section of material（WT%）
Embodiment 2
Technological process is the same as embodiment 1 used by the present embodiment.
Technological parameter involved by the present embodiment, as shown in table 3 and table 4：
3 cracking of ethylene C of table9Separator operating condition table
4 cracking of ethylene C of table9Raw material is formed with separated each section of material（WT%）
Comparative example 1
Existing cracking of ethylene C9In isolation technics, light group of cyclopentadiene and methyl cyclopentadiene in lighter component knockout tower etc.
Part content is higher, make rectifying tower vacuum degree can not stability contorting, influence device steady production.Typical process is as follows：
（1）Cracking of ethylene C9Raw material enters first rectifying column with 12500kg/h speed first, and tower top obtains C9Lighter component into
Enter next unit, tower reactor obtains removing cracking C9 Sent after the heavy components such as dimer, tripolymer in raw material and cooling to tank field,
For fuel or the raw material of deep resin；
（2）First rectifying column tower top material carries out rectification under vacuum in Second distillation column.In the ring that Second distillation column top obtains
Pentadiene, methyl cyclopentadiene and part C9The lighter component of component etc. enters tank field and is sold as oil product after cooling, and second
Rectifying column side take-off part fraction, for producing high-quality Petropols；Second distillation column kettle extraction fraction is directly used in production
Petropols further separate utilization into next unit.
The technological parameter of this comparative example 1, as shown in table 5 and table 6：
5 cracking of ethylene C of table9Separator operating condition table
6 cracking of ethylene C of table9Raw material is formed with separated each section of material（WT%）
It can be seen that to add Second distillation column lighter component dimerization anti-by the comparison of embodiment 1, embodiment 2 and comparative example 1
After answering device and the further piece-rate system of third distillation column, in embodiment 1 and embodiment 2 in the reflux material of Second distillation column tower top
The sum of cyclopentadiene and methyl cyclopentadiene content are 1.02% respectively（WT）With 0.78%（WT）, and the second rectifying in comparative example 1
The sum of the reflux material middle ring pentadiene of column overhead and methyl cyclopentadiene content are 37.13%（WT）, this avoid ethene to split
Solve C9Separated cyclopentadiene and methyl cyclopentadiene gather on Second distillation column top, make the tower of Second distillation column in two embodiments
Top produces the sum of content of above-mentioned two component and is below 35%（WT）Hereinafter, it ensure that the stability contorting of rectifying tower vacuum system.
Comparative example 2
In existing cracking of ethylene C9In isolation technics, in order to solve rectifying tower vacuum system stable control, usually adopt
With the method components such as substantial amounts of styrene, methyl styrene and dicyclopentadienes from this overhead extraction, to reduce tower top
The concentration of cyclopentadiene and methyl cyclopentadiene, and then stablize the vacuum control of rectifying column, operating procedure is the same as comparative example 1, each tower
Process condition be shown in Table 7, cracking of ethylene C9Raw material and separated each section of material composition, are shown in Table 8.
7 cracking of ethylene C of table9Separator operating condition table
8 cracking of ethylene C of table9Raw material is formed with separated each section of material（WT%）
It can be seen that by the comparison of embodiment 1, embodiment 2 and comparative example 2 and add Second distillation column tower top lighter component two
After poly- reactor and the further piece-rate system of third distillation column, there are two significant changes：
1st, Second distillation column side take-off amount is respectively 2406 kg/h and 1987 kg/h in embodiment 1 and embodiment 2, real
The tower reactor produced quantity for applying Second distillation column in example 1 and embodiment 2 is respectively 7969 kg/h and 7550 kg/h, and in comparative example 2
Second distillation column side line and tower reactor produced quantity be 1313kg/h and 6875kg/h respectively, contrast understands embodiment 1 and embodiment 2
Second distillation column side line and tower reactor produced quantity substantially increase, improve high-quality Petropols raw material produced quantity；
2nd, the content of styrene is 9.85% respectively in the side take-off cut of Second distillation column in embodiment 1 and embodiment 2
（WT）With 7.89%（WT）, and the content of styrene is 4.90% in the side take-off cut of Second distillation column in comparative example 2（WT）,
The content of styrene significantly improves in the side take-off cut of the Second distillation column of embodiment 1 and embodiment 2 knowable to contrast, optimizes
Second distillation column side line is used for the cut quality of Petropols raw material.
Claims (8)
- A kind of 1. cracking of ethylene C9Deviate from the method for lighter component in separating technology, specifically include following steps：（1）Cracking of ethylene C9Raw material enters first rectifying column, and first rectifying column tower top lighter component enters Second distillation column, the first essence Sent after evaporating the heavy component cooling of tower tower reactor extraction to tank field；（2）The tower top lighter component of first rectifying column carries out rectification under vacuum in Second distillation column, and Second distillation column tower top contains Cyclopentadiene, methyl cyclopentadiene and part C9The lighter component of component etc. enters dipolymer reactor；At the top of from Second distillation column Fraction oil of the side take-off as high-quality Petropols raw materials for production is taken out below packing section, tower reactor extraction material is used to produce stone Oleoresin or further separation utilize；（3）It is anti-that cyclopentadiene and methyl cyclopentadiene in Second distillation column tower top lighter component carry out dimerization in dipolymer reactor Should, dimers enter third distillation column；（4）Above-mentioned dimers are separated in third distillation column, and third distillation column tower top is separated to contain non-dimerization Cyclopentadiene, the lighter component of methyl cyclopentadiene etc. return to dipolymer reactor and carry out dimerization reaction, third distillation column tower reactor is adopted The material rich in styrene, methyl styrene and dicyclopentadiene gone out is all back in Second distillation column or has part to send outside To storage tank.
- 2. cracking of ethylene C according to claim 19Deviate from the method for lighter component in separating technology, it is characterised in that：It is described The bottom temperature of first rectifying column is 190-230 DEG C, and tower top temperature is 100-140 DEG C, reflux ratio 0.1-1.0, tower top pressure Power is -65~-80KPaG.
- 3. cracking of ethylene C according to claim 19Deviate from the method for lighter component in separating technology, it is characterised in that：It is described The bottom temperature of Second distillation column is 120-170 DEG C, and tower top temperature is 60-110 DEG C, and reflux ratio all flows back for 1-, tower top pressure Power is -55~-80 KPaG.
- 4. cracking of ethylene C according to claim 19Deviate from the method for lighter component in separating technology, it is characterised in that：It is described Dipolymer reactor, can be the series connection of one or more reactor, the reaction temperature of dipolymer reactor is 100-160 DEG C, reaction pressure Power is 1000-1500 KPaG.
- 5. cracking of ethylene C according to claim 19Deviate from the method for lighter component in separating technology, it is characterised in that：It is described The bottom temperature of third distillation column be 110-160 DEG C, tower top temperature be 40-80 DEG C, reflux ratio 1-8, tower top pressure for- 10~-70 KPaG.
- 6. cracking of ethylene C according to claim 39Deviate from the method for lighter component in separating technology, it is characterised in that：Second The bottom temperature of rectifying column is 130-160 DEG C, and tower top temperature is 60-90 DEG C, reflux ratio 2-5, tower top pressure for -60~- 75 KPaG。
- 7. cracking of ethylene C according to claim 49Deviate from the method for lighter component in separating technology, it is characterised in that：Dimerization The reaction temperature of reactor is 110-140 DEG C, and reaction pressure is 1000~1200 KPaG.
- 8. cracking of ethylene C according to claim 59Deviate from the method for lighter component in separating technology, it is characterised in that：3rd The bottom temperature of rectifying column is 120-150 DEG C, and tower top temperature is 40-70 DEG C, reflux ratio 1-5, tower top pressure for -20~- 50 KPaG。
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| CN201610333632.9A CN106008134B (en) | 2016-05-19 | 2016-05-19 | Cracking of ethylene C9Deviate from the method for lighter component in separating technology |
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| CN104276914B (en) * | 2013-07-12 | 2018-11-20 | 中国石油化工股份有限公司 | Utilize the method for rectifying column separation petroleum cracking Crude products.deep process C9~C10 fraction |
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