CN107760357A - Low accessory substance reforms oil-off olefin technique - Google Patents
Low accessory substance reforms oil-off olefin technique Download PDFInfo
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- CN107760357A CN107760357A CN201610707641.XA CN201610707641A CN107760357A CN 107760357 A CN107760357 A CN 107760357A CN 201610707641 A CN201610707641 A CN 201610707641A CN 107760357 A CN107760357 A CN 107760357A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G29/00—Refining of hydrocarbon oils, in the absence of hydrogen, with other chemicals
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Abstract
The present invention relates to a kind of low accessory substance to reform oil-off olefin process for refining, using the invented technology, when overcoming the starting stage that catalyst is run in conventional deolefination process for refining, toluene level is higher in product after reaction, so as to cause follow-up xylene fractionation product to exceed the Con trolling index of adsorbing separation, the problem of causing dimethylbenzene not meet technological requirement.Inlet feed 2 is mixed into using by the material 1 of reaction feed and the product material 4 being recycled back to, into reactor, reacted material 3, which is divided into recycle stock 4 and goes out this technique, enters downstream material 5, material 5 enters down-stream system, recycle stock 4 enters pumping and is mixed into reactor with material 1, preferably solve the problem, greatly reduce byproduct of reaction toluene, can be applied to the industrial production of deolefination.
Description
Technical field
The invention belongs to reform oil-off olefin technique, and in particular to a kind of deolefination method for reducing toluene accessory substance.
Background of invention
The present invention relates to reform oil-off olefin technique.
Catalytic reforming is the main manufacturing process of the industrial chemicals such as benzene,toluene,xylene.With entering for catalytic reforming technology
Step and material composition change, the exploitation of new reforming catalyst, the reaction severity of reformation are improving, and ultralow pressure operating technology is general
All over using, the problem of bringing therewith is that the olefin(e) centent in catalytic reforming generation oil further increases.In catalytic reforming generation oil
Rich in aromatic hydrocarbons and solvent naphtha, qualified aromatic hydrocarbons and solvent naphtha are produced, it is necessary to remove alkene therein.Reformed oil it is a small amount of
Alkene, the corrosion for causing extraction system equipment can be polymerize in extraction solvent.In addition, alkene especially alkadienes is in certain bar
Under part, it is easy to form colloid, adsorb catalyst and adsorbent surface in downstream process, so as to reduce its service life.And
These alkene being rich in have had influence on the qualified aromatic hydrocarbon product of production, must also remove.
Device typically removes reformed oil using the methods of activated particle carclazyte, molecular sieve catalyst both at home and abroad at present
In alkene, also have using hydrofinishing process reduce reformate olefin(e) centent.Atlapulgite is to bentonite by inorganic acid
A kind of acidified modified obtained bentonite modified product is carried out, it is acidified modified to improve bentonitic whiteness, specific surface area, acid
Intensity etc., obtained atlapulgite have the functions such as adsorption bleaching, catalysis.Easily inactivation, hardly possible be present in granular carclazyte process for refining
The shortcomings of to regenerate, change frequently and pollute environment.With reforming reaction severity more and more higher, carclazyte inactivation is caused to be accelerated,
The general tens days carclazytes for just needing more to renew, some devices even replace once a week.
The method of Hydrobon removing alkene is containing base metal (such as Co-Mo or Ni-Mo/Al2O3) or your gold
Belong to (Pt, Pd/Al2O3) catalyst action under alkene in selective hydrogenation saturation reformed oil.The reaction that the former needs
Temperature is higher (typically at 300 DEG C~330 DEG C or so), and high energy consumption, aromatic hydrocarbons loss are larger.And use noble metal catalyst selectivity
The alkene that hydrogenation and removing benzene is rich in into xylene fraction, can (90~150 DEG C) progress under the process conditions more relaxed
Hydrogenation reaction, aromatic hydrocarbons loss is smaller, but expensive catalyst, and the presulfurization generation sulfide of catalyst causes environment pollution.
There is non-hydrogenated molecule sieve catalyst for refining the catalyst single trip use life-span can reach 8 times of granular carclazyte at present
More than, while can regenerate repeatedly.But it is too high in starting stage reactivity to work as olefin of reforming oil catalyst, and alkane easily occurs
The side reactions such as group-transfer, generation toluene accessory substance cause in follow-up xylene products that toluene level is exceeded, cause reaction product not
It is qualified, improve production cost.
In CN103184067A, using atlapulgite and the compound packing method of molecular sieve catalyst for refining, catalysis is extended
Agent service life, but can not solve the problems, such as that toluene accessory substance is excessive in catalyst operation.
The invention aims to overcome under catalyst initial operating stage, substantial amounts of accessory substance toluene generation after reaction
Excessively, the problem of causing production cost too high.The present invention carries out reformate by using the pattern of the circulation products of uniqueness and takes off alkene
Hydrocarbon technique productions, preferably solves the problem.
The content of the invention
The technical problems to be solved by the invention are that mainly solve to reform oil-off olefin technical process, deolefination process for refining
During the starting stage of middle catalyst operation, toluene level is higher in product after reaction, so as to cause follow-up xylene fractionation product
More than the Con trolling index of adsorbing separation, the problem of causing dimethylbenzene not meet technological requirement.The present invention is taken off using a kind of reformate
Olefin process process, by recycle stock 4, reaction system is mixed into fresh material, preferably solves reformation oil-off olefin
Technique, the problem of product toluene accessory substance is exceeded.
In order to solve the above technical problems, the present invention uses reformation oil-off olefin art production process as follows：
One kind reforms oil-off olefin process for refining, by the material 1 of reaction feed and the product material 4 that is recycled back to be mixed into
Mouth material 2, into reactor, the reacted reacted material 3 of material 3, which is divided into recycle stock 4 and goes out this technique, enters downstream thing
Material 5, material 5 enter down-stream system, and recycle stock 4 enters pumping and is mixed into reactor with material 1.
For in above-mentioned offer technical scheme：
The catalyst reformed used in oil-off olefin process for refining is the molecular sieve with acid catalysis function, generally micropore point
Son sieve, such as NaHY, USY, beta-molecular sieve.Wherein USY molecular sieve is the conventional molecular sieve of industry.Catalyst reactor also may be used
Using the molecular sieve of containing mesopore, the molecular sieve selected from least one of NaHY, USY, beta-molecular sieve containing mesopore.
The weight of reformation oil-off olefin process for refining, its recycle stock and import fresh material is than 0.01~10.It is recycled back to
Product material (4) be heated or cooled and contacted again with catalyst with after the mixing of the material (1) of reaction feed afterwards.
The when containing clay tower before reactor, being recycled back to material can enter before reactor or before clay tower, can also enter respectively
Before both.
The reformation oil-off olefin process for refining of the present invention, mixed material enter reactor process condition：Reaction pressure 0.5~
5.0MPa, 130~250 DEG C of reaction temperature, 0.5~8.0h of fresh material meter weight space velocity-1。
The reformation oil-off olefin process for refining of the present invention can operate initial stage, the application of operation later stage in olefinic hydrocarbon expelling catalyzer.
The reformation oil-off olefin process for refining of the present invention is when use tower process containing carclazyte, can be to be recycled back to material progress cold
But or heat into reactor, improve the olefin conversion of clay tower, so as to extend the life-span of catalyst.
The present invention main advantage is that：
1 reduces appliance arrangement.After technique using molecular sieve refining agent, due to initial stage molecular sieve refining agent activity compared with
Height, cause accessory substance toluene level higher, using after this technique, it is not necessary to the equipment such as heat exchanger are accessed in process, it is less
Investment.
2 pairs of products can be adjusted in certain amplitude.When accessory substance is higher, recycle stock can be improved to improve air speed,
The residence time of raw material is reduced so as to reducing the generation of accessory substance.
3 effectively improve technique antigen material fluctuation ability.By improving or reducing recycle ratio, the impact to catalyst is reduced,
So as to improve catalyst life.
4 improve the diffusion rate of material.Air speed is improved, can improve the diffusion rate of reaction mass, so as to reduce aromatic hydrocarbons
In the residence time of catalyst, coking is reduced, extends the service life of catalyst.
5 extend catalyst service life.Initial stage is used in catalyst, because activity is higher, the air speed of catalyst is improved, drops
The bromine index of low raw material, so as to extend the service life of catalyst.
By using example below, the invention will be further elaborated：
Brief description of the drawings：
Fig. 1 is existing process method：1 it is the material of reaction feed, 2 be inlet feed, 3 is reacted material, 4 to follow
The product material of loopback, 5 are this technique to enter downstream material.
Embodiment
Following examples are used for illustrating invention by some specific scopes, and these embodiments are not entirely included invention
It is required that claim scope.It is conventional technology category in other parameters technique change, and the technology of the present invention embodies.
【Embodiment 1】
The bromine index 1105 of this process example reformate fresh feed, in 170 DEG C, 2.0MPa, 1.8h-1Under, Fig. 1 reactions
The material bromine index of USY molecular sieve hydrogen-catalyst reactor is used after not circulating as 22, accessory substance toluene 0.9%.If entering to urge
Have before agent reactor clay tower do not circulate after material bromine index be 12, accessory substance toluene 1.0%.Latter embodiments use phase
Same raw material.
Using such as Fig. 1 technological process.
By recycle stock 4, than mixture material 2 that the mass ratio of fresh feed 1 is 1.0, to enter new USY molecular sieve catalyst anti-
Device is answered, in 170 DEG C, 2.0MPa, 3.6h-1Under reacted material bromine index 23, accessory substance toluene 0.3%, subsequently into follow-up
Liquid-phase separating system.If material bromine index is 18 after having clay tower not circulate before entering hydrogen-catalyst reactor, accessory substance first
Benzene 0.5%.
【Embodiment 2】
Using such as Fig. 1 technological process.Recycle stock 4 is entered into molecular sieve than the mixture material 2 that fresh feed 1 is 0.01
Hydrogen-catalyst reactor, in 160 DEG C, 2.0MPa, 1.8h-1Under reacted material bromine index 22, accessory substance toluene 0.9%, then
Into follow-up liquid-phase separating system.
【Embodiment 3】
Using such as Fig. 1 technological process.Recycle stock 4 is entered into molecular sieve than the mixture material 2 that fresh feed 1 is 0.01
Hydrogen-catalyst reactor, in 170 DEG C, 2.0MPa, 1.8h-1Under reacted material bromine index 22, accessory substance toluene 1.0%, then
Into follow-up liquid-phase separating system.
【Embodiment 4】
Using such as Fig. 1 technological process.Recycle stock 4 is entered into molecular sieve than the mixture material 2 that fresh feed 1 is 1.0
Hydrogen-catalyst reactor, in 190 DEG C, 3.0MPa, 3.6h-1Under reacted material bromine index 29, accessory substance toluene is in product assay
0.4%, subsequently into follow-up liquid-phase separating system.After 1 day, by recycle stock 4 than fresh feed 1 be 0.5 mixture thing
Material 2 enters molecular sieve catalyst reactor, in 170 DEG C, 3.0MPa, 2.7h-1Under reacted material bromine index 26, accessory substance toluene
In product assay 0.3%, subsequently into follow-up liquid-phase separating system.After 2 days, by recycle stock 4 than fresh feed 1 be 0.2
Mixture material 2 enter molecular sieve catalyst reactor, in 150 DEG C, 2.0MPa, 2.2h-1Under reacted material bromine index 23,
Accessory substance toluene is in product assay 0.2%, subsequently into follow-up liquid-phase separating system.After 3 days, by recycle stock 4 than fresh
The mixture material 2 that raw material 1 is 0 enters molecular sieve catalyst reactor, in 140 DEG C, 2.0MPa, 1.8h-1Under reacted material
Bromine index 22, accessory substance toluene is in product assay 0.3%, subsequently into follow-up liquid-phase separating system.Continue to run with, finally exist
250℃、2.0MPa、1.8h-1Reaction run time when lower reaction product bromine index is more than 50 reaches 150 days.
【Embodiment 5】
Using such as Fig. 1 technological process.Recycle stock 4 is entered into molecular sieve than the mixture material 2 that fresh feed 1 is 3 to urge
Agent reactor, in 130 DEG C, 0.5MPa, 7.2h-1Under reacted material bromine index 28, accessory substance toluene 0.1%, Ran Houjin
Enter follow-up liquid-phase separating system.
【Embodiment 6】
Using such as Fig. 1 technological process.Recycle stock 4 is entered into beta molecules than the mixture material 2 that fresh feed 1 is 10
Sieve catalyst reactor, in 250 DEG C, 5.0MPa, 19.8h-1Under reacted material bromine index 29, accessory substance toluene contains in product
Amount 0.4%, subsequently into follow-up liquid-phase separating system.After 3 days, 250 DEG C, 5.0MPa, 5.4h are changed into-1(recycle stock 4 compares
Fresh feed 1 is reacted material bromine index 22 under 2), and accessory substance toluene is in product assay 0.4%, subsequently into follow-up
Liquid-phase separating system.After 5 days, 250 DEG C, 5.0MPa, 2.0h are changed into-1After being reacted under (recycle stock 4 is 0.1 than fresh feed 1)
Material bromine index 22, accessory substance toluene is in product assay 0.4%, subsequently into follow-up liquid-phase separating system.
【Embodiment 7】
Using increasing clay tower before reactor in such as Fig. 1 technological process.At the initial stage of operation by recycle stock 4 than fresh original
Material 1 enters NaHY molecular sieve catalyst reactors for 1.0 mixture material 2, in 180 DEG C, 2.0MPa, 3.6h-1Under it is reacted
Material bromine index 16, accessory substance toluene is in product assay 0.4%, subsequently into follow-up liquid-phase separating system.
【Embodiment 7】
Using increasing clay tower before reactor in such as Fig. 1 technological process..Phase phase follows temperature for 190 DEG C after the activation
Ring material 4 is that the mixture material 2 that 230 DEG C of fresh feeds 1 are 1.0 enters as after carclazyte than temperature, is cooled to another part
170 DEG C recycle stock (with fresh material ratio be 2.0) mix laggard molecular sieve catalyst reactor, 190 DEG C, 2.0MPa,
3.6h-1Under reacted material bromine index 16, toluene accessory substance 0.05%, subsequently into follow-up liquid-phase separating system.
【Embodiment 8】
Using such as Fig. 1 technological process.Recycle stock 4 is entered into containing mesopore than the mixture material 2 that fresh feed 1 is 0.01
USY molecular sieve hydrogen-catalyst reactor, in 200 DEG C, 0.5MPa, 1.8h-1Under reacted material bromine index 30, toluene accessory substance
1.2%, subsequently into follow-up liquid-phase separating system.
【Embodiment 9】
Using such as Fig. 1 technological process.Recycle stock 4 is entered into containing mesopore than the mixture material 2 that fresh feed 1 is 3
Beta molecular sieve catalyst reactors, in 200 DEG C, 1.5MPa, 7.2h-1Under reacted material bromine index 41, toluene accessory substance
0.5%, subsequently into follow-up liquid-phase separating system.
【Embodiment 10】
Using such as Fig. 1 technological process.Recycle stock 4 is entered into containing mesopore than the mixture material 2 that fresh feed 1 is 3
NaHY molecular sieve catalyst reactors, in 200 DEG C, 1.5MPa, 7.2h-1Under reacted material bromine index 50, toluene accessory substance
0.4%, subsequently into follow-up liquid-phase separating system.
【Comparative example 1】
Using increasing clay tower before reactor in such as Fig. 1 technological process..Fresh feed without recycle stock is entered mesoporous
USY molecular sieve hydrogen-catalyst reactor, in 190 DEG C, 3.0MPa, 1.8h-1Under reacted material bromine index 11, accessory substance toluene
In product assay 1.0%, subsequently into follow-up liquid-phase separating system.After 3 days, the fresh feed without recycle stock is entered mesoporous
USY molecular sieve hydrogen-catalyst reactor, in 190 DEG C, 3.0MPa, 1.8h-1Under reacted material bromine index 12, accessory substance toluene exists
Product assay 0.6%, subsequently into follow-up liquid-phase separating system.
【Comparative example 2】
Using such as Fig. 1 technological process.Fresh feed without recycle stock is entered into mesoporous USY molecular sieve catalyst reaction
Device, in 250 DEG C, 5.0MPa, 1.8h-1Under reacted material bromine index 11, accessory substance toluene is in product assay 1.9%, then
Into follow-up liquid-phase separating system.After 3 days, the fresh feed without recycle stock is entered into mesoporous USY molecular sieve catalyst reaction
Device, in 250 DEG C, 5.0MPa, 1.8h-1Under reacted material bromine index 12, accessory substance toluene is in product assay 1.2%, then
Into follow-up liquid-phase separating system.
【Comparative example 3】
Using increasing clay tower before reactor in such as Fig. 1 technological process..At the initial stage of operation, by without the new of recycle stock
Fresh raw material enters mesoporous USY molecular sieve hydrogen-catalyst reactor, in 130 DEG C, 2.0MPa, 1.8h-1Under reacted material bromine index 16,
Accessory substance toluene is in product assay 0.7%, subsequently into follow-up liquid-phase separating system.After 3 days, by without the fresh of recycle stock
Raw material enters mesoporous USY molecular sieve hydrogen-catalyst reactor, in 130 DEG C, 2.0MPa, 1.8h-1Under reacted material bromine index 17, it is secondary
Product toluene is in product assay 0.6%, subsequently into follow-up liquid-phase separating system.After 5 days, by the fresh original without recycle stock
Expect into mesoporous USY molecular sieve hydrogen-catalyst reactor, in 130 DEG C, 2.0MPa, 1.8h-1Under reacted material bromine index 17, by-product
Thing toluene is product assay 0.5% (product requirements are qualified), subsequently into follow-up liquid-phase separating system.Continue to run with, finally
In 250 DEG C, 2.0MPa, 1.8h-1When reaction run time when being more than 50 of reaction product bromine index reach 110 days.
Claims (10)
1. a kind of low accessory substance reforms oil-off olefin process for refining, it is characterised in that by the material (1) of reaction feed and is recycled back to
Product material (4) be mixed into inlet feed (2), into reactor, reacted material (3) is divided into recycle stock (4) and gone out
This technique enters downstream material (5), and material (5) enters down-stream system, and recycle stock (4) enters pumping and is mixed into reactor with material (1).
2. low accessory substance reforms oil-off olefin process for refining according to claim 1, it is characterised in that catalyst reactor
For the molecular sieve catalyst containing acid catalysis function.
3. low accessory substance reforms oil-off olefin process for refining according to claim 1, it is characterised in that the product thing being recycled back to
Expect (4) with the weight of the material (1) of reaction feed than 0.01~10.
4. low accessory substance reforms oil-off olefin process for refining according to claim 1, it is characterised in that exists before reactor
Clay tower, the product material being recycled back to (4) enter before reactor either into before clay tower or respectively enteing reactor and white
Before Tu Ta.
5. low accessory substance reforms oil-off olefin process for refining according to claim 1, it is characterised in that inlet feed (2) is entered
The process conditions for entering reactor are：0.5~5.0MPa of reaction pressure, 130~250 DEG C of reaction temperature, the material (1) of reaction feed
0.5~8.0h of weight space velocity-1。
6. low accessory substance reforms oil-off olefin process for refining according to claim 1, it is characterised in that technique is urged in deolefination
Agent operates initial stage, the application of operation later stage.
7. low accessory substance reforms oil-off olefin process for refining according to claim 1, it is characterised in that using before reactor
Carclazyte tower process be present, the product material (4) being recycled back to is cooled down or heated into reactor.
8. low accessory substance reforms oil-off olefin process for refining according to claim 2, it is characterised in that catalyst reactor
For micro porous molecular sieve, selected from least one of NaHY, USY, beta-molecular sieve.
9. low accessory substance reforms oil-off olefin process for refining according to claim 2, it is characterised in that catalyst reactor
For containing mesopore molecular sieve, the molecular sieve selected from least one of NaHY, USY, beta-molecular sieve containing mesopore.
10. low accessory substance reforms oil-off olefin process for refining according to claim 3, it is characterised in that the product being recycled back to
Material (4) is heated or cooled to be contacted with catalyst again with after material (1) mixing of reaction feed afterwards.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116262881A (en) * | 2021-12-14 | 2023-06-16 | 中国石油化工股份有限公司 | Method for selectively removing olefin impurities in reformate |
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Application publication date: 20180306 |