CN106832070A - For the method and device of continuous production polybutene 1 - Google Patents
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- CN106832070A CN106832070A CN201710109389.7A CN201710109389A CN106832070A CN 106832070 A CN106832070 A CN 106832070A CN 201710109389 A CN201710109389 A CN 201710109389A CN 106832070 A CN106832070 A CN 106832070A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F110/00—Homopolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F110/04—Monomers containing three or four carbon atoms
- C08F110/08—Butenes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/06—Treatment of polymer solutions
- C08F6/12—Separation of polymers from solutions
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Abstract
The invention provides a kind of method for continuous production polybutene 1, belong to high molecular polymer synthesis field, solvent during for recycling addition auxiliary agent used by dissolution aids so that polymerisation continuous-stable is carried out.Methods described includes：There is polymerisation in the presence of catalyst, auxiliary agent etc. by raw material of 1 butene monomers, then removal includes the mixture of the butene monomers of unreacted 1 from reaction mass, obtain polybutene 1, wherein, auxiliary agent was dissolved with solvent in advance before being added in polymer reactor, and the solvent is reclaimed from the mixture comprising the butene monomers of unreacted 1:Mixture comprising the butene monomers of unreacted 1 is carried out into rectifying separation；The the first bottom of towe component that will be obtained carries out rectifying separation；The second overhead components that will be obtained carry out liquid-liquid extraction cleaning, the solvent being recycled；The recovered solvent is returned for dissolving the auxiliary agent.Methods described is used for the continuous flow procedure of polybutene 1.
Description
Technical field
The present invention relates to high molecular polymer synthesis field, more particularly to a kind of method for continuous production PB Polybutene-1
And device.
Background technology
The industrialized production liquid phase method of PB Polybutene-1 can be divided into substance law and slurry process.Wherein, slurry process is to utilize inertia
Solvent such as alkane carries out the method that slurry polymerization prepares isotactic PB Polybutene-1 as diluent, fast with reaction speed, and
The operating condition of reaction is influenceed to be easy to the advantages such as Monitoring and Controlling.But substantial amounts of atent solvent is added in the method so as to poly-
Close technique and polymer reactor proposes more complicated requirement.
Compared with slurry process, reaction speed is faster for substance law.But it is raw due to the requirement by promoter addition and auxiliary agent characteristic
Auxiliary agent can be dissolved or be diluted with some solvents in advance in product, thus can be due to the addition of auxiliary agent in substance law production system
Process and bring solvent into, in process of production, polymerization process produce objectionable impurities can be enriched with the solvent, influence polymerization instead
Should, reaction can be prevented when serious from continuing.
So far, the solvent generally removes unreacted monomer directly as discharging of waste liquid with body, and there are no circulation makes
With the report of solvent.
The content of the invention
It is a primary object of the present invention to, there is provided a kind of method and device for continuous production isotactic polybutylene-1-1,
Solvent when recycling addition auxiliary agent used by dissolution aids.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that：
A kind of method for continuous production PB Polybutene-1, methods described includes：1- butene monomers are given with catalyst, outward
There is polymerisation in electron, auxiliary agent, part reaction mass is released, from the reaction mass in sequentially adding polymer reactor
Mixture of the removal comprising unreacted 1- butene monomers, obtains isotactic polybutylene-1-1, wherein, the auxiliary agent is being added to polymerization
Dissolved with solvent in advance before in reactor, the solvent is reclaimed from the mixture comprising unreacted 1- butene monomers:
The mixture comprising unreacted 1- butene monomers is carried out into rectifying separation, the first bottom of towe component is obtained；
The first bottom of towe component is carried out into rectifying separation, the second overhead components are obtained；
Second overhead components are carried out into the solvent that liquid-liquid extraction cleaning is recycled；
The recovered solvent is returned for dissolving the auxiliary agent before the auxiliary agent is added in polymer reactor.
Wherein, after second overhead components being carried out into liquid-liquid extraction cleaning, after liquid-liquid extraction is cleaned described second
Overhead components carry out solid adsorbent adsorption treatment.
It is described that the process that the second overhead components carry out liquid-liquid extraction cleaning is realized at a temperature of -5~40 DEG C.
It is described that second overhead components are carried out into the process of liquid-liquid extraction cleaning using alcohol, ester or its aqueous solution as extracting and washing
Agent.
The solid adsorbent is molecular sieve.
Methods described also includes reclaiming unreacted 1- butylene lists from the mixture comprising unreacted 1- butene monomers
Body, the unreacted 1- butene monomers of recovery are back in polymer reactor.
A kind of device for continuous production isotactic polybutylene-1-1, described device includes：
Polymer reactor, sends out for 1- butene monomers and catalyst, external electron donor, auxiliary agent in the polymer reactor
Raw polymerisation, releases part reaction mass, mixture of the removal comprising unreacted 1- butene monomers from the reaction mass,
To obtain isotactic polybutylene-1-1, wherein, the auxiliary agent was dissolved with solvent in advance before being added in the polymer reactor；
First rectifying column, the mixture comprising unreacted 1- butene monomers is separated for rectifying, obtains the first bottom of towe
Component；
Second distillation column, the first bottom of towe component is separated for rectifying, obtains the second overhead components；
Extraction tower, for carrying out liquid-liquid extraction cleaning to second overhead components, the solvent being recycled, the recovery
Solvent return for dissolving the auxiliary agent before auxiliary agent is added to the polymer reactor.
Described device also include adsorption tower, for being cleaned to liquid-liquid extraction after the second overhead components carry out solid adsorbent
Adsorption treatment.
In the extraction tower, liquid-liquid extraction cleaning is carried out to second overhead components at a temperature of -5~40 DEG C.
A kind of method and device for continuous production PB Polybutene-1 that the present invention is provided, is existed with 1- butene monomers as raw material
Polymerisation is carried out in the presence of catalyst, external electron donor, auxiliary agent, can continuously be produced and be obtained isotactic polybutylene-1-1, and
Mixture comprising unreacted 1- butene monomers, solvent is passed sequentially through into rectifying separation twice, liquid-liquid extraction cleaning, solvent is removed
The objectionable impurities of middle enrichment and recovery obtains qualified solvent, circulates for being dissolved before auxiliary agent is added in polymer reactor
Or dilution auxiliary agent, realize the recycling of solvent.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
The accompanying drawing to be used needed for having technology description is briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, without having to pay creative labor, may be used also
Other accompanying drawings are obtained with according to these accompanying drawings.
Fig. 1 is the device for continuous production PB Polybutene-1 described in the embodiment of the present invention.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
A kind of method for continuous production PB Polybutene-1 is the embodiment of the invention provides, methods described includes：By 1- fourths
There is polymerisation in alkene monomer, release part reactant in sequentially adding polymer reactor with catalyst, external electron donor, auxiliary agent
Material, mixture of the removal comprising unreacted 1- butene monomers, obtains isotactic polybutylene-1-1 from the partial reaction material, its
In, the auxiliary agent was dissolved with solvent in advance before being added in polymer reactor, from described comprising unreacted 1- butene monomers
Mixture in reclaim the solvent.It is described the solvent is reclaimed from the mixture comprising unreacted 1- butene monomers specifically
To include：
The mixture comprising unreacted 1- butene monomers is carried out into rectifying separation, the first bottom of towe component is obtained；
The first bottom of towe component is carried out into rectifying separation, the second overhead components are obtained；
Second overhead components are carried out into the solvent that liquid-liquid extraction cleaning is recycled；
The recovered solvent is returned for dissolving the auxiliary agent before the auxiliary agent is added in polymer reactor.
It is understood that in the embodiment of the present invention, what " first ", " second " were intend to distinguish between that first time rectifying to be obtained is
Bottom of towe component, what second rectifying to be obtained is overhead components.
A kind of method for continuous production PB Polybutene-1 is the embodiment of the invention provides, is existed as raw material with 1- butene monomers
Polymerisation is carried out in the presence of catalyst, external electron donor, auxiliary agent, it is by continuous discharge unit reaction mass and anti-from this
Answer remove in material comprising unreacted 1- butene monomers, solvent mixture continuously to obtain isotactic polybutylene-1-1, and will
Mixture comprising unreacted 1- butene monomers, solvent passes sequentially through rectifying separation twice, liquid-liquid extraction cleaning, in removing solvent
The objectionable impurities of enrichment and recovery obtains qualified solvent, circulate for the dissolving before auxiliary agent is added in polymer reactor or
Dilution auxiliary agent, realizes the recycling of solvent, and compared to directly liquid waste system is entered as waste liquid, the embodiment of the present invention is provided
Method saved the energy and effectively improved environment, ensured PB Polybutene-1 continuous production stabilization carry out, while avoiding
The product quality fluctuation problem caused by during solvent is recycled.
In embodiments of the present invention, there is provided a kind of body continuous production processes of PB Polybutene-1, it is in process of production, molten
Can enriched objectionable impurities, little by comparison, the conventional separation and recovery side of solvent itself usage amount in the solvent of enzymolysis auxiliary agent
Method is complex, and investment and operating cost are all very high.And the application is directed to this point, the removal of impurities removal process of uniqueness is devised,
The solvent that purity is qualified, can reuse is obtained using rectifying separation, liquid-liquid extraction.
Wherein, applicable catalyst can be supported titanium catalyst, such as titanium system Natta (Natta) catalyst.
Auxiliary agent such as co-catalyst, is specifically as follows alkyl aluminum, such as AlR3、AlR2Cl、AlRCl2, wherein, alkyl R is 2
To the direct-connected of 8 carbon atoms, side chain or cycloalkyl, for example, can be respectively the straight or branched alkyl or C3-C8 of C2-C8
Cycloalkyl, wherein, the straight chained alkyl of C2-C8 can be ethyl, and the branched alkyl of C2-C8 can be isobutyl group, the ring of C3-C8
Alkyl can be cyclopropyl.
Before polymer reactor is added to, co-catalyst can in advance be dissolved or be diluted with some solvents, to realize
Continuously, precisely add, thus solvent can be brought into reaction system.The impurity produced in polymerization process can be enriched in
In the solvent, polymerisation is influenceed, and be constantly enriched with objectionable impurities and can also make catalyst poisoning.The embodiment of the present invention is provided
Method, realize the recycling of solvent, effectively solve auxiliary agent in production process and recycle and cause catalyst consumption
Too high problem.
In order to further adjust the isotacticity of the PB Polybutene-1 for preparing during the course of the reaction, during the course of the reaction
Add external electron donor.Applicable external electron donor can be for one or more in silanization thing, ethers, lipid.
Wherein, silane compound for example can be diphenyldimethyl silane, VTES, vinyl front three
TMOS, MTES, phenyltrimethoxysila,e, phenyl triethoxysilane, diisobutyl dimethoxy
Silane, diisopropyl dimethoxy silane, dicyclopentyl dimethoxyl silane, Cyclohexyl Methyl Dimethoxysilane, cyclohexyl
Trimethoxy silane, di-t-butyl dimethoxysilane, tertiary hexyl trimethoxy silane, tert-butyl trimethoxy silane, uncle oneself
Base trimethoxy silane；Ethers for example can be：Dimethyl ether, Anaesthetie Ether, dipropyl ether, isopropyl sec-butyl ether, Zhong Ding
Base ether isoamyl ether, isopropyl amyl ether, sec-butyl isoamyl ether etc..
In an embodiment of the present invention, it is described by the second overhead components carry out the process of liquid-liquid extraction cleaning with alcohol, ester or
Its aqueous solution is used as extraction cleaning agent.
The solvent is reclaimed from the mixture comprising unreacted 1- butene monomers can specifically wrap that is, described
Include：The mixture comprising unreacted 1- butene monomers is fed to carries out rectifying separation in first rectifying column, obtain first
Bottom of towe component；Then the first bottom of towe component is carried out into rectifying separation again, obtains the second overhead components；Then with ester, alcohol or its
The aqueous solution carries out liquid-liquid extraction cleaning as extraction cleaning agent to the second overhead components, then residual with solid adsorbent Adsorption
The extraction cleaning agent for staying can obtain the qualified solvent of purity.
In still another embodiment of the process, the process for the second overhead components being carried out into liquid-liquid extraction cleaning can be -5~40
Realized at a temperature of DEG C, for example, can be realized at a temperature of 0~35 DEG C, 10~30,15~25.
In still another embodiment of the process, it is also that liquid-liquid extraction is clear after the second overhead components being carried out into liquid-liquid extraction cleaning
Second overhead components solid adsorbent adsorption treatment after washing, with adsorbing and removing residual extraction cleaning agent in a solvent.
In the embodiment of the present invention, solid adsorbent is bigger serface, the big porous adsorbent of pore volume class, adsorbable filtering
Unwanted part in gas or liquid.Applicable solid adsorbent for example can be molecular sieve, natural Rare Earth Mine etc..It is actual to answer
In, used according to material to be adsorbed pore size in itself, reached the adsorbing and removing effect of needs.
In order to be more clearly understood from the method for continuous production PB Polybutene-1 provided in an embodiment of the present invention, hereafter enter one
Step is elaborated.
Method for continuous production PB Polybutene-1 provided in an embodiment of the present invention can specifically include following steps：
Step S1, butene-1 monomer and catalyst, auxiliary agent and external electron donor sequentially add polymer reactor,
Temperature is 10~85 DEG C, pressure is 0.2~2.6MPa, reaction time is to carry out polymerisation under conditions of 1~4 hour；
Step S2, by butene-1 monomer, catalyst, auxiliary agent, external electron donor according to identical ratio in S1 start into
Material, proceeds polymerisation, while releasing reaction mass from the polymer reactor, the material was both poly- including target product
Butene-1, the also mixture including being made up of unreacted butene-1 monomer, solvent, impurity etc..
Wherein, auxiliary agent was dissolved with solvent in advance before being added in polymer reactor, and solvent has brought reactant into therewith
In material, the solvent is reclaimed from said mixture, the process for reclaiming the solvent can specifically include：
Mixture is carried out into rectifying separation, the first bottom of towe component is obtained；The first bottom of towe component is carried out into rectifying separation,
Obtain the second overhead components；Second overhead components are carried out into liquid-liquid extraction cleaning, solid adsorbent absorption to be recycled
Solvent.The solvent that the recovery is obtained returns to for auxiliary agent the dissolution aids before being added in polymer reactor.
A kind of method of continuous production PB Polybutene-1 is the embodiment of the invention provides, the continuous life of PB Polybutene-1 is realized
Produce, be first 10~85 DEG C, the condition that pressure is 0.2~2.6MPa, reaction time is 1~4 hour in temperature specifically
Lower startup polymerisation, makes polymerization reaction system reach the equalization point of stabilization so that the material in polymer reactor has good
Can transporting；Then each reaction raw materials of butene-1 monomer, catalyst, auxiliary agent, external electron donor according to identical ratio in S1
Example starts charging, proceeds polymerisation, while release a certain amount of reaction mass from polymer reactor, so as to by
Constantly charging discharging simultaneously repeats polymerisation, obtains PB Polybutene-1 product under the equilibrium state, realizes PB Polybutene-1
Continuous and stable production, it is ensured that obtain the continual and steady of product quality, effectively eliminates the mass deviation between product when batch is produced,
Meet the raw materials requirement of downstream product processing enterprise.Meanwhile, in the method, using unique processing method, solvent is returned
Receive and remove the objectionable impurities being enriched with system, enabling recycle solvent and do not interfere with polymerisation.
Additionally, in method provided in an embodiment of the present invention, can be using hydrogen as molecular weight regulator, with needed for obtaining
Isotactic polybutylene-1-1 molecular weight.
Another aspect, as shown in figure 1, the embodiment of the present invention provides a kind of device for continuous production PB Polybutene-1, institute
Stating device includes：
Polymer reactor 10, for 1- butene monomers and catalyst, external electron donor, auxiliary agent in the polymer reactor
Generation polymerisation, releases part reaction mass, mixing of the removal comprising unreacted 1- butene monomers from the reaction mass
Thing, to obtain isotactic polybutylene-1-1, wherein, the auxiliary agent is molten with solvent in advance before being added in the polymer reactor
Solution；
First rectifying column 20, the mixture comprising unreacted 1- butene monomers is separated for rectifying, obtains the first tower
Bottom component；
Second distillation column 30, the first bottom of towe component is separated for rectifying, obtains the second overhead components；
Extraction tower 40, for carrying out liquid-liquid extraction cleaning to second overhead components, the solvent being recycled, described time
The solvent of receipts is used to dissolve the auxiliary agent before auxiliary agent is added to the polymer reactor.
In an embodiment of the present invention, described device can also include adsorption tower 50, after being cleaned to liquid-liquid extraction
Second overhead components carry out solid adsorbent adsorption treatment.
It is understood that provided in an embodiment of the present invention for the continuous device for producing PB Polybutene-1, extraction tower may be used also
Be it is any can realize the chemical industry equipment that liquid-liquid extraction is cleaned, adsorption tower can also be any and can realize by solid adsorbant
Agent removes the chemical industry equipment of extraction cleaning agent from solvent.
In an embodiment of the present invention, in extraction tower 40, carried out at a temperature of -5~40 DEG C.
During the body continuous polymerization technique of PB Polybutene-1, due to the requirement by promoter addition and auxiliary agent characteristic,
Auxiliary agent can be dissolved or be diluted with some solvents in production, realized that auxiliary agent is continuous, precisely add, thus added auxiliary agent mistake
Cheng Zhonghui brings a small amount of solvent into, and in process of production, the objectionable impurities that polymerization process is produced can be enriched with a solvent, not only can
Influence polymerisation, can also make catalyst poisoning when serious, prevent reaction from continuing.Typically in process of production directly as residual
Liquid is discharged, and is wasted the energy and is increased environmental burden.
A kind of device for continuous production PB Polybutene-1 provided in an embodiment of the present invention, can continuously be produced by the device
Isotactic polybutylene-1-1, by the mixture comprising solvent, objectionable impurities pass sequentially through first rectifying column 20, Second distillation column 30,
Extraction tower 40, adsorption tower 50, remove objectionable impurities, and the extraction cleaning agent that removing is remained, and have obtained qualified solvent, can be again
It is added to 10 in polymer reactor in order to auxiliary agent for dissolution aids, realizes the use of the circulation of solvent, is reclaimed and eliminate
Objectionable impurities in system, it is to avoid solvent is recycled and causes polymerisation unstable.
The above, specific embodiment only of the invention, but protection scope of the present invention is not limited thereto, and it is any
Those familiar with the art the invention discloses technical scope in, change or replacement can be readily occurred in, should all contain
Cover within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (9)
1. it is a kind of for the continuous method for producing PB Polybutene-1, it is characterised in that methods described includes：By 1- butene monomers with urge
Agent, external electron donor, auxiliary agent are sequentially added in polymer reactor there is polymerisation, release part reaction mass, from described
Mixture of the removal comprising unreacted 1- butene monomers, obtains isotactic polybutylene-1-1 in reaction mass, wherein, the auxiliary agent exists
Advance solvent dissolving before in polymer reactor is added to, is reclaimed from the mixture comprising unreacted 1- butene monomers
The solvent:
The mixture comprising unreacted 1- butene monomers is carried out into rectifying separation, the first bottom of towe component is obtained；
The first bottom of towe component is carried out into rectifying separation, the second overhead components are obtained；
Second overhead components are carried out into the solvent that liquid-liquid extraction cleaning is recycled；
The recovered solvent is returned for dissolving the auxiliary agent before the auxiliary agent is added in polymer reactor.
2. method according to claim 1, it is characterised in that second overhead components are carried out into liquid-liquid extraction cleaning
Afterwards, second overhead components after liquid-liquid extraction is cleaned carry out solid adsorbent adsorption treatment.
3. method according to claim 1, it is characterised in that described that second overhead components are carried out into liquid-liquid extraction cleaning
Process is realized at a temperature of -5~40 DEG C.
4. method according to claim 1, it is characterised in that described that second overhead components are carried out into liquid-liquid extraction cleaning
Process is using alcohol, ester or its aqueous solution as extracting and washing agent.
5. method according to claim 2, it is characterised in that the solid adsorbent is molecular sieve.
6. method according to claim 1, it is characterised in that methods described also includes from described comprising unreacted 1- butylene
Unreacted 1- butene monomers are reclaimed in the mixture of monomer, the unreacted 1- butene monomers of recovery are back to polymer reactor
In.
7. it is a kind of for the continuous device for producing isotactic polybutylene-1-1, it is characterised in that described device includes：
Polymer reactor, occurs poly- for 1- butene monomers and catalyst, external electron donor, auxiliary agent in the polymer reactor
Reaction is closed, part reaction mass is released, mixture of the removal comprising unreacted 1- butene monomers from the reaction mass, with
To isotactic polybutylene-1-1, wherein, the auxiliary agent was dissolved with solvent in advance before being added in the polymer reactor；
First rectifying column, the mixture comprising unreacted 1- butene monomers is separated for rectifying, obtains the first bottom of towe component；
Second distillation column, the first bottom of towe component is separated for rectifying, obtains the second overhead components；
Extraction tower, for carrying out liquid-liquid extraction cleaning to second overhead components, the solvent being recycled, the recovery it is molten
Agent is returned for dissolving the auxiliary agent before auxiliary agent is added to the polymer reactor.
8. device according to claim 7, it is characterised in that described device also includes adsorption tower, for liquid-liquid extraction
The second overhead components after cleaning carry out solid adsorbent adsorption treatment.
9. device according to claim 7, it is characterised in that right at a temperature of -5~40 DEG C in the extraction tower
Second overhead components carry out liquid-liquid extraction cleaning.
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|---|---|---|---|---|
| CN101880346A (en) * | 2010-07-19 | 2010-11-10 | 曹斌豫 | Method for synthesizing high-content cis-1,4-polyisoprene |
| CN102234356A (en) * | 2010-04-30 | 2011-11-09 | 青岛伊科思新材料股份有限公司 | Method for producing rare-earth isoprene butadiene rubber |
| CN105452304A (en) * | 2013-07-30 | 2016-03-30 | 大林产业株式会社 | Device and method for re-circulating raw material used when manufacturing polybutene |
| CN106243255A (en) * | 2016-07-29 | 2016-12-21 | 山东省滕州瑞达化工有限公司 | Isotactic polybutylene-1 1 continuous producing method |
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- 2017-02-27 CN CN201710109389.7A patent/CN106832070B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102234356A (en) * | 2010-04-30 | 2011-11-09 | 青岛伊科思新材料股份有限公司 | Method for producing rare-earth isoprene butadiene rubber |
| CN101880346A (en) * | 2010-07-19 | 2010-11-10 | 曹斌豫 | Method for synthesizing high-content cis-1,4-polyisoprene |
| CN105452304A (en) * | 2013-07-30 | 2016-03-30 | 大林产业株式会社 | Device and method for re-circulating raw material used when manufacturing polybutene |
| CN106243255A (en) * | 2016-07-29 | 2016-12-21 | 山东省滕州瑞达化工有限公司 | Isotactic polybutylene-1 1 continuous producing method |
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