CN104761659A - Method for preparing butyl rubber solution for halogenation, and apparatus thereof - Google Patents
Method for preparing butyl rubber solution for halogenation, and apparatus thereof Download PDFInfo
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- CN104761659A CN104761659A CN201410003515.7A CN201410003515A CN104761659A CN 104761659 A CN104761659 A CN 104761659A CN 201410003515 A CN201410003515 A CN 201410003515A CN 104761659 A CN104761659 A CN 104761659A
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- isobutylene rubber
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Abstract
The invention discloses a method for preparing a butyl rubber solution for halogenations. The method comprises the following steps: 1, allowing a butyl rubber slurry to contact with hexane steam in a flash evaporation kettle to obtain a gas phase product and a hexane solution of butyl rubber; and 2, directly introducing the hexane solution of butyl rubber obtained in step 1 into a guide sieve tray tower, and allowing the hexane solution of butyl rubber to contact with the hexane steam in a countercurrent manner in order to directly obtain the butyl rubber hexane solution for halogenation. The method allows the rubber solution for halogenation to be directly obtained by removing unreacted monomers residual in the hexane solution of butyl rubber through the high efficiency guide sieve tray tower, so the production flow of halogenated butyl products is simplified, and the production cost is reduced.
Description
Technical field
The present invention relates to a kind of method preparing butyl rubber solution, more specifically, relate to a kind of preparation method of halogenation isoprene-isobutylene rubber hexane solution.
Background technology
Halogenated butyl rubber (HIIR) is on the basis keeping the original performance of isoprene-isobutylene rubber, fast with vulcanization rate, can with general purpose resilient body covulcanization, adhesive property is good, has the features such as better thermotolerance and becomes the preferred material of producing tubeless meridian tyre airtight layer.The production technology of current halogenated butyl rubber mainly adopts solution method to carry out, and namely adopts saturated alkane (as hexane) to obtain certain density glue for dissolution with solvents isoprene-isobutylene rubber, then carries out halogenating reaction.The production process of solution method halogenated butyl rubber comprises three parts: the production of (1) basic isoprene-isobutylene rubber; (2) glue carries out halogenating reaction; (3) cohesion of product is dry.Different companies, because production technology level is different, the technological process adopted and process detail are also different, and wherein main difference concentrates in glue preparation technology.For glue preparation technology, then water-setting is had to gather sol method and hexane stripping sol method.Generally, can be used in the glue (isoprene-isobutylene rubber hexane solution) of halogenating reaction, require that isoprene-isobutylene rubber content is 10-20wt%, and the content of unreacted monomer is low.But prior art does not reach the gelatin concentration of regulation, therefore, follow-up concentrating must be carried out to glue, the glue for halogenation can be obtained.
It is first obtain micelle aqueous slurry by water steam stripping coacervation to dehydrate then with hexane colloidal sol formation glue that water-setting gathers sol method again.In the glue adopting this legal system standby, water content is higher, and cannot thoroughly remove, therefore the halogenating reaction process influence to follow-up is larger, bromine utilization ratio is not only caused to decline, more seriously equipment corrosion excessive velocities, thus cause the unplanned parking of device or stopping production, affect quality product and production efficiency.
Have document to disclose and a kind of adopt unreacted monomer and solvent monochloro methane in hot hexane stripping butyl rubber slurry, continuously production halogenation with or prepare the method for glue of latex, i.e. hexane stripping sol method.This method comprises: the butyl rubber slurry of formation is passed into flash vaporization kettle, overheated hexane also passes into flash vaporization kettle in vapour form simultaneously, hexane vapor discharges enough heats and to gasify most monochloro methane and unreacted monomer, isoprene-isobutylene rubber dissolves rapidly and forms hexane solution in hexane simultaneously, the hexane solution being dissolved with isoprene-isobutylene rubber enters glue stripping tower top, the hexane vapor risen with adverse current while glue moves to tower bottom flow contacts carries out mass transfer, to remove unsaturated monomer residual in glue.Substantially the isoprene-isobutylene rubber hexane solution not containing olefinic monomer is discharged bottom stripping tower, enters the second flash vaporization kettle.In the second flash vaporization kettle, the evaporation of part hexane makes butyl rubber solution be concentrated into the gelatin concentration of regulation, and the butyl rubber solution after then concentrating is used for follow-up reaction, as halogenating reaction.Whole technological equipment investment is high, technical process is long.
Still need technique simple and can in efficient removal butyl rubber solution unreacted monomer to prepare the method for halogenation butyl rubber solution.
Summary of the invention
In view of above-mentioned prior art situation, present inventor has carried out research extensively and profoundly at rubber materials and chemical industry rectification and purification field, provide a kind of technique simple and can unreacted monomer in efficient removal butyl rubber solution, directly obtain the method for the isoprene-isobutylene rubber hexane solution of high density (10-20wt%), directly obtain the isoprene-isobutylene rubber hexane solution that can be used for halogenating reaction.
According to an aspect of the present invention, provide a kind of method preparing halogenation butyl rubber solution, it comprises:
Step I. butyl rubber slurry is contacted with hexane steam in flash vaporization kettle, obtains the hexane solution containing isoprene-isobutylene rubber,
The hexane solution of the isoprene-isobutylene rubber obtained in step I is directly passed into guide sieve-plate tower by step I i., contacts in guide sieve-plate tower with hexane steam is reverse, directly obtains the isoprene-isobutylene rubber hexane solution that can be used for halogenation.
In a specific embodiment of the method for the invention, in the isoprene-isobutylene rubber hexane solution obtained in described step I i, isoprene-isobutylene rubber content is 10-20wt%.In another is specifically implemented, in the hexane solution of the isoprene-isobutylene rubber obtained in described step I i, unreacted monomer content is lower than 1ppm.
According to method of the present invention, the flash vaporization kettle still top in described step I obtains gas-phase product, and wherein, gas-phase product comprises unreacted monomer, haloalkane thinner and hexane.
According to a preferred embodiment of the method for the invention, butyl rubber slurry passes into the charging position of charging position higher than hexane steam of flash vaporization kettle.As hexane can pass in the bottom of flash vaporization kettle, butyl rubber slurry passes on the top of flash vaporization kettle.
According to another preferred embodiment of the method for the invention, the hexane solution containing isoprene-isobutylene rubber obtained in step I passes into the charging position of charging position higher than hexane steam of guide sieve-plate tower.As hexane can pass in the bottom of guide sieve-plate tower, the hexane solution containing isoprene-isobutylene rubber passes on the top of guide sieve-plate tower.
According to method of the present invention, the service temperature of described flash vaporization kettle is 30-70 DEG C, and working pressure is 0.1-0.5MPa.The temperature of described guide sieve-plate tower is 30-150 DEG C, preferred 50-90 DEG C; Pressure is 5-500KPa, preferred 20-200KPa.
According to method provided by the invention, overcome deficiency of the prior art, the combination of guide sieve-plate tower is added by flash vaporization kettle, just directly can obtain the isoprene-isobutylene rubber hexane solution that concentration is 10-20wt%, described solution can be directly used in halogenating reaction, and without the need to other enrichment step, simplify the technological process of production, reduce facility investment, reduce production cost, improve economic benefit.
According to another aspect of the present invention, provide a kind of device utilizing above-mentioned method to prepare halogenation butyl rubber solution, comprising:
Flash vaporization kettle,
The guide sieve-plate tower be directly connected with flash vaporization kettle.
According to device provided by the invention, the isoprene-isobutylene rubber hexane solution obtained at the bottom of guide sieve-plate tower tower can be directly used in halogenating reaction.
According to a specific embodiment of device of the present invention, from the isoprene-isobutylene rubber hexane solution that described Linde sieve tray tower bottom directly obtains, isoprene-isobutylene rubber concentration is 10-20wt%.In another specific examples, from the isoprene-isobutylene rubber hexane solution that described Linde sieve tray tower bottom directly obtains, unreacted monomer content is lower than 1ppm.
Also comprise some connecting tubes according to device of the present invention, do not elaborate again herein.Described in a specific examples, the service temperature of flash vaporization kettle is 30-70 DEG C, and working pressure is 0.1-0.5MPa.The temperature of described guide sieve-plate tower is 30-150 DEG C, preferred 50-90 DEG C; Pressure is 5-500KPa, preferred 20-200KPa.
Utilize method and apparatus provided by the invention, butyl rubber slurry is passed into flash vaporization kettle, overheated hexane also passes into flash vaporization kettle in vapour form simultaneously, the heat utilizing hexane vapor to discharge gasifies most haloalkane thinner (as monochloro methane) and unreacted monomer, and isoprene-isobutylene rubber dissolves rapidly and forms hexane solution in hexane simultaneously.The hexane solution being dissolved with isoprene-isobutylene rubber is sent into high-efficiency guide sieve-plate tower by pump or dependence pressure reduction, residual unreacted monomer and haloalkane thinner (as monochloro methane) in removing glue.Obtain substantially not containing unreacted monomer and the isoprene-isobutylene rubber hexane solution that concentration is 10-20% directly carries out halogenating reaction.
According to method and apparatus provided by the invention, employing guide sieve-plate tower removes the unreacted monomer in the hexane solution of isoprene-isobutylene rubber, not only plate pressure drop is low, efficiency is high, can realize saving energy and reduce the cost, and be specially adapted to high sticky material, can effectively overcome the defects such as stifled tower, liquid flooding, entrainment, make substantially to remove the unreacted monomer in butyl rubber solution and monochloro methane completely, the solution obtained at the bottom of tower directly can carry out halogenating reaction.
According to method and apparatus provided by the invention, butyl rubber slurry is passed into flash vaporization kettle, contact and mass transfer with hexane steam is reverse, remove the most of unreacted monomer in butyl rubber slurry and haloalkane thinner, isoprene-isobutylene rubber simultaneously in slurry is dissolved in hexane rapidly, obtain the hexane solution containing isoprene-isobutylene rubber, meanwhile, from the flash vaporization kettle hexane solution containing isoprene-isobutylene rubber out still containing unreacted monomer and haloalkane thinner; Hexane solution containing isoprene-isobutylene rubber is directly passed into guide sieve-plate tower, utilize the structure of guide sieve-plate tower, viscosity can be removed containing unreacted monomer residual in the hexane solution of isoprene-isobutylene rubber and monochloro methane, the content of unreacted monomer in the hexane solution of the isoprene-isobutylene rubber obtained at the bottom of tower is made to be reduced to below 1ppm, the concentration of the hexane solution of isoprene-isobutylene rubber is enough high simultaneously, as being 10-20%, directly halogenating reaction can be carried out.
According to method and apparatus of the present invention, the hexane solution that can carry out the isoprene-isobutylene rubber of halogenating reaction directly can be obtained, and without the need to the step of other extra treatment soln.Compare with prior art, technical process is simple, and the unreacted monomer in energy efficient removal butyl rubber solution, reduce energy consumption and material consumption; Simplify the Production Flow Chart of halobutyl, reduce production cost.
These and other purposes, features and advantages of the present invention, after considering the present invention in conjunction with following accompanying drawing entirety, will be easy to as those of ordinary skill is understood.
Accompanying drawing explanation
Fig. 1 is process flow sheet according to an embodiment of the invention.
Embodiment
In embodiments of the present invention, step I. adopt the butyl rubber slurry obtained as slurry polymerization to pass into flash vaporization kettle, overheated hexane also passes into flash vaporization kettle in vapour form simultaneously, the heat utilizing hexane vapor to discharge gasifies most monochloro methane and unreacted monomer, and isoprene-isobutylene rubber dissolves rapidly and forms hexane solution in hexane simultaneously; Then the hexane solution being dissolved with isoprene-isobutylene rubber is sent into guide sieve-plate tower (preferably adopting high-efficiency guide sieve-plate tower) as relied on pressure reduction by step I i., at the bottom of tower, pass into hexane vapor simultaneously, glue and hexane vapor counter current contact is made to carry out mass transfer, residual unreacted monomer and monochloro methane in removing solution.Finally by unreacted monomer content lower than 1ppm and the isoprene-isobutylene rubber hexane solution that concentration is 10-20wt% directly carries out halogenating reaction.
In another embodiment of the inventive method, step I. adopt the butyl rubber slurry obtained as slurry polymerization to pass into flash vaporization kettle, overheated hexane also passes into flash vaporization kettle in vapour form simultaneously, the heat utilizing hexane vapor to discharge gasifies most monochloro methane and unreacted monomer, and isoprene-isobutylene rubber dissolves rapidly and forms hexane solution in hexane simultaneously; Then step I i. will be dissolved with the hexane solution of isoprene-isobutylene rubber by being pumped into efficient sieve plate tower, residual unreacted monomer and monochloro methane in removing glue.Finally by unreacted monomer content lower than 1ppm and the isoprene-isobutylene rubber hexane solution that concentration is 10-20wt% directly carries out halogenating reaction.
Term " isoprene-isobutylene rubber " used in the context of the present invention should be interpreted as and refer to that carbonatoms is the isomeric olefine of 4-8, as iso-butylene, and carbonatoms is the conjugated diene of 4-8, as the multipolymer of isoprene.Wherein the massfraction of isomeric olefine is 60-99.5%, and the massfraction of conjugated diene is 40-0.5%.Unreacted monomer in the present invention, just refers to that carbonatoms is the isomeric olefine of 4-8, and as iso-butylene, and carbonatoms is the conjugated diene of 4-8, as isoprene.The production of isoprene-isobutylene rubber adopts slurry process usually, is thinner with halogenated alkane, and as monochloro methane, temperature of reaction controls at-90 DEG C ~-107 DEG C.
It is thinner that butyl rubber slurry in the present invention refers to halogenated alkane, take carbonatoms as the conjugated diene that the isomeric olefine of 4-8 and carbonatoms are 4-8 is monomer, adopts the polymer slurries that slurry polymerization obtains.
Before halogenating butyl rubber, first isoprene-isobutylene rubber must be dissolved in varsol and form solution.According to method provided by the invention, the glue of halogenating reaction directly can be obtained.Compared with gathering sol method with water-setting, not only eliminate basic isoprene-isobutylene rubber micelle aqueous slurry dehydration drying system, also owing to there is not the circulation of water in system and eliminating the dehumidification system of monochloro methane, production technique is simplified.
Also remain a small amount of unreacted monomer and monochloro methane in the isoprene-isobutylene rubber hexane solution formed in flash vaporization kettle, need to be removed, otherwise remain in monomer in glue and to react formation halogenide with halogen.These halogenide finally can remain in the product, not only affect the content of halogen index of product, and especially bromide can become lacrymator, cause comparatively burden to aftertreatment packaging and mixed refining process.
By the isoprene-isobutylene rubber hexane solution remaining a small amount of unreacted monomer and monochloro methane is passed into guide sieve-plate tower, residual unreacted monomer and monochloro methane in viscous glue solution (or claiming the hexane solution of isoprene-isobutylene rubber) can be removed.The concrete structure of (efficiently) guide sieve-plate tower can with reference to raw etc. the document of Lie group: high-efficiency guide sieve-plate tower removes the technological transformation of VAc monomer rectifying to PVAc, and chemical industry is in progress, 2011, the 30th volume supplementary issue, 783-786 page.The column plate of high-efficiency guide sieve-plate tower has the pilot hole of some amount, makes there is prograding forward from the gas of pilot hole level ejection to liquid plate, effectively eliminate gradient of liquid level and backmixing of liquid phase.On the other hand, the bubbling arranging sloping platform shape projection in the liquid-inlet district of column plate promotes device, makes liquid one enter column plate and is namely activated, cause the favourable condition of whole column plate bubbling, effectively reduces plate pressure drop simultaneously, improves plate efficiency.Adopt the favourable configurations of guide sieve-plate tower, the content of unreacted monomer in the glue obtained at the bottom of tower can be made to be reduced to below 1ppm, gelatin concentration is enough high simultaneously, as being 10-20%, directly can carry out halogenating reaction.
The present invention compared with prior art, mainly contains following beneficial effect:
(1) directly adopt hot hexane to remove monochloro methane and unreacted monomer, directly can obtain the glue of halogenating reaction, production technique is simplified.
(2) efficient guide sieve-plate tower is adopted to remove unreacted monomer in glue and monochloro methane, not only plate pressure drop is low, efficiency is high, can realize saving energy and reduce the cost, and be specially adapted to high sticky material, can effectively overcome the defects such as stifled tower, liquid flooding, entrainment, make the concentration of solution in tower can up to 20wt%, the glue obtained at the bottom of tower directly can carry out halogenating reaction, simplify the production process of halobutyl, reduce production cost.
Hereafter will 1 pair of the inventive method be described further by reference to the accompanying drawings.As shown in Figure 1, the inventive method equipment therefor mainly comprises flash vaporization kettle I and guide sieve-plate tower II.In flash vaporization kettle I, agitator is housed.Should be understood that in order to clear object, Fig. 1 does not provide the details of some parts or device structure, because this type of details is conventional and known to those skilled in the art.In addition, in order to clearly describe the present invention, control or the proofing unit of many chemical field routines is also eliminated in FIG.
First, polymer slurries 1 is sent into flash vaporization kettle I.The temperature of flash vaporization kettle I is enough high, with the haloalkane thinner (as monochloro methane) that effectively gasifies.The service temperature of flash vaporization kettle I is at 30 ~ 70 DEG C, and as 55 DEG C, working pressure is between 0.1 ~ 0.5MPa, and as 0.14MPa, overheated hexane vapor 2 also sprays into flash vaporization kettle I simultaneously.Hexane vapor discharges enough heat gasification monochloro methanes.The amount of vaporization of haloalkane thinner (as monochloro methane) is controlled by the temperature and pressure of adjustment flash vaporization kettle I, make a large amount of haloalkane thinner (as monochloro methane) gasifications, nearly 70% ~ 99%(is as 90%) haloalkane thinner (as monochloro methane) removed by evaporation, simultaneously isoprene-isobutylene rubber dissolves in hexane rapidly.Gas-phase product 3(comprises the haloalkane thinner (as monochloro methane) of gasification and unreacted monomer and part hexane) flow out from still top, the hexane solution (glue) 4 being simultaneously dissolved with isoprene-isobutylene rubber enters (efficiently) guide sieve-plate tower II.Hexane vapor 2 ' enters and upwards flows at the bottom of tower, contact with the glue 4 flowed downward and carry out mass transfer, unreacted monomer residual in glue and haloalkane thinner (as monochloro methane) rise with hexane vapor, flow out from tower top with the form of gas-phase product 5, obtain the isoprene-isobutylene rubber hexane solution 6 of unreacted monomer content lower than 1ppm at the bottom of tower, isoprene-isobutylene rubber hexane solution 6 concentration is 10-20%.The temperature of high-efficiency guide sieve-plate tower II should control to make polymer degradation, is usually no more than 150 DEG C, and working pressure is 5-500KPa.
Hereafter by reference example, the present invention is specifically described, but described embodiment does not form any restriction to the scope of the invention.
Embodiment 1
The butyl rubber slurry adopting slurry polymerization to obtain is passed into the flash vaporization kettle that volume is 120m3, and the inlet amount of butyl rubber slurry is 21681.3kg/h, consists of: monochloro methane 77.0%, isoprene-isobutylene rubber 18.4%, iso-butylene 4.4%, isoprene 0.2%.The overheated hexane vapor of 150 DEG C is also passed into flash vaporization kettle.55 DEG C, carry out flash distillation under 0.13MPa, the amount of vaporization of monochloro methane is 92%, under stirring, isoprene-isobutylene rubber dissolves and forms glue in hexane, the flow of glue is 43961.5kg/h, consist of hexane 87.5%, monochloro methane 3.1%, isoprene-isobutylene rubber 9.1%, iso-butylene 0.3%, isoprene 353ppm.Under the effect of pressure reduction, glue enters the top of high-efficiency guide sieve-plate tower, passes into the overheated hexane vapor of 150 DEG C at the bottom of tower, the number of theoretical plate of high-efficiency guide sieve-plate tower 15 pieces, the 3rd piece of charging.The operational condition of tower and tower top, material composition at the bottom of tower are respectively in table 1 and table 2.In glue, the content of isoprene is 0.8ppm, and gelatin concentration is 10%.The glue obtained at the bottom of tower directly carries out halogenating reaction.
The operational condition of table 1 high-efficiency guide sieve-plate tower
Table 2 tower top and materials at bottom of tower composition
Embodiment 2
The butyl rubber slurry adopting slurry polymerization to obtain is passed into the flash vaporization kettle that volume is 120m3, and the inlet amount of butyl rubber slurry is 21681.3kg/h, consists of: monochloro methane 77.0%, isoprene-isobutylene rubber 18.4%, iso-butylene 4.4%, isoprene 0.2%.The overheated hexane vapor of 150 DEG C is also passed into flash vaporization kettle.40 DEG C, carry out flash distillation under 0.13MPa, the amount of vaporization of monochloro methane is 75%, under stirring, isoprene-isobutylene rubber dissolves and forms glue in hexane, the flow of glue is 64152.8kg/h, consist of hexane 86.6%, monochloro methane 6.5%, isoprene-isobutylene rubber 6.2%, iso-butylene 0.6%, isoprene 485ppm.With pump, glue is sent into high-efficiency guide sieve-plate tower, the number of theoretical plate of guide sieve-plate tower 14 pieces, the 5th piece of charging.The operational condition of tower and tower top, material composition at the bottom of tower are respectively in table 1 and table 2.In glue, the content of isoprene is 0.11ppm, and gelatin concentration is 15%.The glue obtained at the bottom of tower directly carries out halogenating reaction.
The operational condition of table 1 high-efficiency guide sieve-plate tower
Table 2 tower top and materials at bottom of tower composition
Embodiment 3
The butyl rubber slurry adopting slurry polymerization to obtain is passed into the flash vaporization kettle that volume is 120m3, and the inlet amount of butyl rubber slurry is 21681.3kg/h, consists of: monochloro methane 77.0%, isoprene-isobutylene rubber 18.4%, iso-butylene 4.4%, isoprene 0.2%.The overheated hexane vapor of 150 DEG C is also passed into flash vaporization kettle.70 DEG C, carry out flash distillation under 0.25MPa, the amount of vaporization of monochloro methane is 82%, under stirring, isoprene-isobutylene rubber dissolves and forms glue in hexane, the flow of glue is 54277.0kg/h, consist of hexane 86.8%, monochloro methane 5.3%, isoprene-isobutylene rubber 7.4%, iso-butylene 0.5%, isoprene 432ppm.Under the effect of pressure reduction, glue enters the top of high-efficiency guide sieve-plate tower, the number of theoretical plate of high-efficiency guide sieve-plate tower 10 pieces, the 3rd piece of charging.The operational condition of tower and tower top, material composition at the bottom of tower are respectively in table 1 and table 2.In glue, the content of isoprene is 0.3ppm, and gelatin concentration is 20%.The glue obtained at the bottom of tower directly carries out halogenating reaction.
The operational condition of table 1 high-efficiency guide sieve-plate tower
Table 2 tower top and materials at bottom of tower composition
Can be learnt by above data, according to method provided by the invention, effectively can remove the unreacted monomer in butyl rubber slurry and haloalkane thinner, in the hexane solution of the isoprene-isobutylene rubber obtained, the concentration of isoprene-isobutylene rubber is high, the content of unreacted monomer is low, can be directly used in halogenating reaction.
It should be noted that above-described embodiment only for explaining the present invention, not forming any limitation of the invention.By referring to exemplary embodiments, invention has been described, but to should be understood to word wherein used be descriptive and explanatory vocabulary, instead of limited vocabulary.Can modify the present invention by the scope being defined in the claims in the present invention, and the present invention be revised not deviating from scope and spirit of the present invention.Although the present invention wherein described relates to specific method, material and embodiment, and do not mean that the present invention is limited to particular case disclosed in it, on the contrary, easily extensible of the present invention is to other all methods and applications with identical function.
Claims (10)
1. prepare a method for halogenation butyl rubber solution, it comprises:
Step I. butyl rubber slurry is contacted with hexane steam in flash vaporization kettle, obtains the hexane solution containing isoprene-isobutylene rubber;
The hexane solution containing isoprene-isobutylene rubber obtained in step I is directly passed into guide sieve-plate tower by step I i., contacts, directly obtain the isoprene-isobutylene rubber hexane solution for halogenation in guide sieve-plate tower with hexane steam is reverse.
2. method according to claim 1, is characterized in that, in the isoprene-isobutylene rubber hexane solution obtained in described step I i, isoprene-isobutylene rubber content is 10-20wt%.
3. method according to claim 1 and 2, is characterized in that, in the isoprene-isobutylene rubber hexane solution obtained in described step I i, unreacted monomer content is lower than 1ppm.
4. according to the method in right 1-3 described in any one, it is characterized in that, the service temperature of described flash vaporization kettle is 30-70 DEG C, and working pressure is 0.1-0.5MPa.
5. according to the method in claim 1-4 described in any one, it is characterized in that, the temperature of described guide sieve-plate tower is 30-150 DEG C, preferred 50-90 DEG C; Pressure is 5-500KPa, preferred 20-200KPa.
6. utilize the method in claim 1-5 described in any one to prepare a device for halogenation butyl rubber solution, comprising:
Flash vaporization kettle,
The guide sieve-plate tower be directly connected with flash vaporization kettle.
7. device according to claim 6, is characterized in that, the isoprene-isobutylene rubber hexane solution directly obtained from described Linde sieve tray tower bottom is directly used in halogenating reaction.
8. the device according to claim 6 or 7, is characterized in that, directly obtains isoprene-isobutylene rubber hexane solution that unreacted monomer content is lower than 1ppm from described Linde sieve tray tower bottom, and isoprene-isobutylene rubber content is 10-20wt%.
9. according to the device in right 6-8 described in any one, it is characterized in that, the service temperature of described flash vaporization kettle is 30-70 DEG C, and working pressure is 0.1-0.5MPa.
10. according to the device in claim 6-9 described in any one, it is characterized in that, the temperature of described guide sieve-plate tower is 30-150 DEG C, preferred 50-90 DEG C; Pressure is 5-500KPa, preferred 20-200KPa.
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| CN109942841A (en) * | 2019-03-27 | 2019-06-28 | 山东京博石油化工有限公司橡胶分公司 | A kind of butyl rubber solution and preparation method thereof |
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| CN111548436A (en) * | 2020-04-26 | 2020-08-18 | 浙江信汇新材料股份有限公司 | Preparation method of butyl rubber base rubber solution for halogenation reaction |
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