CN103044598B - Method for flash evaporating and concentrating of liquid ethylene propylene rubber - Google Patents
Method for flash evaporating and concentrating of liquid ethylene propylene rubber Download PDFInfo
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- CN103044598B CN103044598B CN201110315141.9A CN201110315141A CN103044598B CN 103044598 B CN103044598 B CN 103044598B CN 201110315141 A CN201110315141 A CN 201110315141A CN 103044598 B CN103044598 B CN 103044598B
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Abstract
The invention relates to a method for flash evaporating and concentrating of liquid ethylene propylene rubber. The liquid ethylene propylene rubber which is obtained by a solution method through adopting a hexa certaine solvent is heated in a multiple-effect tubular heater to 140-190 DEG C and then flows into flash evaporation tanks at the flow velocity of 2 meters/second to be subjected to flash evaporation, pressure difference and external supplementary heat are utilized to instantly volatilize the hexa certaine solvent, and the internal temperatures of the flash evaporation tanks are controlled to be between 80 and 140 DEG C; flash evaporation adopts first level, second level or multiple levels; a first-level flash evaporation tank adopts positive pressure or vacuum operation; and when the second-level or the multi-level flash evaporation is carried out, the vacuum degrees of all the flash evaporation tanks are sequentially increased, and flash evaporation tank bodies are sequentially reduced. By the method, the concentration of the liquid ethylene propylene rubber can be increased to 60-90% from 3-12%, and the liquid rubber viscosity is increased to 6000 cp from 500 cp, so that the working requirements of double-screw extruders can be satisfied.
Description
Technical field:
The present invention relates to a kind of simply, the method for the rubber of flash distillation concentrate effectively glue, the method for particularly flash distillation concentrate ethylene-propylene rubber(EPR) glue.
Background technology:
Ethylene-propylene rubber(EPR) is a kind of rubber of excellent performance, its synthetic method has solution method, suspension method and vapor phase process, current vapor phase process does not also have industrialization to report, company larger in the world all adopts solution method to produce, namely adopt with ethene, propylene, Third monomer as raw material, hexane is solvent, under the initiation of Ziegler-Natta catalyst, is that molecular weight regulator synthesizes ethylene-propylene rubber(EPR) with hydrogen.Different according to the processing condition of polyreaction, after reaction, ethylene-propylene rubber(EPR) gelatin concentration is 3 ~ 12%.
When ethylene-propylene rubber(EPR) is produced in solution polymerization, traditional method for recovering solvents has air-extraction and roller desiccating method.What GB804535 proposed is exactly roller desiccating method, the ethylene-propylene rubber(EPR) glue be obtained by reacting is coated onto on the roller that a kind of special substance makes by this method uniformly, roller steam direct heating, can make solvent be down to less than 3% after reaching certain residence time.But this method heating is uneven, easily produces close-burning, affects quality product, without industrial prospect.What US2592814 proposed is air-extraction recycling design, glue is passed in the relatively high liquid medium of another boiling point (being generally water), this medium is heated to certain temperature (higher than solvent boiling point), utilize the energy that it stores, solvent gasification reclaimed, the glue after desolventizing forms small-particle and is isolated to qualified product in high boiling medium.This method is simple to operate, but during industrial enforcement, postorder processing technological flow is long, and required equipment is many, and cause solvent loss amount large, increase energy consumption, production cost is higher simultaneously, also can bring adverse influence to the raising of quality product.
Now ethylene-propylene rubber(EPR) full scale plant mostly adopts water vapor air-extraction, namely using water as high boiling medium desolvation, as previously mentioned, this method solvent loss amount is large, energy consumption is high, therefore in order to avoid long flow path, water vapor air-extraction that equipment is many, utilize the direct desolvation of flash distillation concentrate twin-screw extrusion, volatile content is made to reach criterion of acceptability, just become the developing direction of ethylene-propylene rubber(EPR) solvent recuperation technology, therefore the glue concentrate that obtains after reaction is needed to certain concentration, to make its viscosity reach certain value, the job requirement of forcing machine could be met like this.
Under certain temperature and pressure, require that solvent for use has good solubleness to ethylene-propylene rubber(EPR), require that again low being easy to of boiling point is reclaimed, therefore solution method is produced on ethylene-propylene rubber(EPR) industrialized unit and is mostly adopted hexane to be solvent.
Summary of the invention
The object of the invention is, for taking hexane as the ethylene-propylene rubber(EPR) glue that solvent is produced, to provide a kind of method of flash distillation concentrate ethylene-propylene rubber(EPR) glue.Utilize the direct desolvation hexane of flash distillation concentrate, gelatin concentration is carried to 60% ~ 90%.
The present invention wants the ethylene-propylene rubber(EPR) glue of concentrate, and adopt solution method to produce, hexane is solvent, and after reaction, ethylene-propylene rubber(EPR) gelatin concentration is 3 ~ 12% (mass percents).
The present invention is the ethylene-propylene rubber(EPR) glue that will hexane solvent adopted to be obtained by solution method, 140 ~ 190 DEG C of temperature are heated in multiple-effect tubular heater, enter in flash tank with the flow velocity of 2m/s, utilize the heat of pressure difference and external complement, solvent is volatilized instantaneously reclaimed, gelatin concentration is carried to 60 ~ 90% simultaneously.
The present invention is the ethylene-propylene rubber(EPR) glue that will hexane solvent adopted to be obtained by solution method, is heated to 140 ~ 190 DEG C, not only can provides the energy that glue is certain, reduce system viscosity simultaneously in multiple-effect tubular heater, improves trickling property.
Flash distillation can be one-level, secondary or multistage.Because ethylene-propylene rubber(EPR) is heated to degradable after certain temperature, belong to temperature-sensitive material, therefore Heating temperature can not be too high, so often primary flash can not reach concentrate requirement.When secondary or multistage flash evaporation, need before flash tank, to be equipped with heating system simultaneously, consider gelatin viscosity simultaneously, require that the heater design technology of heating system is more and more higher.Along with the raising of gelatin concentration, flash tank volume will reduce successively.
In order to make concentrate better effects if, primary flash tank adopts malleation or vacuum operating, when secondary or multistage flash evaporation, the vacuum tightness of each flash tank increases successively.
Will maintain the temperature at more than the boiling point of hexane in flash tank, be beneficial to the quick volatilization of hexane, rapid diffusion, usually controlling its internal temperature is 80 ~ 140 DEG C.Flash distillation will absorb a large amount of heat, and therefore flash tank will attach chuck heating, and this not only can supplement the energy needed for flash distillation, can also solve ethylene-propylene rubber(EPR) gelatin concentration increase after the problem of large, the trickling property difference of viscosity.
The present invention can by ethylene-propylene rubber(EPR) gelatin concentration by 3 ~ 12% concentrate to 60 ~ 90%, and gelatin viscosity rises to 10000cp by 100cp, can meet the job requirement of twin screw extruder, reach the effect of ethylene-propylene rubber(EPR) glue flash distillation concentrate.
Embodiment
Embodiment 1
By concentration be 7.2% ethylene-propylene rubber(EPR) glue (solvent is hexane) 8.0kg heat in multiple-effect tubular heater and make it be warming up to 180 DEG C, keep this temperature, (flash tank volume is for 100L to be sent into flash tank with the flow velocity of about 2m/s, top establishes a perforate to be connected with condenser), flash tank sets chuck to heat to keep internal temperature as 100 DEG C, pressure is higher than normal atmosphere, and hexane is discharged by the perforate of flash tank top and reclaimed after condensation.Glue after concentrate is discharged by the toothed gear pump of flash tank bottom.
By analysis, after concentrate, gelatin concentration is 66.2%.
Embodiment 2
Equipment used and working method are with embodiment 1, and ethylene-propylene rubber(EPR) original gelatin concentration is 7.2%, and solvent is hexane, and changing flash tank internal temperature is 120 DEG C, and by analysis, after concentrate, gelatin concentration is 68.6%.
Embodiment 3
Equipment used and working method are substantially with embodiment 1, ethylene-propylene rubber(EPR) gelatin concentration is 5.9%, solvent is hexane, glue temperature is heated to 170 DEG C, in flash tank, temperature remains on 120 DEG C, the outlet of flash tank upper gaseous phase adds a vacuum pump makes absolute pressure in tank be 500mmHg, and by analysis, after concentrate, gelatin concentration is 76.0%.
Embodiment 4
Equipment used and working method are with embodiment 3, ethylene-propylene rubber(EPR) gelatin concentration is 10.6%, solvent is hexane, glue temperature is heated to 180 DEG C, in flash tank, temperature remains on 120 DEG C, the outlet of flash tank upper gaseous phase adds a vacuum pump makes absolute pressure in tank be 300mmHg, and by analysis, after concentrate, gelatin concentration is 73.1%.
Embodiment 5
Get ethylene-propylene rubber(EPR) glue (solvent the is hexane) 8.0kg that concentration is 8.2%, 160 DEG C are heated in multiple-effect tubular heater, sent in the 2nd tubular heater with the flow velocity of about 2m/s, at this, glue is reheated to be entered in flash tank after 180 DEG C, and the volume of flash tank is about 100L, keeps wherein temperature to be 120 DEG C, pressure is higher than normal atmosphere, and the solvent hexane of being discharged by flash tank reclaims after condensation.
By analysis, the gelatin concentration after two-stage preheating brings up to 89.6%.
Embodiment 6
Equipment used and working method are substantially with embodiment 5, ethylene-propylene rubber(EPR) gelatin concentration is 5.9%, solvent is hexane, the venting port of flash tank is connected with a vacuum pump, controlling absolute pressure in tank is 500mmHg, temperature is 110 DEG C, and two-stage tubular heater heats glue to 150 DEG C and 170 DEG C respectively.
By analysis, after concentrate, gelatin concentration is 67.8%.
Embodiment 7
Equipment used and working method are substantially with embodiment 5, ethylene-propylene rubber(EPR) gelatin concentration is 9.6%, solvent is hexane, the venting port of flash tank is connected with a vacuum pump, controlling absolute pressure in tank is 400mmHg, temperature is respectively 120 DEG C, and two-stage tubular heater heats glue to 160 DEG C and 180 DEG C respectively.
By analysis, after concentrate, gelatin concentration is 80.5%.
Claims (1)
1. the method for a flash distillation concentrate ethylene-propylene rubber(EPR) glue, it is characterized in that: by the ethylene-propylene rubber(EPR) glue adopting hexane solvent to be obtained by solution method, be heated to 140 ~ 190 DEG C of temperature in multiple-effect tubular heater after, flash distillation in flash tank is entered with 2m/s flow velocity, utilize the heat of pressure difference and external complement, hexane solvent is volatilized instantaneously, and controlling flash tank internal temperature is 80 ~ 140 DEG C; Flash distillation adopts one-level, secondary or multistage; Primary flash tank adopts malleation or vacuum operating; When secondary or multistage flash evaporation, the vacuum tightness of each flash tank increases successively, and flash tank tank body reduces successively.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110315141.9A CN103044598B (en) | 2011-10-17 | 2011-10-17 | Method for flash evaporating and concentrating of liquid ethylene propylene rubber |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110315141.9A CN103044598B (en) | 2011-10-17 | 2011-10-17 | Method for flash evaporating and concentrating of liquid ethylene propylene rubber |
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| CN103044598A CN103044598A (en) | 2013-04-17 |
| CN103044598B true CN103044598B (en) | 2014-12-24 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539882A (en) * | 2013-09-29 | 2014-01-29 | 安徽同丰橡塑工业有限公司 | Production technology of ethylene propylene rubber |
| KR101568186B1 (en) * | 2014-01-06 | 2015-11-11 | 대림산업 주식회사 | Apparatus and method for polymerizing ethylene and alpha-olefin |
| CN105987915A (en) * | 2015-02-16 | 2016-10-05 | 中国石油天然气股份有限公司 | Ethylene propylene polymer solution aqueous phase testing method |
| CN108341897B (en) * | 2017-01-24 | 2021-03-16 | 中国石油化工股份有限公司 | Method for removing solvent from polymer solution |
| CN107670318B (en) * | 2017-09-19 | 2019-10-25 | 中国石油集团东北炼化工程有限公司吉林设计院 | EP rubbers produces method for recovering solvents and recovery system |
| CN107941051A (en) * | 2017-10-11 | 2018-04-20 | 中国石油集团东北炼化工程有限公司吉林设计院 | Heat exchanger and EP rubbers production solvent recovering system |
| CN111909422A (en) * | 2020-08-17 | 2020-11-10 | 浙江信汇新材料股份有限公司 | Butyl rubber base rubber preparation equipment set and preparation method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1916037A (en) * | 2005-08-17 | 2007-02-21 | 中国石油天然气股份有限公司 | Method for concentrating glue liquor of chlorosulfonated polyethylene through flash distillation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1916037A (en) * | 2005-08-17 | 2007-02-21 | 中国石油天然气股份有限公司 | Method for concentrating glue liquor of chlorosulfonated polyethylene through flash distillation |
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