CN103044598A - 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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- CN103044598A CN103044598A CN2011103151419A CN201110315141A CN103044598A CN 103044598 A CN103044598 A CN 103044598A CN 2011103151419 A CN2011103151419 A CN 2011103151419A CN 201110315141 A CN201110315141 A CN 201110315141A CN 103044598 A CN103044598 A CN 103044598A
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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 effectively flash distillation concentrate rubber 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, vapor phase process does not also have the industrialization report at present, larger company all adopts solution method production in the world, namely adopt take ethene, propylene, the 3rd monomer as raw material, hexane is solvent, under the initiation of Ziegler-Natta catalyst, and the synthetic ethylene-propylene rubber(EPR) take hydrogen as molecular weight regulator.Processing condition according to polyreaction are different, and the ethylene-propylene rubber(EPR) gelatin concentration is 3～12% after the reaction.
When ethylene-propylene rubber(EPR) was produced in solution polymerization, traditional method for recovering solvents had air lift method and roller desiccating method.What GB804535 proposed is exactly the roller desiccating method, the ethylene-propylene rubber(EPR) glue that this method obtains reaction is coated onto on the roller that a kind of special substance makes uniformly, the roller steam direct heating can make solvent be down to below 3% after reaching certain residence time.But this method heating is inhomogeneous, produces easily close-burning, affects quality product, without industrial prospect.What US2592814 proposed is that the air lift method reclaims solvent, glue is passed in the relatively high liquid medium of another boiling point (being generally water), this medium is heated to certain temperature (being higher than solvent boiling point), the energy that utilizes it to hold, the solvent gasification is reclaimed, and the glue behind the desolventizing forms small-particle and is isolated to qualified product in high boiling medium.This method is simple to operate, but the postorder processing technological flow is long during industrial enforcement, and required equipment is many, causes the solvent loss amount large, has strengthened simultaneously energy consumption, and production cost is higher, also can bring adverse influence to the raising of quality product.
Mostly adopt now water vapor air lift method on the ethylene-propylene rubber(EPR) full scale plant, namely with water as the 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, equipment water vapor air lift method how, utilize the direct desolvation of flash distillation concentrate twin-screw extrusion, make volatile content reach criterion of acceptability, just become the developing direction of ethylene-propylene rubber(EPR) solvent recuperation technology, therefore the glue concentrate that obtains after the reaction need to be arrived certain concentration, make its viscosity reach certain value, could satisfy like this job requirement of forcing machine.
Under certain temperature and pressure, require solvent for use that ethylene-propylene rubber(EPR) is had good solubleness, require again low being easy to of boiling point to reclaim, so solution method is produced, and mostly to adopt hexane on the ethylene-propylene rubber(EPR) industrialized unit be solvent.
Summary of the invention
The objective of the invention is the ethylene-propylene rubber(EPR) glue for the production take hexane as solvent, a kind of method of flash distillation concentrate ethylene-propylene rubber(EPR) glue is provided.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, adopts solution method production, and hexane is solvent, and the ethylene-propylene rubber(EPR) gelatin concentration is 3～12% (mass percents) after the reaction.
The present invention is the ethylene-propylene rubber(EPR) glue that will adopt hexane solvent to obtain by solution method, in the multiple-effect tubular heater, be heated to 140～190 ℃ of temperature, flow velocity with 2m/s enters in the flash tank, utilize the heat of pressure difference and external complement, solvent moment volatilization is reclaimed, simultaneously gelatin concentration is carried to 60～90%.
The present invention is the ethylene-propylene rubber(EPR) glue that will adopt hexane solvent to obtain by solution method, is heated to 140～190 ℃ in the multiple-effect tubular heater, not only can provide glue certain energy, reduces simultaneously system viscosity, improves trickling property.
Flash distillation can be one-level, secondary or multistage.Because ethylene-propylene rubber(EPR) is heated to degradable after the certain temperature, belong to temperature-sensitive material, so Heating temperature can not be too high, so often the one-level flash distillation can not reach the concentrate requirement.When secondary or multistage flash evaporation, need before flash tank, to be equipped with heating system simultaneously, consider simultaneously gelatin viscosity, require the heater design technology of heating system more and more higher.Along with the raising of gelatin concentration, the flash tank volume will reduce successively.
In order to make the concentrate better effects if, adopt malleation or vacuum operating on the one-level flash tank, 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 the flash tank, be beneficial to quick volatilization, the rapid diffusion of hexane, usually controlling its internal temperature is 80～140 ℃.Flash distillation will absorb a large amount of heat, so flash tank will attach chuck heating, and this not only can replenish the required energy of flash distillation, can also solve the problem that viscosity was large, trickling property is poor after the ethylene-propylene rubber(EPR) gelatin concentration increased.
The present invention can be with the ethylene-propylene rubber(EPR) gelatin concentration by 3～12% concentrates to 60～90%, and gelatin viscosity rises to 10000cp by 100cp, can satisfy the job requirement of twin screw extruder, reaches the effect of ethylene-propylene rubber(EPR) glue flash distillation concentrate.
Embodiment
Embodiment 1
Be that 7.2% ethylene-propylene rubber(EPR) glue (solvent is hexane) 8.0kg heats in the multiple-effect tubular heater and makes it be warming up to 180 ℃ with concentration, keep this temperature, flow velocity take about the 2m/s is sent it into flash tank, and (the flash tank volume is as 100L, top is established a perforate and is linked to each other with condenser), flash tank is established chuck, and to heat to keep internal temperature be 100 ℃, pressure is higher than normal atmosphere, and hexane is discharged by the perforate of flash tank top and reclaimed after condensation.Glue after the concentrate is discharged by the toothed gear pump of flash tank bottom.
By analysis, gelatin concentration is 66.2% after the concentrate.
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 the flash tank internal temperature is 120 ℃, and by analysis, gelatin concentration is 68.6% after the concentrate.
Embodiment 3
Equipment used and working method are basically with embodiment 1, the ethylene-propylene rubber(EPR) gelatin concentration is 5.9%, solvent is hexane, glue temperature is heated to 170 ℃, temperature remains on 120 ℃ in the flash tank, flash tank upper gaseous phase outlet adds a vacuum pump makes that absolute pressure is 500mmHg in the tank, and by analysis, gelatin concentration is 76.0% after the concentrate.
Embodiment 4
Equipment used and working method are with embodiment 3, the ethylene-propylene rubber(EPR) gelatin concentration is 10.6%, solvent is hexane, glue temperature is heated to 180 ℃, temperature remains on 120 ℃ in the flash tank, flash tank upper gaseous phase outlet adds a vacuum pump makes that absolute pressure is 300mmHg in the tank, and by analysis, gelatin concentration is 73.1% after the concentrate.
Embodiment 5
Get concentration and be 8.2% ethylene-propylene rubber(EPR) glue (solvent is hexane) 8.0kg, in the multiple-effect tubular heater, be heated to 160 ℃, with the flow velocity about 2m/s it is sent in the 2nd tubular heater, at this, glue is reheated after 180 ℃ and is entered in the flash tank, and the volume of flash tank is about 100L, and keeping wherein, temperature is 120 ℃, 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 the two-stage preheating brings up to 89.6%.
Embodiment 6
Equipment used and working method are basically with embodiment 5, the ethylene-propylene rubber(EPR) gelatin concentration is 5.9%, solvent is hexane, venting port at flash tank is connected with a vacuum pump, absolute pressure is 500mmHg in the control tank, temperature is 110 ℃, and the two-stage tubular heater heats respectively glue to 150 ℃ and 170 ℃.
By analysis, gelatin concentration is 67.8% after the concentrate.
Embodiment 7
Equipment used and working method are substantially with embodiment 5, the ethylene-propylene rubber(EPR) gelatin concentration is 9.6%, solvent is hexane, venting port at flash tank is connected with a vacuum pump, absolute pressure is 400mmHg in the control tank, temperature is respectively 120 ℃, and the two-stage tubular heater heats respectively glue to 160 ℃ and 180 ℃.
By analysis, gelatin concentration is 80.5% after the concentrate.
Claims (1)
1. the method for a flash distillation concentrate ethylene-propylene rubber(EPR) glue, it is characterized in that: the ethylene-propylene rubber(EPR) glue that will adopt hexane solvent to obtain by solution method, after in the multiple-effect tubular heater, being heated to 140～190 ℃ of temperature, enter flash distillation in the flash tank with the 2m/s flow velocity, utilize the heat of pressure difference and external complement, make hexane solvent moment volatilization, control flash tank internal temperature is 80～140 ℃; One-level, secondary or multistage are adopted in flash distillation; The one-level flash tank adopts malleation or vacuum operating; When secondary or multistage flash evaporation, the vacuum tightness of each flash tank increases successively, and the 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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| 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 true CN103044598A (en) | 2013-04-17 |
| CN103044598B CN103044598B (en) | 2014-12-24 |
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Cited By (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 |
| 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 |
| CN106132533A (en) * | 2014-01-06 | 2016-11-16 | 大林产业株式会社 | ethylene and alpha-olefin polymerization device and preparation method |
| CN107670318A (en) * | 2017-09-19 | 2018-02-09 | 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 |
| CN108341897A (en) * | 2017-01-24 | 2018-07-31 | 中国石油化工股份有限公司 | A method of removing solvent from polymer solution |
| 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 |
-
2011
- 2011-10-17 CN CN201110315141.9A patent/CN103044598B/en active Active
Patent 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 |
Cited By (9)
| 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 |
| CN106132533A (en) * | 2014-01-06 | 2016-11-16 | 大林产业株式会社 | ethylene and alpha-olefin polymerization device and preparation method |
| CN106132533B (en) * | 2014-01-06 | 2019-05-17 | 大林产业株式会社 | Ethylene and alpha-olefine polymerizing device and preparation method |
| 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 |
| CN108341897A (en) * | 2017-01-24 | 2018-07-31 | 中国石油化工股份有限公司 | A method of removing solvent from polymer solution |
| CN107670318A (en) * | 2017-09-19 | 2018-02-09 | 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 |
| 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 |
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| CN103044598B (en) | 2014-12-24 |
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