CN102504066A - Method for solvent refining during isoprene rubber production - Google Patents
Method for solvent refining during isoprene rubber production Download PDFInfo
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- CN102504066A CN102504066A CN2011103567477A CN201110356747A CN102504066A CN 102504066 A CN102504066 A CN 102504066A CN 2011103567477 A CN2011103567477 A CN 2011103567477A CN 201110356747 A CN201110356747 A CN 201110356747A CN 102504066 A CN102504066 A CN 102504066A
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Abstract
The invention relates to a method for solvent refining during isoprene rubber production. According to the method, the solvent recovered from a self-condensation process is conveyed into a distillation tower from the top of the tower; light components on the top of the tower are subjected to a total reflux operation through a tower top condenser and a reflux tank, or are subjected to small amount continuous recovery under the operation with a large reflux ratio more than 20, and the free water is separated from the reflux tank, and a small amount of uncondensed gases on the top of the tower are discharged to a tail gas condenser; the tower kettle liquid containing weight components is subjected to intermittent or continuous small flow rate recovery; the treated solvent is recovered from the side stream through the middle part of the tower in a vapor phase form, and is condensed by a side stream condenser, and the resulting solvent is conveyed to a polymerization process to directly use, wherein the treated solvent is the qualified solvent through the refining. According to the present invention, only a distillation tower is adopted in the method, the removal works of the water and other light components, and the heavy components are achieved in the single tower, the process is simple, the equipment investment is low, and the energy consumption is small, such that the production and operation cost can be effectively reduced.
Description
Technical field
The invention belongs to the viton production technical field, relate to the solvent-refined method in a kind of polyisoprene rubber production.
Background technology
In solution polymerization process viton production process; In cis-1,4-polybutadiene rubber (BR), solution styrene butadiene rubber (SSBR), solution polymerization process ethylene-propylene rubber(EPR), polyisoprene rubber (IR) and styrenic block copolymer SBC (SBS, SIS, SEBS) production; In polymerization process, use high amounts of solvents; Be generally hexanaphthene, normal hexane etc.; Generally contain 80～95% solvent in the glue after the polymerization, the agglomeration process of a large amount of solvents through glue reclaims the back and in device, recycles, and therefore device has all disposed solvent recuperation refined unit and relevant device.
At present, nearly all solvent treatment all is to adopt double-column process, promptly reclaims solvent and at first gets into a dehydration tower; Boil again and overhead condensation through the tower still; In tower, carry out sufficient thermal exchange, water-containing solvent from the cat head extraction, the back of leaving standstill, dewater refluxes and extraction, tower still material gets into weight-removing column; Refining solvent is from the cat head extraction after thermal exchange in tower, and heavy constituent are from the regular or continuous extraction of tower still.Double-column process is owing to adopt two rectifying tower, and technical process is comparatively complicated, and facility investment is big, energy consumption is high, thereby production cost is higher relatively.
Summary of the invention
The objective of the invention is to eliminate the deficiency of above-mentioned two tower process, a kind of solvent-refined method that polyisoprene rubber is produced that is used for is provided,, thereby reduce the products production cost with reduction facility investment and energy consumption.This method only adopts a rectifying tower, in single tower, realizes the task that removes of light constituent such as water and heavy constituent, and flow process is simple, and facility investment is low, and energy consumption is little, thereby can effectively reduce production and operation cost.
For achieving the above object; The present invention is light with taking off of traditional solvent dehydration tower, the heavy constituent that remove of dehydration and weight-removing column are incorporated in a Tai Tanei and carry out; Promptly in the separate unit tower, accomplish solvent dehydration, take off light and heavies removal task, this method is that self coagulation operation recovered solvent is sent into rectifying tower by cat head; The cat head light constituent carries out total reflux operation through overhead condenser and return tank, or a small amount of extraction is continuously carried out in operation under greater than 20 big reflux ratio, and isolates free-water from return tank, and the gas that cat head is not condensed on a small quantity then enters tail gas condenser; The tower bottoms that contains heavy constituent carries out intermittence or low discharge extraction continuously from the tower still; Refining solvent through tower middle part with the vapour phase form by the side line extraction, after the side line condenser condenses, go polymerization process directly to use.
In the present invention, tower top temperature is at 35～55 ℃, and tower top pressure is at 0.03～0.09Mpa; Tower still temperature is controlled at 75～100 ℃, and tower still pressure is at 0.05～0.12Mpa; 15～25 ℃ of the outflow temperatures of tail gas condenser 4, trim the top of column amount are 0.1～2 times of inlet amount; Self coagulation operation recovered solvent on the top of rectifying tower apart from 10～40 theoretical tray place chargings of cat head; Refining solvent from rectifying tower middle part apart from 10～30 theoretical stage place extraction of tower still.
The present invention can accurately control parameters such as rectifying tower working pressure, temperature through charging, side line extraction point position rationally are set, and reduces cat head emptying flow and tower still heavy constituent extraction, thereby reduces the consumption of solvent.
The present invention can be applicable to the refining of solvent in the polyisoprene rubber production process, also can be applicable in the solvent treatment in various solution polymerization process viton such as cis-1,4-polybutadiene rubber (BR), solution styrene butadiene rubber (SSBR), solution polymerization process ethylene-propylene rubber(EPR) and styrenic block copolymer SBC (SBS, SIS, the SEBS) production process.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Embodiment 1:
As shown in Figure 1, from the cohesion process recovered solvent, get into from the top of rectifying tower 1 apart from 30 theoretical stages of cat head; Unreacted monomer mass concentration 3% in this solvent; And contain 200ppm water and a small amount of heavy constituent, under the acting in conjunction of overhead condenser 2 and tower still reboiler 6, material carries out sufficient heat and mass in rectifying tower 1; The light constituent that comprises unreacted monomer carries out total reflux after overhead condenser 2 condensations; Its quantity of reflux is 0.5 times of inlet amount, can regularly discharge free-water from return tank 3, and the gas that cat head is not condensed on a small quantity then enters tail gas condenser 4.Refining qualified solvent at rectifying tower 1 middle part apart from 20 blocks of theoretical trays of tower still with the vapour phase form by the side line extraction, behind side line condensing surface 5, directly be used for polymerization process.This tower is operated under positive pressure, and the tower internal pressure is controlled at 0.04～0.06MPa (gauge pressure), and tower top temperature is 40～42 ℃, 78～80 ℃ of tower still temperature.
Side line extraction place can guarantee tower still heavy constituent content more than 30% apart from 20 theoretical stages of tower still, to reduce the quantity discharged of heavy constituent.
Owing to carried out total reflux operation at cat head; Comprise the constantly accumulation of light constituent content of unreacted monomer; When light constituent concentration reaches 95% can extraction part regularly light constituent individual curing, or according to a small amount of continuously extraction light constituent of the variation of tower top temperature pressure.
This solvent treatment steam that technology consumes is merely double tower about 50% when refining, 30% when cooling-water consumption is the double tower operation, and power consumption is 45% of a double tower operating procedure.
Embodiment 2:
As shown in Figure 1,1 top gets into unreacted monomer mass concentration 15% in this solvent apart from 15 theoretical stages of cat head from the cohesion process recovered solvent from rectifying tower; And contain 200ppm water and a small amount of heavy constituent; Under the acting in conjunction of overhead condenser 2 and tower still reboiler 6, material carries out sufficient heat and mass in rectifying tower 1, comprise that the light constituent of unreacted monomer carries out total reflux after overhead condenser 2 condensations; Its quantity of reflux is 1 times of inlet amount; Change continuous low discharge extraction light constituent according to temperature and pressure in the tower, can regularly discharge free-water from return tank 3, the gas that cat head is not condensed on a small quantity then enters tail gas condenser 4; The tower bottoms of heavy constituent carries out intermittence or low discharge extraction continuously from the tower still.Refining qualified solvent through at rectifying tower 1 middle part apart from 25 blocks of theoretical trays of tower still with the vapour phase form by the side line extraction, behind side line condensing surface 5, directly be used for polymerization process.This tower is operated under positive pressure, and the tower internal pressure is controlled at 0.06～0.08MPa (gauge pressure), and tower top temperature is 36～38 ℃, 75～78 ℃ of tower still temperature.
Side line extraction place can guarantee tower still heavy constituent content more than 35% apart from 25 theoretical stages of tower still, to reduce the quantity discharged of heavy constituent.
This solvent treatment steam that technology consumes is merely double tower about 60% when refining, 45% when cooling-water consumption is the double tower operation, and power consumption is 55% of a double tower operating procedure.
Claims (6)
1. solvent-refined method during a polyisoprene rubber is produced is characterized in that this method is that self coagulation operation recovered solvent is sent into rectifying tower by cat head; The cat head light constituent carries out total reflux operation through overhead condenser and return tank, or a small amount of extraction is continuously carried out in operation under greater than 20 big reflux ratio, and isolates free-water from return tank, and the gas that cat head is not condensed on a small quantity then enters tail gas condenser; The tower bottoms of heavy constituent carries out intermittence or low discharge extraction continuously from the tower still; Refining qualified solvent through the tower middle part with the vapour phase form by the side line extraction, after the side line condenser condenses, go polymerization process directly to use.
2. solvent-refined method during a kind of polyisoprene rubber according to claim 1 is produced is characterized in that tower top temperature is at 35～55 ℃, and tower top pressure is at 0.03～0.09Mpa; Tower still temperature is controlled at 75～100 ℃, and tower still pressure is at 0.05～0.12Mpa.
3. solvent-refined method during a kind of polyisoprene rubber according to claim 1 is produced is characterized in that 15～25 ℃ of the outflow temperatures of tail gas condenser 4.
4. solvent-refined method during a kind of polyisoprene rubber according to claim 1 is produced is characterized in that the trim the top of column amount is 0.1～2 times of inlet amount.
5. solvent-refined method during a kind of polyisoprene rubber according to claim 1 is produced is characterized in that, self coagulation operation recovered solvent on the top of rectifying tower apart from 10～40 theoretical tray place chargings of cat head.
6. solvent-refined method during a kind of polyisoprene rubber according to claim 1 is produced is characterized in that, refining solvent from the rectifying tower middle part apart from 10～30 theoretical stage place extraction of tower still.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011103567477A CN102504066A (en) | 2011-11-11 | 2011-11-11 | Method for solvent refining during isoprene rubber production |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104629082A (en) * | 2013-11-08 | 2015-05-20 | 中国石油天然气股份有限公司 | Method for recovering and refining solvent and monomer in industrial production of rare earth isoprene rubber |
| CN105949500A (en) * | 2016-06-07 | 2016-09-21 | 中国石油集团东北炼化工程有限公司吉林设计院 | Waste solvent treatment method for rubber production |
| CN107474174A (en) * | 2016-06-07 | 2017-12-15 | 中国石油化工股份有限公司 | A kind of method for producing butadiene rubber |
| CN109776853A (en) * | 2017-11-10 | 2019-05-21 | 中国石油化工股份有限公司 | Method for recovering solvents for ethylene/alpha-olefin technique for producing elastomer |
| CN110002941A (en) * | 2018-01-04 | 2019-07-12 | 抚顺伊科思新材料有限公司 | The method of recycling design in a kind of production of rubber composition |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101045798A (en) * | 2007-04-13 | 2007-10-03 | 青岛伊科思新材料股份有限公司 | Recovery and using method of solution and unreaction monomer in process of producting polymer by solution polymerization process |
| CN101337858A (en) * | 2007-07-03 | 2009-01-07 | 中国石油化工股份有限公司 | Process and equipment for preparing 1,2-butadiene by continuous method |
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- 2011-11-11 CN CN2011103567477A patent/CN102504066A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101045798A (en) * | 2007-04-13 | 2007-10-03 | 青岛伊科思新材料股份有限公司 | Recovery and using method of solution and unreaction monomer in process of producting polymer by solution polymerization process |
| CN101337858A (en) * | 2007-07-03 | 2009-01-07 | 中国石油化工股份有限公司 | Process and equipment for preparing 1,2-butadiene by continuous method |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104629082A (en) * | 2013-11-08 | 2015-05-20 | 中国石油天然气股份有限公司 | Method for recovering and refining solvent and monomer in industrial production of rare earth isoprene rubber |
| CN104629082B (en) * | 2013-11-08 | 2018-05-04 | 中国石油天然气股份有限公司 | Method for recovering and refining solvent and monomer in industrial production of rare earth isoprene rubber |
| CN105949500A (en) * | 2016-06-07 | 2016-09-21 | 中国石油集团东北炼化工程有限公司吉林设计院 | Waste solvent treatment method for rubber production |
| CN107474174A (en) * | 2016-06-07 | 2017-12-15 | 中国石油化工股份有限公司 | A kind of method for producing butadiene rubber |
| CN105949500B (en) * | 2016-06-07 | 2019-10-25 | 中国石油集团东北炼化工程有限公司吉林设计院 | For the solvent slop processing method in rubber production |
| CN107474174B (en) * | 2016-06-07 | 2020-07-24 | 中国石油化工股份有限公司 | Method for producing butadiene rubber |
| CN109776853A (en) * | 2017-11-10 | 2019-05-21 | 中国石油化工股份有限公司 | Method for recovering solvents for ethylene/alpha-olefin technique for producing elastomer |
| CN110002941A (en) * | 2018-01-04 | 2019-07-12 | 抚顺伊科思新材料有限公司 | The method of recycling design in a kind of production of rubber composition |
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Application publication date: 20120620 |