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CN105949500B - For the solvent slop processing method in rubber production - Google Patents

For the solvent slop processing method in rubber production Download PDF

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Publication number
CN105949500B
CN105949500B CN201610398221.8A CN201610398221A CN105949500B CN 105949500 B CN105949500 B CN 105949500B CN 201610398221 A CN201610398221 A CN 201610398221A CN 105949500 B CN105949500 B CN 105949500B
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China
Prior art keywords
solvent
processing method
light component
flash column
rectifying column
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CN201610398221.8A
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CN105949500A (en
Inventor
陶琳
宋顺利
秦宁
李鸿飞
王翠菊
罗艳梅
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PetroChina Jilin Chemical Engineering Co.,Ltd.
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Jilin Design Institute
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J11/00Recovery or working-up of waste materials
    • C08J11/02Recovery or working-up of waste materials of solvents, plasticisers or unreacted monomers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/16Ethene-propene or ethene-propene-diene copolymers

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The present invention provides a kind of solvent slop processing method in rubber production, includes the following steps: S10: providing thick solvent to flash column with gas phase, the heavy constituent and light component in thick solvent are separated in flash column;S20: being passed through rectifying column after heat exchanger exchanges heat for light component, and organic solvent and moisture in light component are separated in rectifying column;S30: thermal energy is provided by light component of the heat exchanger into rectifying column.The purpose of the present invention is to provide a kind of reduction energy consumption, make full use of the solvent slop processing method of thermal energy in treating material.

Description

For the solvent slop processing method in rubber production
Technical field
The present invention relates to a kind of solvent slop processing methods in rubber production, more particularly, to organic solvent Refining methd.
Background technique
In the production of solwution method EP rubbers, using hexane solvent to complete polymerization reaction, it will form after polymerization mixed There is the thick solvent of a variety of sundries such as oligomer, moisture and organic solvent, which is referred to as solvent slop, so hexane solvent needs Recycling after refining.
In the prior art, the solvent containing the impurity such as water and oligomer is usually entered into refined unit with liquid form, Successively rectifying removing light component, heavy constituent (i.e. first light rear weight), are removed with conventional rectification mode.For the prior art, by In organic solvent during purification, reboiler need to provide heating steam thermal energy with guarantee the purification of organic solvent smoothly into Row, so that energy consumption is excessively high.Solvent causes conventional rectification with the treatment process that liquid form enters refined unit and first light rear weight The high energy consumption defect of mode.
In addition, load fluctuation is big when treating material enters flash column and rectifying column, flash column and rectifying column is caused to grasp Make unstable, also becomes organic solvent problem to be solved during purification.
Summary of the invention
For problem present in the relevant technologies, the purpose of the present invention is to provide a kind of reduction energy consumption, make full use of to Handle the solvent slop processing method of the high-grade thermal energy in material.
The present invention provides a kind of solvent slop processing methods in rubber production, include the following steps: S10: with gas Phase form provides thick solvent to flash column, and the heavy constituent and light component in thick solvent are separated in flash column;S20: by light component It is passed through rectifying column after heat exchanger exchanges heat, organic solvent and moisture in light component are separated in rectifying column;S30: by changing Light component of the hot device into rectifying column provides thermal energy.
According to the present invention, reboiler is respectively set in flash column and rectifying column, it is additional to be provided to flash column and rectifying column Thermal energy.
According to the present invention, the recombination sub-export and tower body of the first reboiler and flash column that are arranged on flash column connect respectively It is logical, to constitute first circulation circuit;Organic solvent outlet and the tower body of the second reboiler and rectifying column on rectifying column are set It is respectively communicated with, to constitute second circulation circuit.
According to the present invention, reboiler obtains additional thermal energy by low-pressure steam.
According to the present invention, recombination is divided into the component that thick solvent mid-boiling point is greater than moisture, and light component is organic in thick solvent Solvent and moisture.
According to the present invention, the temperature for the light component isolated at the top of flash column is higher by than the temperature of the tower reactor of rectifying column 20℃-30℃。
According to the present invention, in S20 step, light component passes through water in the first receiver between heat exchanger and flash column With the mode separating most moisture of organic solvent fluid liquid layering.
According to the present invention, condenser and second receiver are sequentially connected between the moisture outlet of rectifying column and tower body, To constitute third circulation loop, wherein in second receiver water and organic solvent fluid liquid layering by way of separating most Moisture.
According to the present invention, the partial reflux of the light component after the separation of the first receiver enters flash column.
According to the present invention, the solvent after second receiver separates and water azeotropic mixture partial reflux enter rectifying Tower.
The beneficial technical effect of the present invention lies in:
The present invention is with gas phase by the solvent of front directly as this unit feed, successively rectifying removing heavy constituent, Light component, and realize the thermal coupling in two distillation processes.Energy consumption of the invention is compared to the prior art for first taking off light weight de- again 25% or so.In addition, the present invention uses the thick solvent feed of high temperature gas phase, the thermal energy in treating material is made full use of, is substantially dropped The low energy consumption of rectifying tower reboiler.There are also thermal coupled process is used, the secondary steam of column overhead will be flashed as rectifying column The heat source of heat exchanger, further decreases energy consumption.
Detailed description of the invention
Fig. 1 is the schematic diagram of thick solvent processing method of the invention.
Specific embodiment
The embodiment shown is disclosed with reference to attached drawing.It will be appreciated, however, that the disclosed embodiments be only can with various and The embodiment that alternative form is shown.Attached drawing is not necessarily drawn to scale, and it is specific to show to zoom in or out some features The details of component.Disclosed specific structure and functional details should not be construed as limiting, but as instructing this field Technical staff's representative basis how of the disclosure.
The present invention shown in FIG. 1 is for the solvent slop processing method in rubber production, comprising: flash column 2, flash column 2 have first charging aperture 21, recombination sub-export 23 and gas vent 22;Rectifying column 6, rectifying column 6 have second charging aperture 61, have Solvent outlet 63 and moisture outlet 62, and gas vent 22 is connected by heat exchanger 5 with second charging aperture 61;Wherein, Heat exchanger 5 is connected with the tower body of organic solvent outlet 63 and rectifying column 6 to constitute circulation loop.The thick solvent of gas phase high temperature enters It to first charging aperture 21, is steamed using water and organic solvent azeotropic from 2 tower top of flash column, and heavy from tower bottom removing oligomer etc. Component.Moisture and organic solvent gas are layered former by the liquefaction arrival second charging aperture 61 of heat exchanger 5 using solvent and aqueous liquid Reason obtains pure organic solvent from organic solvent outlet 63, recombinates and be divided into the component that thick solvent mid-boiling point is greater than moisture, and light group The organic solvent and moisture being divided into thick solvent.In addition, the temperature for the light component isolated from flash column should be than the tower of rectifying column The temperature of kettle is 20 DEG C -30 DEG C high, and the discharged heat that liquefies in heat exchanger 5 is provided to rectifying column tower, as rectifying column Heat source further decreases energy consumption.In other embodiments, the energy that heat exchanger 5 is discharged can be provided to reboiler 7, or Person's heat exchanger 5 and reboiler 7 are combined into a new heat exchanger, and heat exchange is carried out inside the new heat exchanger.
In addition, in order to adapt to the case where feed loading fluctuates greatly, causes tower fluctuation of service, the first reboiler 1 and flash distillation Tower 2 connects, and the second reboiler 7 is connect with rectifying column 6.That is, the first reboiler 1 being arranged on flash column 2 with The recombination sub-export 23 and tower body of flash column 2 are respectively communicated with, to constitute first circulation circuit;It is arranged in second on rectifying column 6 The organic solvent of reboiler 7 and rectifying column 6 outlet 63 and tower body are respectively communicated with, to constitute second circulation circuit.To adjust two The load of tower is conducive to control production and stablizes.
It continues to refer to figure 1, the first reboiler 1 and the second reboiler 7 are separately connected low-pressure steam LS to provide additional heat Can, because flash column 2 and rectifying column 6 need the first reboiler 1 and the second reboiler 7 to provide thermal energy constantly to guarantee to adjust flash distillation The load of tower 2 and rectifying column 6, control production are stablized.
The principle that light component in the first receiver 3 and second receiver 9 is layered using solvent, aqueous liquid, passes through water With the mode separating most moisture of organic solvent fluid liquid layering, which is 99% range of moisture gross mass.Wherein The organic solvent containing minor amount of water of first receiver 3 passes through the transmission of delivery pump 4, and 40%~50% is used as charging to be transported to rectifying In tower 6,40%~50% flows back into flash column 2.With reference to Fig. 1, in the preferred embodiment of this method, in the water of rectifying column 6 It is sequentially connected condenser 11, second receiver 9 and the second delivery pump 10 between sub-export and tower body, is recycled back to constituting third Road passes through water in second receiver 9 wherein cooling down by recirculated water CCW to water and organic solvent in condenser 11 With the mode separating most moisture of organic solvent fluid liquid layering.With this, pure organic solvent after separation passes through third Delivery pump 8 is pumped to organic solvent outlet 63.
The present invention provides a kind of solvent slop processing methods in rubber production, include the following steps:
S10: providing thick solvent to flash column 2 with gas phase, since solvent and water form azeotropic mixture in flash column 2, It is branched away with lower energy penalty in tower top, reaches from thick solvent that (solvent and water are total to by heavy constituent and light component and water Boil object) it separates;
S20: light component and water (azeotropic mixture of solvent and water) temperature are higher, and the high temperature using this part is that rectifying column boils again Device provides heat source, it is therefore an objective to save heating steam, reach saving non-renewable energy.Specific practice is light component and water (solvent and water Azeotropic mixture) after heat exchanger 5 (energy-saving appliance) heat exchange enter rectifying column 6, it is light with azeotropic principles separation again in rectifying column 6 Organic solvent and moisture in component;
S30: thermal energy is provided by light component of the heat exchanger 5 into rectifying column.
According to the present invention, the first reboiler 1 and the second reboiler 7 is respectively set in flash column 2 and rectifying column 6, is to adjust Tower fluctuation of service caused by being fluctuated due to feed loading is rapidly reached stable operation at tower driving initial stage.
Heat exchanger 5 and the second reboiler 7 is respectively set in rectifying column, heat exchanger 5 is energy-saving appliance, recovery section high-grade heat Can, achieve the purpose that save primary steam, the second reboiler 7 is auxiliary reboiler, is made when the thermal energy deficiency that energy-saving appliance provides With.
According to the present invention, the recombination sub-export 23 and tower body difference of the first reboiler and flash column on flash column are set Connection, to constitute first circulation circuit;Be arranged in the second reboiler and rectifying column on rectifying column organic solvent outlet 63 and Tower body is respectively communicated with, to constitute second circulation circuit.
According to the present invention, reboiler 1,7 obtains additional thermal energy by low-pressure steam.
According to the present invention, recombination is divided into the component that thick solvent mid-boiling point is greater than moisture, and light component is organic in thick solvent Solvent and moisture.
According to the present invention, the temperature for the light component isolated from the tower top of flash column 2 is higher than the temperature of the tower reactor of rectifying column 6 20 DEG C -30 DEG C out.
According to the present invention, in S20 step, light component (solvent azeotrope with water object) is between heat exchanger 5 and flash column 1 In first receiver water and organic solvent fluid liquid layering by way of separating most moisture.
According to the present invention, condenser 11 and the second reception are sequentially connected between the moisture outlet and tower body of rectifying column 6 Device 9, to constitute third circulation loop, wherein being separated by way of the layering of organic solvent fluid liquid in second receiver 9 water Most of moisture.
According to the present invention, the fraction of the light component after the separation of the first receiver 3 flows back into flash column 2.
These are only the preferred embodiment of the present invention, is not intended to restrict the invention, for those skilled in the art For member, the invention may be variously modified and varied.All within the spirits and principles of the present invention, it is made it is any modification, Equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.

Claims (10)

1. a kind of solvent slop processing method in rubber production, which comprises the steps of:
S10: providing thick solvent to flash column with gas phase, separated in the flash column heavy constituent in the thick solvent and Light component;
S20: the light component is passed through rectifying column after heat exchanger exchanges heat, is separated in the rectifying column in the light component Organic solvent and moisture;
S30: thermal energy is provided by the light component of the heat exchanger into the rectifying column.
2. solvent slop processing method according to claim 1, which is characterized in that in the flash column and the rectifying column point Not She Zhi reboiler, to provide additional thermal energy to the flash column and the rectifying column.
3. solvent slop processing method according to claim 2, which is characterized in that be arranged on the flash column first again The recombination sub-export and tower body of boiling device and the flash column are respectively communicated with, to constitute first circulation circuit;It is arranged in the rectifying Organic solvent outlet and tower body of second reboiler with the rectifying column on tower is respectively communicated with, to constitute second circulation circuit.
4. solvent slop processing method according to claim 2, which is characterized in that the reboiler is obtained by low-pressure steam The additional thermal energy.
5. solvent slop processing method according to claim 1, which is characterized in that the recombination, which is divided into the thick solvent, boils Point is greater than the component of moisture, and the light component is the organic solvent and the moisture in the thick solvent.
6. solvent slop processing method according to claim 1, which is characterized in that isolated at the top of the flash column The temperature of the light component is higher by 20 DEG C -30 DEG C than the temperature of the tower reactor of the rectifying column.
7. solvent slop processing method according to claim 1, which is characterized in that in the S20 step, the light component It is separated by way of the layering of organic solvent fluid liquid in the first receiver between the heat exchanger and the flash column water Most of moisture.
8. solvent slop processing method according to claim 1, which is characterized in that in the moisture outlet and tower of the rectifying column Condenser and second receiver are sequentially connected between body, to constitute third circulation loop, wherein in the second receiver The separating most moisture by way of water and the layering of organic solvent fluid liquid.
9. solvent slop processing method according to claim 7, which is characterized in that after first receiver separation The partial reflux of the light component enters the flash column.
10. solvent slop processing method according to claim 8, which is characterized in that after second receiver separation Solvent and water azeotropic mixture partial reflux enter the rectifying column.
CN201610398221.8A 2016-06-07 2016-06-07 For the solvent slop processing method in rubber production Active CN105949500B (en)

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CN105949500B true CN105949500B (en) 2019-10-25

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BR112020021759A2 (en) * 2018-11-01 2021-06-15 Lg Chem, Ltd method for separating organic solvent from mixed solution containing the organic solvent

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CN102585283A (en) * 2011-01-07 2012-07-18 中国石油化工股份有限公司 Method for recovering solvent from oligomer
CN203447806U (en) * 2013-07-31 2014-02-26 山东华懋新材料有限公司 Recovery device for solution polymerized styrene-butadiene rubber solvent
CN104592544A (en) * 2015-01-27 2015-05-06 湖南百利工程科技股份有限公司 Process for refining solvent in synthetic rubber production process

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US5575979A (en) * 1991-03-04 1996-11-19 Phillips Petroleum Company Process and apparatus for separating diluents from solid polymers utilizing a two-stage flash and a cyclone separator
EP2083020A1 (en) * 2008-01-18 2009-07-29 Total Petrochemicals Research Feluy Process for monomer recovery from a polymerization process
US8524972B1 (en) * 2012-04-18 2013-09-03 Exxonmobil Chemical Patents Inc. Low temperature steam stripping for byproduct polymer and solvent recovery from an ethylene oligomerization process
CN103570576B (en) * 2012-07-20 2016-06-15 中国石油化工集团公司 A kind of cracking c_5 tripping device circulating solvent regeneration system rapidly and method
CN104606911A (en) * 2015-01-22 2015-05-13 中建安装工程有限公司 Device and method for coupled separation of propylene and propane by extractive distillation and flash evaporation

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
CN102585283A (en) * 2011-01-07 2012-07-18 中国石油化工股份有限公司 Method for recovering solvent from oligomer
CN102504066A (en) * 2011-11-11 2012-06-20 茂名鲁华化工有限公司 Method for solvent refining during isoprene rubber production
CN203447806U (en) * 2013-07-31 2014-02-26 山东华懋新材料有限公司 Recovery device for solution polymerized styrene-butadiene rubber solvent
CN104592544A (en) * 2015-01-27 2015-05-06 湖南百利工程科技股份有限公司 Process for refining solvent in synthetic rubber production process

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Effective date of registration: 20200928

Address after: 132002 3-6 and 9-13 floors of Block A, Jihua Economic and Trade Center, Tongtan Road, Changyi District, Jilin Province

Patentee after: PetroChina Jilin Chemical Engineering Co.,Ltd.

Address before: 132002, Jilin, Jilin Province tung Chi Road East Economic and Trade Building

Patentee before: JILIN DESIGNING INSTITUTE OF CNPC NORTHEAST REFINING & CHEMICAL ENGINEERING Co.,Ltd.

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