CN106478363A - The technique of recycling design and monomer in Butyl Rubber - Google Patents
The technique of recycling design and monomer in Butyl Rubber Download PDFInfo
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- CN106478363A CN106478363A CN201610861081.3A CN201610861081A CN106478363A CN 106478363 A CN106478363 A CN 106478363A CN 201610861081 A CN201610861081 A CN 201610861081A CN 106478363 A CN106478363 A CN 106478363A
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- chloromethanes
- tower
- isobutene
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- isoprene
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The technique of recycling design and monomer in a kind of Butyl Rubber, belongs to chemical rubber field.Chloromethanes tower top and side line produce the chloromethanes of two kinds of different purity respectively, and overhead extraction high-purity chloro methane is used as catalyst solvent；The slightly lower chloromethanes of side take-off purity is used as solvent monomer.Chloromethanes tower is hot coupling rectifying with chloromethanes recovery tower, it is achieved that the secondary utilization of heat in chloromethanes recovery tower.The present invention is compared compared with existing process, under the premise of solvent and monomer mass index is ensured, saves equipment investment and operating cost.
Description
Technical field
The invention belongs to chemical rubber field, particularly, it is related to recycling design and monomer in a kind of Butyl Rubber
Technique.
Background technology
Butyl rubber is the random copolymer of isobutene and a small amount of isoprene, and isobutene is referred to as being polymerized with isoprene
Monomer, butyl rubber polymerization process are usually used chloromethanes as solvent, and chloromethanes is circulated as catalyst and solvent monomer
Use.Wherein, the chloromethanes purity as catalyst solvent is higher, and the chloromethanes purity as solvent monomer is slightly lower.Due to fourth
Base rubber polymerisation is extremely sensitive to impurity, and a small amount of impurity can all cause butyl rubber chain length to change, and is to ensure reacting balance
Carry out, it is necessary in the factor that Sources controlling is unfavorable to polymerisation.Circulation chloromethanes purity is to weigh the weight of polymerisation quality
Index is wanted, the complete hydro carbons of inert substance in chloromethanes and unreacted, such as isoprene, butylene and oligomer etc. is mixed,
Must be separated off.
Patent GB770265A is proposed in butyl rubber separation process, the complete isobutene of unreacted, isoprene and solvent
Chloromethanes enters compression section eliminating water and dries, and entering back into a series of rectifying columns carries out order separation, successively obtains high-purity chloromethane
Alkane, low-purity chloromethanes.Isobutene separated with isoprene, purify detailed process illustrates.
Patent US2999083A utilizes four-column process flow, order separating high-purity chloromethanes, low-purity chloromethane there is provided one kind
The method of alkane, isobutene and isoprene.Though the process can obtain meeting the isobutene of quality requirement, isoprene and molten
Agent chloromethanes, but energy consumption is larger with equipment investment.
Therefore, a kind of new method is found, under the premise of Separation Indexes are met, realizes energy-saving target, meaning ten
Divide great.
Content of the invention
For above-mentioned actual conditions, the present invention provides the technique of recycling design and monomer in a kind of Butyl Rubber, should
Technical process is mainly made up of chloromethanes tower, chloromethanes recovery tower and isobutene tower, and material to be separated is chloromethanes, isobutyl
Alkene, isoprene and the mixture of other alkene on a small quantity, mixed material initially enter chloromethanes tower, and tower top obtains high-purity chloro
Methane is recycled as catalyst solvent, and the slightly lower chloromethanes of side take-off purity is recycled as solvent monomer, is contained
The bottom of towe distillate of remaining chloromethanes and a large amount of isobutenes, isoprene enters chloromethanes recovery tower by feed pump.Chloromethane
Alkane reclaims top gaseous phase and is back to chloromethanes tower, and bottom of towe distillate is mainly isobutene and isoprene, is entered by feed pump
Isobutene tower is carried out isobutene and is separated with isoprene.Tower top obtains isobutene, and bottom of towe obtains isoprene.Wherein, chloromethane
Alkane recovery tower belongs to hot coupling rectifying column with chloromethanes tower, it is achieved that the secondary utilization of energy.Especially, each tower reboiler is all adopted
The mode of heat medium water heating, can effectively reduce rectifying tower reactor wall temperature, it is to avoid in separation process, isobutene autohemagglutination produces dimer.
Technical scheme：
The technique of recycling design and monomer in Butyl Rubber, Butyl Rubber include chloromethanes tower, chloromethanes tower
Reboiler, chloromethanes tower condenser, chloromethanes tower return tank, first order cooler, first order knockout drum, second-stage cooler,
Second level knockout drum, third level cooler, third level knockout drum, chloromethanes column bottoms pump, chloromethanes tower reflux pump, chloromethanes are reclaimed
Tower, chloromethanes recovery tower reboiler, isobutene tower, isobutene tower reboiler, isobutene tower condenser, isobutene tower return tank and
Isobutene tower reflux pump；
Technical process is as follows：
The mixed material of chloromethanes, isobutene and isoprene, mixed material are initially entered in chloromethanes tower, tower overhead gas warp
Chloromethanes tower condenser is crossed, by circulating water to 42 DEG C, enters back into chloromethanes tower return tank；Gas in chloromethanes tower return tank
Through first order cooler, 20 DEG C are cooled to, enter back into first order knockout drum；Gas phase in first order knockout drum is through
Secondary coolers, are cooled to -18 DEG C by -38 DEG C of propylene refrigeration agent, enter back into second level knockout drum；In the knockout drum of the second level
Gas phase is cooled to -75 DEG C by -112 DEG C of cold-producing medium ethene through third level cooler, enters back into third level knockout drum, and the 3rd
Gas phase in level knockout drum enters tail gas recycle；First order knockout drum is returned to chloromethanes tower with the liquid phase in the knockout drum of the second level
In return tank；, through chloromethanes tower reflux pump, a part is used as backflow, another part conduct for liquid phase in chloromethanes tower return tank
High-purity chloro methane is produced, and is recycled as catalyst solvent；The low chloromethanes of chloromethanes tower side take-off purity, used as list
Body solvent is recycled；Chloromethanes tower reboiler is heated using heat medium water, tower reactor distillate through chloromethanes column bottoms pump, as chlorine
Methane recovery tower feeds, and chloromethanes reclaims tower overhead gas by being back to chloromethanes tower bottom, chloromethanes recovery tower reboiler from pressure
Heated using heat medium water；Chloromethanes recovery tower kettle distillate is by from being pressed into into isobutene tower, isobutene tower overhead gas is through isobutyl
Alkene tower condenser, by circulating water to 42 DEG C, enters back into isobutene tower return tank；Isobutene tower return tank liquid phase is through isobutyl
Alkene tower reflux pump, a part are produced as isobutene as backflow, another part, and isobutene product is delivered to outside battery limit (BL), isobutene
Recovery tower reboiler is heated using heat medium water, and tower reactor produces isoprene.
Chloromethanes tower process parameter：1.00～1.1MPa of operating pressure, 49～53 DEG C of tower top temperature, column bottom temperature 54～58
DEG C, theoretical cam curve 40～50, reflux ratio 25～30, side take-off position are the 25th～27 block of theoretical tray；Chloromethanes bottom of towe
Distillate includes chloromethanes, isobutene and isoprene, and wherein, the mass percent of chloromethanes is 92wt%～94wt%；Different
The mass percent of butylene is 6wt%～8wt%；The mass percent of isoprene is 0.1wt%～0.3wt%.
Chloromethanes recovery tower technological parameter：1.10～1.20MPa of operating pressure, 52～60 DEG C of tower top temperature, column bottom temperature
80～90 DEG C, theoretical cam curve 30～40, reflux ratio 1～1.2；Chloromethanes recovery tower top gaseous phase includes chloromethanes, isobutene
And isoprene, wherein, the mass percent of chloromethanes is 93wt%～96wt%；The mass percent of isobutene is 4wt%
～7wt%；The mass percent of isoprene is 0.1wt%～0.1.5wt%；Chloromethanes recovery tower bottom of towe distillate includes chlorine
Methane, isobutene and isoprene, wherein, chloromethanes≤100ppm；The mass percent of isobutene is 90wt%～92wt%；
The mass percent of isoprene is 8wt%～10wt%.
Isobutene tower process parameter：0.3～0.5MPa of operating pressure, 40～45 DEG C of tower top temperature, column bottom temperature 65～70
DEG C, theoretical cam curve 20～30, reflux ratio 6～8.
In the mixed material of chloromethanes, isobutene and isoprene the mass percent of chloromethanes be 90wt%～
96wt%；The mass percent of isobutene is 3wt%～6wt%；The mass percent of isoprene be 0.1wt%～
0.5wt%.
Beneficial effects of the present invention：Under the premise of solvent and monomer index is ensured, compared with existing process, the present invention adopts three towers
Flow process, the non-clear segmentation of chloromethanes tower reactor, chloromethanes recovery tower thermic load increase, and corresponding heat is further through being thermally integrated return chloromethane
Alkane tower, so as to significantly save equipment investment and the operating cost of recovery system.
Description of the drawings
Fig. 1 is the process schematic representation of recycling design and monomer.
In figure：1 chloromethanes tower；2 chloromethanes tower reboilers；3 chloromethanes tower condensers；
4 chloromethanes tower return tanks；5 first order coolers；6 first order knockout drums；7 second-stage coolers；
8 second level knockout drums；9 third level coolers；10 third level knockout drums；11 chloromethanes column bottoms pumps；
12 chloromethanes tower reflux pumps；13 chloromethanes recovery towers；14 chloromethanes recovery tower reboilers；
15 isobutene towers；16 isobutene tower reboilers；17 isobutene tower condensers；
18 isobutene tower return tanks；19 isobutene tower reflux pumps.
Specific embodiment
Below in conjunction with technical scheme and accompanying drawing, the in detail specific embodiment of the narration present invention.
The mixed material of chloromethanes, isobutene and isoprene, initially enters in chloromethanes tower 1, and tower overhead gas is through chloromethane
Alkane tower condenser 3, by circulating water to 42 DEG C, enters back into chloromethanes tower return tank 4；4 gas phase of chloromethanes tower return tank is passed through
First order cooler 5, is water-cooled to 20 DEG C by 5 DEG C of freezings, enters back into first order knockout drum 6；6 gas phase of first order knockout drum is passed through
Second-stage cooler 7, is cooled to -18 DEG C by -38 DEG C of propylene refrigeration agent, enters back into second level knockout drum 8；Second level knockout drum
8 gas phases are cooled to -75 DEG C by -112 DEG C of cold-producing medium ethene, enter back into third level knockout drum 10 through third level cooler 9,
10 gas phase of third level knockout drum enters tail gas recycle.First order knockout drum 6 is returned to chloromethanes tower with 8 liquid phase of second level knockout drum
In return tank 4.4 liquid phase of chloromethanes tower return tank is used as backflow through chloromethanes tower reflux pump 12, a part, and a part is made
Produce for high-purity chloro methane, recycle as catalyst solvent, the slightly lower chloromethanes of side take-off purity, molten as monomer
Agent is recycled.Chloromethanes tower reboiler 2 is heated using heat medium water, tower reactor distillate through chloromethanes column bottoms pump 11, as chlorine
Methane recovery tower 13 feeds, and by being back to 1 bottom of chloromethanes tower from pressure, chloromethanes recovery tower boils 13 top gas of chloromethanes recovery tower again
Device 14 is heated using heat medium water.13 kettle distillate of chloromethanes recovery tower is by from being pressed into into isobutene tower 15, isobutene tower 15 is pushed up
Gas enters back into isobutene tower return tank 18 through isobutene tower condenser 17 by circulating water to 42 DEG C.Isobutene tower flows back
18 liquid phase of tank is produced as isobutene as backflow, a part through isobutene tower reflux pump 19, a part, and isobutene product send
To outside battery limit (BL), isobutene recovery tower reboiler 16 is heated using heat medium water, and tower reactor produces isoprene.
In chloromethanes, isobutene and isoprene mixture, chloromethanes content (wt) is generally 90%～96%；Isobutene
Content (wt) is generally 3%～6%；Isoprene content (wt) is generally 0.1%～0.5%；
For ten thousand tons/year of Butyl Rubbers of xx rubber company xx, recycle section material quality constitutes：Chloromethanes
94.4%, iso-butane 0.2%, isobutene 4.7%, n-butene 0.0186%, 1- amylene 0.0041%, isoprene 0.3%.Warp
After crossing the proposed device and method separation of the present invention, the high-purity chloro methane mass fraction as catalyst solvent reaches 99.9%,
Wherein, isobutene content≤10ppm；Chloromethanes mass fraction as solvent monomer is 98.3%；Chloromethanes recovery tower bottom evaporates
Go out chloromethanes content≤100ppm in liquid；Isoprene content≤10ppm in isobutene.
1 technological parameter of chloromethanes tower：Operating pressure 1.05MPa (G), 51 DEG C of tower top temperature, 55.7 DEG C of column bottom temperature, theoretical
The number of plates 45, reflux ratio 26, side take-off position are the 26th piece of theoretical plate.
13 technological parameter of chloromethanes recovery tower：Operating pressure 1.17MPa (G), 56.7 DEG C of tower top temperature, column bottom temperature 85.5
DEG C, theoretical cam curve 30, reflux ratio 1.03.
15 technological parameter of isobutene tower：Operating pressure 0.4MPa (G), 42.6 DEG C of tower top temperature, 67.8 DEG C of column bottom temperature, reason
By the number of plates 20, reflux ratio 6.21.
The invention provides in a kind of Butyl Rubber recycling design and monomer technique, ensureing that solvent and monomer refer to
Under the premise of mark, compared with existing process, the present invention adopts three-column process flow, the non-clear segmentation of chloromethanes tower reactor, and chloromethanes recovery tower heat is negative
Lotus increase, corresponding heat further through be thermally integrated return chloromethanes tower, so as to significantly save recovery system equipment investment and
Operating cost.
Claims (8)
1. in a kind of Butyl Rubber recycling design and monomer technique, it is characterised in that the Butyl Rubber includes chlorine
Methane tower, chloromethanes tower reboiler, chloromethanes tower condenser, chloromethanes tower return tank, first order cooler, the first order are separated
Tank, second-stage cooler, second level knockout drum, third level cooler, third level knockout drum, chloromethanes column bottoms pump, chloromethanes tower
Reflux pump, chloromethanes recovery tower, chloromethanes recovery tower reboiler, isobutene tower, isobutene tower reboiler, the condensation of isobutene tower
Device, isobutene tower return tank and isobutene tower reflux pump；
Technical process is as follows：
The mixed material of chloromethanes, isobutene and isoprene, mixed material are initially entered in chloromethanes tower, and tower overhead gas is through chlorine
Methane tower condenser, by circulating water to 42 DEG C, enters back into chloromethanes tower return tank；Gas phase warp in chloromethanes tower return tank
First order cooler is crossed, 20 DEG C are cooled to, enter back into first order knockout drum；Gas phase in first order knockout drum is through the second level
Cooler, is cooled to -18 DEG C by -38 DEG C of propylene refrigeration agent, enters back into second level knockout drum；Gas phase in the knockout drum of the second level
Through third level cooler, -75 DEG C being cooled to by -112 DEG C of cold-producing medium ethene, entering back into third level knockout drum, the third level is divided
Gas phase in tank enters tail gas recycle；First order knockout drum is returned to the backflow of chloromethanes tower with the liquid phase in the knockout drum of the second level
In tank；, through chloromethanes tower reflux pump, used as backflow, another part is used as high-purity for a part for liquid phase in chloromethanes tower return tank
Degree chloromethanes extraction, recycles as catalyst solvent；The low chloromethanes of chloromethanes tower side take-off purity, molten as monomer
Agent is recycled；Chloromethanes tower reboiler is heated using heat medium water, tower reactor distillate through chloromethanes column bottoms pump, as chloromethanes
Recovery tower feeds, and chloromethanes reclaims tower overhead gas by being back to chloromethanes tower bottom from pressure, and chloromethanes recovery tower reboiler is used
Heat medium water is heated；Chloromethanes recovery tower kettle distillate is by from being pressed into into isobutene tower, isobutene tower overhead gas is through isobutene tower
Condenser, by circulating water to 42 DEG C, enters back into isobutene tower return tank；Isobutene tower return tank liquid phase is through isobutene tower
Reflux pump, a part are produced as isobutene as backflow, another part, and isobutene product is delivered to outside battery limit (BL), and isobutene is reclaimed
Tower reboiler is heated using heat medium water, and tower reactor produces isoprene.
2. technique according to claim 1, it is characterised in that chloromethanes tower process parameter：Operating pressure 1.00～
1.1MPa, 49～53 DEG C of tower top temperature, 54～58 DEG C of column bottom temperature, theoretical cam curve 40～50, reflux ratio 25～30, side line is adopted
Out position is the 25th～27 block of theoretical tray；Chloromethanes bottom of towe distillate includes chloromethanes, isobutene and isoprene, wherein,
The mass percent of chloromethanes is 92wt%～94wt%；The mass percent of isobutene is 6wt%～8wt%；Isoprene
Mass percent be 0.1wt%～0.3wt%.
3. technique according to claim 1 and 2, it is characterised in that chloromethanes recovery tower technological parameter：Operating pressure 1.10
～1.20MPa, 52～60 DEG C of tower top temperature, 80～90 DEG C of column bottom temperature, theoretical cam curve 30～40, reflux ratio 1～1.2；Chlorine
Methane recovery column overhead gas phase includes chloromethanes, isobutene and isoprene, and wherein, the mass percent of chloromethanes is 93wt%
～96wt%；The mass percent of isobutene is 4wt%～7wt%；The mass percent of isoprene be 0.1wt%～
0.1.5wt%；Chloromethanes recovery tower bottom of towe distillate includes chloromethanes, isobutene and isoprene, wherein, chloromethanes≤
100ppm；The mass percent of isobutene is 90wt%～92wt%；The mass percent of isoprene be 8wt%～
10wt%.
4. technique according to claim 1 and 2, it is characterised in that isobutene tower process parameter：Operating pressure 0.3～
0.5MPa, 40～45 DEG C of tower top temperature, 65～70 DEG C of column bottom temperature, theoretical cam curve 20～30, reflux ratio 6～8.
5. technique according to claim 3, it is characterised in that isobutene tower process parameter：Operating pressure 0.3～
0.5MPa, 40～45 DEG C of tower top temperature, 65～70 DEG C of column bottom temperature, theoretical cam curve 20～30, reflux ratio 6～8.
6. the technique according to claim 1,2 or 5, it is characterised in that the mixture of chloromethanes, isobutene and isoprene
In material, the mass percent of chloromethanes is 90wt%～96wt%；The mass percent of isobutene is 3wt%～6wt%；Isoamyl
The mass percent of diene is 0.1wt%～0.5wt%.
7. technique according to claim 3, it is characterised in that in the mixed material of chloromethanes, isobutene and isoprene
The mass percent of chloromethanes is 90wt%～96wt%；The mass percent of isobutene is 3wt%～6wt%；Isoprene
Mass percent be 0.1wt%～0.5wt%.
8. technique according to claim 4, it is characterised in that in the mixed material of chloromethanes, isobutene and isoprene
The mass percent of chloromethanes is 90wt%～96wt%；The mass percent of isobutene is 3wt%～6wt%；Isoprene
Mass percent be 0.1wt%～0.5wt%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610861081.3A CN106478363A (en) | 2016-09-29 | 2016-09-29 | The technique of recycling design and monomer in Butyl Rubber |
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| CN201610861081.3A CN106478363A (en) | 2016-09-29 | 2016-09-29 | The technique of recycling design and monomer in Butyl Rubber |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109438165A (en) * | 2018-12-29 | 2019-03-08 | 山东京博石油化工有限公司 | A kind of separation and recovery method of isobutene recycling tower bottom liquid |
| CN110041450A (en) * | 2018-01-17 | 2019-07-23 | 中国石油化工股份有限公司 | The method for producing butyl rubber |
| CN111072440A (en) * | 2019-12-02 | 2020-04-28 | 浙江信汇新材料股份有限公司 | Method for improving comprehensive utilization rate of isobutene |
| CN111808222A (en) * | 2020-06-30 | 2020-10-23 | 北京诺维新材科技有限公司 | Preparation method of halogenated butyl rubber |
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| US2999083A (en) * | 1958-11-28 | 1961-09-05 | Polymer Corp | Polymerization of unsaturated hydrocarbons |
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| US2999083A (en) * | 1958-11-28 | 1961-09-05 | Polymer Corp | Polymerization of unsaturated hydrocarbons |
Non-Patent Citations (1)
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| 李凤华等: "热耦精馏塔在化工节能改造中的可行性", 《石油化工》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110041450A (en) * | 2018-01-17 | 2019-07-23 | 中国石油化工股份有限公司 | The method for producing butyl rubber |
| CN110041450B (en) * | 2018-01-17 | 2021-11-19 | 中国石油化工股份有限公司 | Process for producing butyl rubber |
| CN109438165A (en) * | 2018-12-29 | 2019-03-08 | 山东京博石油化工有限公司 | A kind of separation and recovery method of isobutene recycling tower bottom liquid |
| CN109438165B (en) * | 2018-12-29 | 2022-03-15 | 山东京博石油化工有限公司 | Separation and recovery method of isobutene recovery tower bottom liquid |
| CN111072440A (en) * | 2019-12-02 | 2020-04-28 | 浙江信汇新材料股份有限公司 | Method for improving comprehensive utilization rate of isobutene |
| CN111808222A (en) * | 2020-06-30 | 2020-10-23 | 北京诺维新材科技有限公司 | Preparation method of halogenated butyl rubber |
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