CN105566544B - The method for controlling butyl reactor temperature - Google Patents

The method for controlling butyl reactor temperature Download PDF

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Publication number
CN105566544B
CN105566544B CN201610044888.8A CN201610044888A CN105566544B CN 105566544 B CN105566544 B CN 105566544B CN 201610044888 A CN201610044888 A CN 201610044888A CN 105566544 B CN105566544 B CN 105566544B
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ethene
pressure
tank
tube bundle
exchanging tube
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CN105566544A (en
Inventor
王跃
李迎辉
巩传志
朱晓晶
金萍
李亚楠
宋顺利
刘利
蒋凯
吕亮
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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
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F210/00Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
    • C08F210/04Monomers containing three or four carbon atoms
    • C08F210/08Butenes
    • C08F210/10Isobutene
    • C08F210/12Isobutene with conjugated diolefins, e.g. butyl rubber
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2400/00Characteristics for processes of polymerization
    • C08F2400/02Control or adjustment of polymerization parameters

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polymerisation Methods In General (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention provides the method for control butyl reactor temperature, including:Fed back by the signal of the pressure transmitter of ethene tank to adjust ethene pressure tank regulating valve, by the Stress control of ethene tank at the first pressure, the ethene vapor pressure that first pressure is equal at 100 DEG C subtracts ethene normal level absolute altitude with reactor heat-exchanging tube bundle elevation of top head of liquid difference along with ethene tank is exported to the pipe resistance drop and the regulation margin value of the adjustable decompression members of 10KPa of reactor heat-exchanging tube bundle entrance;The pressure drop of adjustable decompression member is adjusted, the ethylene pressure made into reactor heat-exchanging tube bundle is equal to the ethene vapor pressure at 100 DEG C.This method ensures that reaction is stable at 100 DEG C and carried out, and extends polymerization time, reduces and react unexpected Stopping probability, improve production capacity and production efficiency, reduces the unstability of polymerization process.This method technological process is simple, easy for installation, is easily manipulated;Control accuracy is high, and process is not required to expend energy, and operating cost is low, and production safety is reliable.

Description

The method for controlling butyl reactor temperature
Technical field
The invention belongs to rubber production field, more particularly, to the method for control butyl reactor temperature.
Background technology
Butyl rubber (IIR), for the fourth-largest synthetic rubber in the world, there is excellent air-tightness, resistance to ag(e)ing and damping and amortization Can, it is auto industry and the important raw material of Tire production industry, mainly for the manufacture of tire flap and the inner tube of a tyre, high-quality rotating radial Tire, it is also used for producing electrically insulating material, encapsulant, poison gas protection equipment and Medical bottle stopper.
The production method of butyl rubber mainly has two kinds of slurry process and solwution method.Slurry process be using chloromethanes as solvent, with H2O-AlCl3To trigger system, isobutene and a small amount of isoprene are passed through cationic copolymerization by (- 100 DEG C or so) at low temperature It is obtained.The production of slurry process butyl rubber mainly includes polymerisation, product purification, recovery circulation and clear kettle, drier Regeneration, refrigeration system composition.
First, dry the raw material isoprene after de- weight to mix by a certain percentage with isobutene, match somebody with somebody by solvent of chloromethanes Catalyst solution processed.Afterwards, catalyst solution and reaction mass are cooled to -94 DEG C with propylene and ethene, introduce polymeric kettle and enter Row polymerisation.The polymerisation is exothermic reaction, and reaction heat low temperature ethylene steam as caused by vaporizing liquid ethylene is removed, gathered Reaction is closed in -100 DEG C or so progress.
The process that liquid ethylene gasification removes reaction heat can be expressed by following formula:
(formula 1).
Polymerisation is carried out at -100 DEG C, therefore should make liquid ethylene at -100 DEG C in equal in reactor heat-exchanging tube bundle Even gasification.And in a practical situation, due to relative position and the difference of pipeline trend, into supercooled liquid during reactor heat-exchanging tube bundle The pressure of state ethene often deviates saturated vapour pressure at -100 DEG C.
According to Clausius-carat Bai Long equations:(formula 2), when the liquid for entering reactor When state ethylene pressure is higher, the increase of ethene vapor pressure, ethene gasification temperature also increases therewith, therefore causes reaction temperature liter It is high.Meanwhile from formula 1, reaction temperature, which raises, causes ethene amount of vaporization n to reduce, and the liquid ethylene amount for being back to ethene tank increases Add, cause liquid level in ethene tank to raise.Under ethene tank liquid level adjustment effect, the supercooled liquid ethylene volume for being supplemented in ethene tank subtracts It is small.The accumulation of this effect will prevent reaction heat cause the speed that reaction temperature is stepped up to be accelerated from removing well, accelerate The termination of reaction, causes the production capacity to decline.On the contrary, when ethylene pressure is relatively low, gasification temperature reduces, and amount of vaporization increase, causes Ethylene compressor treating capacity increases, and adds construction and production cost.
Therefore, rightly control pressure when liquid ethylene enters reactor heat-exchanging tube bundle, make its in reactor in- Homogeneous gasification reduces production cost and suffers from important meaning to improving production efficiency under 100 DEG C of reaction temperature.
The content of the invention
It is an object of the invention to provide a kind of method for controlling butyl reactor temperature.This method uses ethene tank pressure The mode that power interlocking is combined with the adjustable decompression member of reactor heat-exchanging tube bundle entrance setting, technological process is simple, easy for installation, It is easily manipulated;Control accuracy is high, and process is not required to expend energy, and operating cost is low, and production safety is reliable.
The invention provides a kind of method for controlling butyl reactor temperature, including:Become by the pressure of ethene tank Send the signal of device to feed back to adjust ethene pressure tank regulating valve, described first by the Stress control of ethene tank at the first pressure The ethene vapor pressure that pressure is equal at -100 DEG C subtracts ethene normal level absolute altitude and reactor heat-exchanging tube bundle elevation of top liquid Column pressure difference is exported to the pipe resistance drop and the adjustable decompression members of 10KPa of reactor heat-exchanging tube bundle entrance along with ethene tank Regulation margin value;Adjust the pressure drop of the adjustable decompression member, make into reactor heat-exchanging tube bundle ethylene pressure be equal to- Ethene vapor pressure at 100 DEG C.
In the above-mentioned methods, wherein, the adjustable decompression member includes fixed strip orifice plate and rotation strip orifice plate.
In the above-mentioned methods, wherein, the adjustable decompression member is arranged on the liquid of the reactor air inlet channel under heat exchange tube bundle At ethylene inlet.
In the above-mentioned methods, wherein, the pressure drop of the adjustable decompression member passes through the fixed strip orifice plate and described turn The relative angle of dynamic bar orifice plate carries out fine adjustments.
In the above-mentioned methods, wherein, the first pressure is 0.04MPaG.
In the above-mentioned methods, wherein, the ethene vapor pressure at described -100 DEG C is 0.026MPaG.
Adjustable decompression member is made up of two panels bar shaped orifice plate and fixed shell, is had between two panels orifice plate between a bit of fixation Away from first orifice plate orientation is fixed, and second orifice plate orientation can rotate, i.e., make pressure by the relative angle between two panels orifice plate Trickle change occurs for power drop, and orifice plate and housing are made by low temperature stainless steel.
By adjusting gaseous ethene Flow-rate adjustment ethene pressure tank, before preliminary control liquid ethylene enters reactor heat-exchanging tube bundle Pressure, then judged by pressure gauge before heat-exchanging tube bundle, change bar shaped orifice plate relative angle, reach fine setting ethylene pressure Effect, ensure that liquid ethylene gasifies in -100 DEG C in reactor.Office is caused because bar shaped orifice plate is not easy fluid flow state Portion influences, and so can ensure liquid ethylene homogeneous gasification in reactor heat-exchanging tube bundle while decompression, indulge reactor Keep uniform to temperature, be advantageous to the progress of course of reaction.
The beneficial effects of the invention are as follows:The method of this control butyl reactor temperature, thus it is ensured that supercooled liquid second Alkene is entering butyl reactor heat-exchanging tube bundle after homogeneous gasification at -100 DEG C, it is ensured that reaction is stably entered at -100 DEG C OK, extend polymerization time, reduce and react unexpected Stopping probability, improve production capacity and production efficiency, reduce the unstable of polymerization process Property.This method technological process is simple, easy for installation, is easily manipulated;Control accuracy is high, and process is not required to expend energy, operating cost Low, production safety is reliable.
Brief description of the drawings
Fig. 1 is the flow chart of one embodiment of the control of the temperature of reactor of slurry process production butyl rubber.
Fig. 2 is the schematic diagram of adjustable decompression member.
In Fig. 1:1st, liquid ethylene enters ethene tank pipeline, 2, ethene tank, 3, gaseous ethylene remove ethylene compressor pipeline, 4, Ethene pressure tank transmitter, 5, ethene pressure tank regulating valve, 6, ethene tank liquid level gauge, 7, ethene tank Liquid level adjusting valve, 8, liquid Ethene enters pipe reactor, and 9, reactor heat-exchanging tube bundle inlet pressure gauge, 10, adjustable decompression member, 11, butyl reactor Heat-exchanging tube bundle, 12, butyl reactor, 13, return to ethene tank pipeline after ethylene moiety gasification, 14, hot ethylene vapor -3- blows Sweep binder pipeline, 15, residual liquid ethene remove ethene waste liquid tank pipeline.
In fig. 2:1st, fixed strip orifice plate, 2, rotation strip orifice plate, 3, bar shaped screen hole.
Embodiment
The following examples can make those skilled in the art that the present invention be more fully understood, but not limit in any way The present invention.
As shown in figure 1, polymerisation is carried out in butyl reactor 12 during industrial production butyl rubber.Polymerization process Caused reaction heat is absorbed by the ethene gasification in butyl reactor heat-exchanging tube bundle 11 and returns to ethene tank 2, gasification Ethene afterwards is admitted to ethylene compressor by pipeline 3.Liquid level in ethene tank 2 is by ethene tank liquid level gauge 6 and ethene tank liquid level The interlocked control of regulating valve 7, fresh liquid ethylene are supplemented into ethene tank 2 by pipeline 1.At the end of reaction time, by hot ethene Steam, which is passed through pipeline 14, makes most of liquid ethylene gasify, and residual liquid ethene in system is depressed into ethene waste liquid by pipeline 15 Tank.Gasify to ensure liquid ethylene at -100 DEG C in reactor heat-exchanging tube bundle, be that ethene tank 2 sets pressure to join first Lock, the upper gaseous phase space pressure value of ethene tank 2 determined by pressure transmitter 4 adjust ethene pressure tank regulating valve 5, make ethene Pressure inside the tank maintains under a certain pressure, and ethene vapor pressure (0.026MPaG) subtracts second when this pressure value is equal to -100 DEG C Alkene normal level absolute altitude changes with reactor heat-exchanging tube bundle elevation of top head of liquid difference along with ethene tank is exported to reactor Heat pipe bundle entrance pipe resistance drop and the fine-tuning decompression member regulation margin values of 10KPa.As known in the art, ethene tank exports It is calculated according to ethene flow velocity, viscosity of technology parameter in pipeline to reactor heat-exchanging tube bundle entrance pipe resistance drop, also may be used To use the other method of calculating resistance drop commonly used in the art.In this embodiment, this pressure value is 0.04MPaG.Liquid Ethene through pipeline 8 and its branches to reactor heat-exchanging tube bundle entrance after being controlled by ethene tank pre-pressure, according to reactor The reading of pressure gauge 9 on heat-exchanging tube bundle inlet duct, the pressure drop of adjustable decompression member 10 is adjusted, made into heat-exchanging tube bundle 11 Liquid ethylene pressure is equal to 0.026MPaG, and liquid ethylene gasifies at -100 DEG C, maintains polymerisation and enters at -100 DEG C OK.
Fig. 2 shows the general principle of adjustable pressure element.Adjustable pressure element by fixed strip orifice plate, rotation strip orifice plate, Housing and rotating mechanism composition.Liquid ethylene is dropped by that can produce certain pressure during fixed strip orifice plate, and it is trickle that some occur for manifold Change, ethene after by fixed strip orifice plate nearby (being 25mm in the embodiment), it is before manifold is not yet recovered and logical Second rotatable bar orifice plate is crossed, further produces pressure drop, this partial pressure drop can pass through the relative angle of bar orifice plate Regulation, the change of bar hole relative angle, can be considered the change of orifice plate circulation area to a certain extent.Rotation strip orifice plate angle Change and completed by gear drive, pressure drop values corresponding to each angle are determined by experiment, and straight on corresponding angle Connect the pressure value for identifying liquid ethylene before the corresponding adjustable decompression member of heat-exchanging tube bundle entrance.This method can both be adjusted Pressure drop in turn ensure that manifold, allow liquid ethylene homogeneous gasification in heat-exchanging tube bundle at -100 DEG C.
Embodiment makes polymerization process more stable, in temperature using the method for this control butyl reactor temperature Rise and slow down, polymerization reaction time can extend to 50 hours by 30 hours.
It will be understood by those skilled in the art that above example is only exemplary embodiment, in the spirit without departing substantially from the present invention In the case of scope, a variety of changes can be carried out, replaces and changes.

Claims (3)

1. a kind of method for controlling butyl reactor temperature, including:
Fed back by the signal of the pressure transmitter of ethene tank to adjust ethene pressure tank regulating valve, by the Stress control of ethene tank In first pressure, the ethene vapor pressure when first pressure is equal to -100 DEG C subtracts ethene normal level absolute altitude and reactor Heat-exchanging tube bundle elevation of top head of liquid difference is exported to the pipe resistance drop of reactor heat-exchanging tube bundle entrance along with ethene tank With the regulation margin value 10KPa of adjustable decompression member;
The pressure drop of the adjustable decompression member is adjusted, when the ethylene pressure for making to enter reactor heat-exchanging tube bundle is equal to -100 DEG C Ethene vapor pressure, wherein, the adjustable decompression member includes fixed strip orifice plate and rotation strip orifice plate, the adjustable decompression member Pressure drop be adjusted by the relative angle of the fixed strip orifice plate and the rotation strip orifice plate.
2. according to the method for claim 1, it is characterised in that the adjustable decompression member is arranged on the reactor heat exchange Restrain the liquid ethylene porch of lower section.
3. according to the method for claim 1, it is characterised in that the first pressure is 0.04MPaG.
CN201610044888.8A 2016-01-22 2016-01-22 The method for controlling butyl reactor temperature Active CN105566544B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN202808662U (en) * 2012-07-05 2013-03-20 中国石油集团东北炼化工程有限公司吉林设计院 Device for improving quality of acrylonitrile-styrene copolymer product
CN103842150A (en) * 2011-09-28 2014-06-04 朗盛德国有限责任公司 Method for removing volatile components from polymer-containing media and degassing devices therefor
CN105542050A (en) * 2016-01-14 2016-05-04 中国石油集团东北炼化工程有限公司吉林设计院 Polymerization reaction initiating method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103842150A (en) * 2011-09-28 2014-06-04 朗盛德国有限责任公司 Method for removing volatile components from polymer-containing media and degassing devices therefor
CN202808662U (en) * 2012-07-05 2013-03-20 中国石油集团东北炼化工程有限公司吉林设计院 Device for improving quality of acrylonitrile-styrene copolymer product
CN105542050A (en) * 2016-01-14 2016-05-04 中国石油集团东北炼化工程有限公司吉林设计院 Polymerization reaction initiating method

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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.

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

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