CN103333278B - A kind of device and technique thereof preparing fluoropolymer and fluorinated copolymer - Google Patents
A kind of device and technique thereof preparing fluoropolymer and fluorinated copolymer Download PDFInfo
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- CN103333278B CN103333278B CN201310035545.1A CN201310035545A CN103333278B CN 103333278 B CN103333278 B CN 103333278B CN 201310035545 A CN201310035545 A CN 201310035545A CN 103333278 B CN103333278 B CN 103333278B
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Abstract
The invention discloses a kind of device and the preparation technology thereof that prepare fluoropolymer and fluorinated copolymer.This device comprises: polyreaction pipeline, gas-liquid separation equipment, solid-liquid separating equipment, aqueous phase circulation tank, recycle pump, thermostatted; Polyreaction pipeline entrance end exports with thermostatted and is connected, and polyreaction pipe outlet is connected with gas-liquid separation equipment; The fluid output port of gas-liquid separation equipment is connected with solid-liquid separating equipment, and the fluid output port of solid-liquid separation is connected with aqueous phase circulation tank; The import of recycle pump is connected with aqueous phase circulation tank, and circulation pump outlet is connected with thermostatted import; Polyreaction pipeline is provided with multiple feed-pipe along its length, and the junction of every root feed-pipe and polyreaction pipeline is all provided with a nozzle.The present invention has the advantage that polymerization efficiency is high, production operation simple, convenient, reaction is even, polymerization temperature is controlled, avoid monomer local accumulation.
Description
Technical field
The present invention relates to the device of a kind of fluoropolymer and fluorinated copolymer, also relate to a kind of this device that utilizes and fluorochemical monomer is carried out the manufacturing process of successive polymerization or copolymerization.
Background technology
Fluoropolymer has function and the characteristic of a series of excellence, such as: all Practical Performances such as high temperature resistant, low temperature resistant, corrosion-resistant, weather is anti-aging, high-insulativity, dielectric properties are stable, high lubrication, toxicological harmless, make it can exhibit one's skill to the full in many fields of the national economy such as chemical engineering, petrochemical complex, construction work, aircraft industry, textile industry, automobile, optics and microelectronic industry.Lining on such as chemical anticorrosion pipeline and equipment and coating, the filtering material of ultrapure material, the hydraulic pressure transfer flexible pipe of high-low temperature resistant, the seal washer of resistance to various severe rugged environment, the bridge of low friction stretch surrogates etc. of slide block, all kinds of oil-free lubricating piston ring, the insulation of high-temperature high-frequency electronic machine, flexible cable, advanced printed wiring board, piezoelectricity pressure thermal characteristics material, release coating, human vas and cardiopulmonary internal organs without oil cooking kitchenware, are all its representative purposes in these fields.Along with manufacturing the progress with processing technology, more fluoropolymer product will be had to be applied in each department of all trades and professions; Therefore, the manufacture method of exploitation fluoropolymer, has great economic worth and social value.
Fluoropolymer is divided into homopolymer and multipolymer, and homopolymer is the product after a kind of monomer polymerization reactions, as: tetrafluoroethylene (PTFE, be called for short F4), voltalef (PCTFE, be called for short F3), polyvinylidene difluoride (PVDF) (PVDF, be called for short F2), fluorinated ethylene propylene (PVF is called for short F1) etc., multipolymer is the product after 2 kinds or the common polyreaction of two or more monomer, as: the multipolymer-perfluoroethylene-propylene (FEP of tetrafluoroethylene and R 1216, be called for short F46), tetrafluoroethylene and perfluoroalkyl vinyl ether multipolymer-Meltability polytetrafluorethyletubular (PFA), vinylidene and chlorotrifluoroethylene (Kel-F, be called for short F23), vinylidene and TFE copolymer (ф Oomph, be called for short F24), vinylidene and hexafluoropropylene copolymer (vitonA, be called for short F26), trifluorochloroethylene and ethylene copolymer (Halar, be called for short F30), tetrafluoroethylene and ethylene copolymer (Tefzel, be called for short F40), vinylidene and hexafluoro-isobutene multipolymer (CM-1), vinylidene and chlorotrifluoroethylene, copolymer from vinylidene fluoride and hexafluoropropylene, vinylidene and R 1216 and tetrafluoroethylene terpolymer etc.
The main method of synthesis homopolymer has emulsion polymerization, suspension polymerization, rear emulsion process and emulsification pretreatment method both at home and abroad at present, and wherein conventional method is emulsion polymerization and suspension polymerization.The method that synthetic copolymer is conventional is also emulsion polymerization and suspension polymerization, just in polymeric kettle, adds 2 kinds or monomer of more than two kinds respectively.
Letex polymerization refers to the effect by emulsifying agent, under mechanical stirring or vibration, and the polymerization that monomer forms emulsion and carries out in water; Emulsion polymerization product is latex, can directly apply, and also latex can be destroyed, and through postprocessing working procedures such as washing, dryings, obtains powdery or needle-like polymkeric substance.Letex polymerization can under higher speed of response, and obtain the polymkeric substance of higher molecular weight, the viscosity of material is low, and be easy to heat transfer and mixing, produce and easily control, residual monomer easily removes.The shortcoming of letex polymerization is that the emulsifying agent etc. added in polymerization process affects product properties.For obtaining solid polymer, need through technological processs such as cohesion, separation, washings.
Suspension polymerization refers to that monomer is under mechanical stirring or vibration, and by the effect of dispersion agent, monomer dispersion becomes drop, and suspend in water the polymerization process of carrying out usually, therefore also known as pearl polymerization.Feature is: have large water gaging in reactor, material viscosity is low, easily heat transfer and control; Polymerization is rear only through operations such as being simply separated, washing, be dry, need be obtained rosin products, can be directly used in forming process; Product is purer, even.Shortcoming is that reactor throughput and product purity are lower, and, continuous processing can not be adopted to produce.
The production technique of existing fluoropolymer, although formula is different, the processing parameter of temperature, pressure, polymerization time etc. is different, and their preparation all completes in reactor with aqueous phase form, namely completes in device as shown in Figure 1.There is following shortcoming in process of production:
1, continuous seepage can not be carried out; The reaction of each still is complete, needs to clear up reactor, needs again to prepare burden.Therefore product production is little, can not scale operation.
2, because technique controlling difficulty is large, there is comparatively big error in each still, make the quality of this still product and a upper still product there is larger difference, unstable product quality in batching, technology controlling and process etc.
3, material (comprising the several or all of pure water, tensio-active agent, initiator, dispersion agent, telogen, pH value conditioning agent, stablizer, chain-transfer agent etc.) in aqueous phase, along with constantly adding of monomer, component concentration is wherein changing always, be equivalent to monomer polymerization condition in constantly changing, cause the quality product in this still also to there are differences thus, have impact on result of use.
4, reactor is all generally adopt the mode of stirring rake, but limited due to the structure of still and the structure of stirring rake, and stirring can not ensure that in still, material reaches even, and improves stirring intensity and not only increase energy consumption, and effect is also very limited; Therefore in still, the polymerization of each point is uneven.
5, due to the feature of tank reactor, space is left on the top of reactor, if when the material stirred can not arrive this space or stir not evenly, monomer gas can accumulate somewhere, produces autohemagglutination.If the material of autohemagglutination is more, will blast.
6, because monomer polymerization is thermopositive reaction, the heat energy produced during polymerization is very large; The heat transfer area of reactor is little, and heat-transfer effect is undesirable, and therefore monomer can only enter reactor with the form of gas, makes polymerization reaction time length, yields poorly; If do not control polymerization temperature well, blast during excess temperature, also can be caused.
7, completing the material after polymerization occurs gluing mutually, needs mashing device to carry out being separated or after fragmentation, just reaching service requirements.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, provide the preparation facilities of a kind of fluoropolymer and fluorinated copolymer, this is a kind of device of applicable successive polymerization, carries out in the aqueous phase of polyreaction in pipeline; Additionally provide a kind of preparation technology utilizing the carrying out of apparatus of the present invention to be polymerized simultaneously.
The technical solution used in the present invention is as follows: a kind of device preparing fluoropolymer and fluorinated copolymer, comprising:
Polyreaction pipeline, gas-liquid separation equipment, solid-liquid separating equipment, aqueous phase circulation tank, recycle pump, thermostatted;
Polyreaction pipeline entrance end exports with thermostatted and is connected, and polyreaction pipe outlet is connected with gas-liquid separation equipment;
The fluid output port of gas-liquid separation equipment is connected with solid-liquid separating equipment, and the fluid output port of solid-liquid separation is connected with aqueous phase circulation tank;
The import of recycle pump is connected with aqueous phase circulation tank, and circulation pump outlet is connected with thermostatted import;
Polyreaction pipeline is provided with multiple feed-pipe along its length, and the junction of every root feed-pipe and polyreaction pipeline is all provided with a nozzle;
Polyreaction pipeline is also provided with internal or external heat transfer tube;
One or more positions in polyreaction pipeline are also provided with static mixer;
Aqueous phase circulation tank is provided with multiple feed-pipe for inputting the material such as pure water, tensio-active agent;
Recycle pump can make aqueous phase in aqueous phase circulation tank at this device internal recycle.
As preferably, described polyreaction pipeline is formed by withstand voltage seamless tube manufacture, and its length is 100-12000 with the ratio of caliber.
As preferably, monomer is in a liquid state, by nozzle with the form of fine droplet, enters into the aqueous phase flowed in pipeline.
As preferably, the aqueous phase flow rate in polyreaction pipeline is 6-25m/s.
This device of application prepares a technique for fluoropolymer, for the preparation of the polymerization of a kind of fluorochemical monomer, comprises following steps:
A, by the many feed-pipes be arranged on aqueous phase circulation tank, the material such as pure water, tensio-active agent to be input in aqueous phase circulation tank, and ON cycle pump, the material in aqueous phase circulation tank is circulated in whole device.
B, monomer, with the form of liquid, enter into the nozzle in polyreaction pipeline from monomer A feed-pipe, become microlayer model by nozzle atomization, and mix at the aqueous phase of whole device internal recycle, and static mixer makes this mixing more abundant.
C, while monomer sprays into aqueous phase, initiator is also entered at the aqueous phase of whole device internal recycle by initiator feed pipe.
In d, aqueous phase in polyreaction pipeline, monomer is polymerized under initiator effect; After the polymerization completing 90% ~ 100% monomer mass, the whole materials in polyreaction pipeline enter gas-liquid separation equipment, unconverted monomer with gas form be separated and shift out from gas-liquid separation equipment top.
E, separated in gas-liquid separation equipment monomer gas solidliquid mixture send into equipment for separating liquid from solid, isolated liquid enters aqueous phase circulation groove, continues at system internal recycle; Isolated solid is fluoropolymer solids thing.
The heat energy that f, polyreaction produce is taken away by the heat transferring medium in heat transfer tube internal or external on polyreaction pipeline; From aqueous phase circulation groove aqueous phase out, before entering polyreaction pipeline, in thermostatted, carry out heat exchange, make the temperature of aqueous phase remain on temperature needed for polyreaction.
This device of application prepares a technique for fluorinated copolymer, for the preparation of the copolymerization of 2 kinds of fluorochemical monomers or two or more fluorochemical monomer, comprises following steps:
A, by the many feed-pipes be arranged on aqueous phase circulation tank, the material such as pure water, tensio-active agent to be input in aqueous phase circulation tank, and ON cycle pump, the material in aqueous phase circulation tank is circulated in whole device.
B, monomer A, with the form of liquid, enter into the nozzle in polyreaction pipeline, become microlayer model by nozzle atomization from first feed-pipe, and mix at the aqueous phase of whole device internal recycle.Monomers B, with the form of liquid, enters into the nozzle in polyreaction pipeline, becomes microlayer model by nozzle atomization from second feed-pipe, and mix at the aqueous phase of whole device internal recycle.
C, monomer C ~ N, with the form of liquid, enter into the nozzle in polyreaction pipeline, become microlayer model by nozzle atomization from 3rd ~ n root feed-pipe, and mix at the aqueous phase of whole device internal recycle.
D, initiator are entered at the aqueous phase of whole device internal recycle by (n+1)th feed-pipe.
In e, aqueous phase in polyreaction pipeline, there is copolymerization in each monomer under initiator effect; After the copolymerization completing 10% ~ 100% monomer mass, the whole materials in polyreaction pipeline enter gas-liquid separation equipment, unconverted monomer with gas form be separated and shift out from gas-liquid separation equipment top.
F, separated in gas-liquid separation equipment monomer gas solidliquid mixture send into equipment for separating liquid from solid, isolated liquid enters aqueous phase circulation groove, continues at system internal recycle; Isolated solid is fluoropolymer solids thing.
The heat energy that g, copolyreaction produce is taken away by the heat transferring medium in heat transfer tube internal or external on polyreaction pipeline; From aqueous phase circulation groove aqueous phase out, before entering polyreaction pipeline, in thermostatted, carry out heat exchange, make the temperature of aqueous phase remain on temperature needed for copolyreaction.
Compared with prior art, the present invention has following beneficial effect:
1, aqueous phase is at device internal recycle, completes in the aqueous phase of polyreaction in pipeline, and be carry out with the form of liquid droplet, polymerization efficiency is high.
2, the step such as polyreaction, gas-liquid separation, solid-liquid separation all continuously, circulation carries out, and completes in distinct device; So just can realize continuous seepage, industrial production efficiency improves greatly.
3, polyreaction pipeline structure is simple, easy to manufacture, reduced investment.
4, production operation is simple, convenient, according to existing computer, instrument, the equipment technology such as electric, can form full-automatic production system and Controlling System.
5, the material in aqueous phase can increase and decrease after circulation each time, makes the polymerization of monomer be carry out under stable proportioning, constant product quality.
6, heat exchange is very simple, reliable.All can heat transfer tube be set inside and outside polyreaction pipeline, also the forms such as thermostatted heat exchange can be set; Heat interchanging area increases greatly, even if polymerization efficiency increase makes reaction heat increase a lot, but is still easy to the control of temperature of reaction, polyreaction can be made to be in optimum temps all the time and carry out; But also the blast that occurs because of overheated can be avoided.
7, the static mixer in polyreaction pipeline, to the stirring intensity of fluxion, with stirring rake in reactor to compared with the stirring intensity of liquid, at least improves more than 10 times; Avoid stirring non-uniform phenomenon.
8, because the material in polyreaction pipeline is full of pipeline and in quick flowing, monomer can not produce the phenomenon of local accumulation.The material completing polymerization also can not produce bonding, makes subsequent disposal become simple.
9, owing to stirring evenly, polymerization temperature is controlled, avoid monomer local accumulation, therefore the safety performance of production process improves greatly.
Accompanying drawing explanation
The setting drawing of the original technology of Fig. 1.
Fig. 2 device 200 of the present invention.
01 polyreaction pipeline;
02 gas-liquid separation equipment;
03 recycle pump;
04 solid-liquid separating equipment;
05 aqueous phase circulation tank;
The external heat transfer tube of 06A polyreaction pipeline;
The inner-heating tube of 06B polyreaction pipeline;
06C thermostatted;
07 static mixer;
Monomer A import in 08A polyreaction pipeline and nozzle, be connected with the container of monomer A;
Monomers B import in 08B polyreaction pipeline and nozzle, be connected with the container of monomers B;
Monomer C import in 08C polyreaction pipeline and nozzle, be connected with the container of monomer C;
Initiator import in 08D polyreaction pipeline and nozzle, be connected with the container of initiator;
Return line interface on 11 gas-liquid separation equipments, is connected with polyreaction pipeline;
Monomer outlet on 12 gas-liquid separation equipments;
Liquid exit on 13 gas-liquid separation equipments, is connected with the material inlet of solid-liquid separating equipment;
Liquid exit on 14 solid-liquid separating equipments, is connected with the material inlet of aqueous phase circulation tank;
Solid outlet on 15 solid-liquid separating equipments;
Tensio-active agent import on 16 aqueous phase circulation tanks, is connected with surfactivity agent container;
Purified water inlet on 17 aqueous phase circulation tanks, is connected with pure water container;
18 pump inlet, are connected with aqueous phase circulation tank;
19 circulating-pump outlets, are connected with thermostatted import;
20 thermostatted outlets, are connected with the import of polyreaction pipeline.
Embodiment
Embodiment 1, see Fig. 2, the invention provides the device 200 preparing fluoropolymer and fluorinated copolymer, comprising: polyreaction pipeline 01, gas-liquid separation equipment 02, solid-liquid separating equipment 04, aqueous phase circulation tank 05, recycle pump 03, thermostatted 06C.Polyreaction pipeline 01 entrance end and thermostatted 06C export 20 and are connected, and polyreaction pipeline 01 exit end is connected with the return line interface 11 of gas-liquid separation equipment 02.The fluid output port 13 of gas-liquid separation equipment 02 is connected with solid-liquid separating equipment, and the fluid output port 14 of solid-liquid separating equipment is connected with aqueous phase circulation tank 05.Gas-liquid separation equipment 02 is also provided with monomer outlet 12.Solid-liquid separating equipment 04 is also provided with solid outlet 15.The import 18 of recycle pump 03 is connected with aqueous phase circulation tank, and circulation pump outlet 19 is connected with thermostatted 06C import.Polyreaction pipeline 01 being provided with along its length four feed-pipes, is monomer A, monomers B, monomer C and initiator four feed-pipes respectively.The junction of each feed-pipe and polyreaction pipeline is provided with a nozzle.As shown in the figure, the feed-pipe of monomer A and the junction of polyreaction pipeline 01 are provided with a nozzle 08A, the feed-pipe of monomers B and the junction of polyreaction pipeline 01 are provided with a nozzle 08B, the feed-pipe of monomer C and the junction of polyreaction pipeline 01 are provided with a nozzle 08C, and the feed-pipe of initiator and the junction of polyreaction pipeline 01 are provided with a nozzle 08D.Monomer and initiator in a liquid state, respectively by nozzle with the form of fine droplet, enter into the aqueous phase flowed in pipeline.Aqueous phase flow rate in polyreaction pipeline is 6-25m/s.The duct length of polyreaction pipeline is 100-12000 with the ratio of caliber.Polyreaction pipeline 01 is also provided with inner-heating tube 06B and external heat transfer tube 06A.Multiple positions in polyreaction pipeline 01 are also provided with static mixer 07.Aqueous phase circulation tank 05 is provided with for inputting the feed-pipe 17 of pure water and the feed-pipe for input surface promoting agent 16.Recycle pump 03 can make aqueous phase in aqueous phase circulation tank 05 at this device internal recycle.
Utilize above device first in aqueous phase circulation groove, to add pure water, tensio-active agent etc., ON cycle pump 03, make aqueous phase be in recurrent state.
Initiator, according to proportioning, sprays into polyreaction pipeline 01 by nozzle 08D, enters into the aqueous phase of flowing in polyreaction pipeline 01.
Monomer A, with liquid form, according to proportioning, sprays into polyreaction pipeline by nozzle 08A, enters into the aqueous phase flowed in polyreaction pipeline; Under the effect of initiator, monomer is polymerized in polyreaction pipeline.Static mixer 07 makes the material of flowing play the effect of violent stirring and mixing in pipeline.After the polymerization completing 95% quality monomer, material enters gas-liquid separation equipment, and unconverted monomer gas delivery is exported outside 12 take-off equipments from the monomer gas-liquid separation equipment; The solid-liquid mixture of gas-liquid separation equipment bottom enters solid-liquid separating equipment by the liquid exit 13 on gas-liquid separation equipment, and isolated solids is exactly monomer-polymer, exports this device by the solid outlet 15 on solid-liquid separating equipment; Isolated liquid enters aqueous phase circulation groove by the liquid exit 14 on solid-liquid separating equipment, continues at device internal recycle under recycle pump 03 acts on.
The heat energy that polymerization process is produced is taken away by external heat transfer tube 06A, inner-heating tube 06B, thermostatted 06C; When temperature of charge in pipeline is lower than set(ting)value, heated by thermostatted 06C.
The import of nozzle 08B, nozzle 08C is in closing condition, does not have monomers B or monomer C to enter this device; This embodiment is prepare the embodiment of fluoropolymer.
Embodiment 2, the device of the present embodiment is identical with the apparatus structure of embodiment 1; Just the present embodiment is the embodiment that 2 kinds of fluorochemical monomers prepare multipolymer.Concrete technology is as follows:
First in aqueous phase circulation groove, add pure water, tensio-active agent etc., ON cycle pump, make aqueous phase be in recurrent state.
Initiator, according to proportioning, sprays into polyreaction pipeline by nozzle 08D, enters into the aqueous phase flowed in pipeline reactor.
Monomer A, with liquid form, according to proportioning, sprays into polyreaction pipeline by nozzle 08A, enters into the aqueous phase flowed in polyreaction pipeline; Monomers B, with liquid form, according to proportioning, sprays into polyreaction pipeline by nozzle 08B, enters into the aqueous phase flowed in polyreaction pipeline.Under the effect of initiator, monomer A and monomers B are polymerized in polyreaction pipeline.Static mixer makes the material of flowing play the effect of violent stirring and mixing in pipeline.Monomer A after the polymerization completing 30% quality and monomers B after the polymerization completing 100% quality, material enters gas-liquid separation equipment, and unconverted monomer gas delivery is exported outside 12 take-off equipments from the monomer gas-liquid separation equipment; The solid-liquid mixture of gas-liquid separation equipment bottom enters solid-liquid separating equipment by the liquid exit 13 on gas-liquid separation equipment, and isolated solids is exactly monomer-polymer, exports this device by the solid outlet 15 on solid-liquid separating equipment; Isolated liquid enters aqueous phase circulation groove by the liquid exit 14 on solid-liquid separating equipment, continues at device internal recycle under recycle pump effect.
The heat energy that polymerization process is produced is taken away by external heat transfer tube 06A, inner-heating tube 06B, thermostatted 06C; When temperature of charge in pipeline is lower than set(ting)value, heated by thermostatted 06C.
The import of nozzle 08C is in closing condition, does not have monomer C to enter this device; This embodiment is the embodiment that 2 kinds of fluorochemical monomers prepare multipolymer.
Embodiment 3, the device of the present embodiment is identical with the apparatus structure of embodiment 1; Just the present embodiment is the embodiment that 3 kinds of fluorochemical monomers prepare multipolymer.Concrete technology is as follows:
First in aqueous phase circulation groove, add pure water, tensio-active agent etc., ON cycle pump, make aqueous phase be in recurrent state.
Initiator, according to proportioning, sprays into polyreaction pipeline by nozzle 08D, enters into the aqueous phase flowed in pipeline reactor.
Monomer A, with liquid form, according to proportioning, sprays into polyreaction pipeline by nozzle 08A, enters into the aqueous phase flowed in polyreaction pipeline; Monomers B, with liquid form, according to proportioning, sprays into polyreaction pipeline by nozzle 08B, enters into the aqueous phase flowed in polyreaction pipeline; Monomer C, with liquid form, according to proportioning, sprays into polyreaction pipeline by nozzle 08C, enters into the aqueous phase flowed in polyreaction pipeline.Under the effect of initiator, monomer A, monomers B, monomer C are polymerized in polyreaction pipeline.Static mixer makes the material of flowing play the effect of violent stirring and mixing in pipeline.Monomer A, monomers B, monomer C are after the polymerization completing 10%, 70%, 99% quality respectively, and material enters gas-liquid separation equipment, unconverted monomer gas delivery and from 12 take-off equipments; The solid-liquid mixture of gas-liquid separation equipment bottom enters solid-liquid separating equipment by the liquid exit 13 on gas-liquid separation equipment, and isolated solids is exactly monomer-polymer, exports this device by the solid outlet 15 on solid-liquid separating equipment; Isolated liquid enters aqueous phase circulation groove by the liquid exit 14 on solid-liquid separating equipment, continues at device internal recycle under recycle pump effect.
The heat energy that polymerization process is produced is taken away by external heat transfer tube 06A, inner-heating tube 06B, thermostatted 06C; When temperature of charge in pipeline is lower than set(ting)value, heated by thermostatted 06C.
Claims (6)
1. prepare a device for fluoropolymer and fluorinated copolymer, it is characterized in that, comprising:
Polyreaction pipeline, gas-liquid separation equipment, solid-liquid separating equipment, aqueous phase circulation tank, recycle pump, thermostatted;
Polyreaction pipeline entrance end exports with thermostatted and is connected, and polyreaction pipe outlet is connected with gas-liquid separation equipment
Connect;
The fluid output port of gas-liquid separation equipment is connected with solid-liquid separating equipment, and the fluid output port of solid-liquid separation and aqueous phase circulate
Tank is connected;
The import of recycle pump is connected with aqueous phase circulation tank, and circulation pump outlet is connected with thermostatted import;
Polyreaction pipeline is provided with multiple feed-pipe along its length, the junction of every root feed-pipe and polyreaction pipeline
All be provided with a nozzle;
Polyreaction pipeline is also provided with internal or external heat transfer tube;
One or more positions in polyreaction pipeline are also provided with static mixer;
Aqueous phase circulation tank is provided with multiple feed-pipe for inputting pure water, surfactant material;
Recycle pump can make aqueous phase in aqueous phase circulation tank at this device internal recycle.
2. prepare the device of fluoropolymer and fluorinated copolymer as claimed in claim 1, it is characterized in that, described polymerization
Reacting pipe is formed by withstand voltage seamless tube manufacture, and its length is 100-12000 with the ratio of caliber.
3. prepare the device of fluoropolymer and fluorinated copolymer as claimed in claim 1, it is characterized in that, monomer is at liquid
Under body state, by nozzle with the form of fine droplet, enter into the aqueous phase flowed in pipeline.
4. prepare the device of fluoropolymer and fluorinated copolymer as claimed in claim 1, it is characterized in that, polymerisation tube
Aqueous phase flow rate in road is 6-25m/s.
5. application rights requires that the device described in 1 prepares a technique for fluoropolymer, for the preparation of the polymerization of a kind of fluorochemical monomer, it is characterized in that comprising following steps:
A, by being arranged on many feed-pipes on aqueous phase circulation tank, pure water, surfactant material are input to aqueous phase circulation
In tank, and ON cycle pump, the material in aqueous phase circulation tank is circulated in whole device;
B, monomer, with the form of liquid, enter into the nozzle in polyreaction pipeline from monomer A feed-pipe, pass through nozzle atomization
Become microlayer model, and to mix at the aqueous phase of whole device internal recycle, static mixer makes this mixing more abundant;
C, while monomer sprays into aqueous phase, initiator is also entered at whole device internal recycle by initiator feed pipe
In aqueous phase;
In d, aqueous phase in polyreaction pipeline, monomer is polymerized under initiator effect; Complete 90% ~ 100% list
After the polymerization of weight, the whole materials in polyreaction pipeline enter gas-liquid separation equipment, unconverted monomer with gas form be separated and shift out from gas-liquid separation equipment top;
E, separated in gas-liquid separation equipment monomer gas solidliquid mixture send into equipment for separating liquid from solid, isolated liquid
Body enters aqueous phase circulation groove, continues at system internal recycle; Isolated solid is fluoropolymer solids thing;
The heat energy that f, polyreaction produce is taken away by the heat transferring medium in heat transfer tube internal or external on polyreaction pipeline;
From aqueous phase circulation groove aqueous phase out, before entering polyreaction pipeline, in thermostatted, carry out heat exchange, make the temperature of aqueous phase
Spend the temperature remained on needed for polyreaction.
6. application rights requires that device described in 1 prepares a technique for fluorinated copolymer, for the preparation of 2 kinds of fluorochemical monomers or
The copolymerization of two or more fluorochemical monomer, is characterized in that comprising following steps:
A, by the many feed-pipes be arranged on aqueous phase circulation tank, pure water, surfactant material to be input in aqueous phase circulation tank, and ON cycle pump, the material in aqueous phase circulation tank is circulated in whole device;
B, monomer A, with the form of liquid, enter into the nozzle in polyreaction pipeline, by nozzle mist from first feed-pipe
Change into microlayer model, and to mix at the aqueous phase of whole device internal recycle; Monomers B with the form of liquid, from second feed-pipe
Enter into the nozzle in polyreaction pipeline, become microlayer model by nozzle atomization, mix with the aqueous phase at whole device internal recycle
Close;
C, monomer C ~ N, with the form of liquid, enter into the nozzle in polyreaction pipeline, become microlayer model by nozzle atomization from 3rd ~ n root feed-pipe, and mix at the aqueous phase of whole device internal recycle;
D, initiator enter at the aqueous phase of whole device internal recycle by (n+1)th feed-pipe;
In e, aqueous phase in polyreaction pipeline, there is copolymerization in each monomer under initiator effect; Complete 10% ~ 100%
After the copolymerization of monomer mass, the whole materials in polyreaction pipeline enter gas-liquid separation equipment, unconverted monomer with gas
Volume morphing is separated and shifts out from gas-liquid separation equipment top;
F, separated in gas-liquid separation equipment monomer gas solidliquid mixture send into equipment for separating liquid from solid, isolated liquid
Body enters aqueous phase circulation groove, continues at system internal recycle; Isolated solid is fluoropolymer solids thing;
The heat energy that g, copolyreaction produce is taken away by the heat transferring medium in heat transfer tube internal or external on polyreaction pipeline;
From aqueous phase circulation groove aqueous phase out, before entering polyreaction pipeline, in thermostatted, carry out heat exchange, make the temperature of aqueous phase remain on temperature needed for copolyreaction.
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| CN103554318B (en) * | 2013-10-21 | 2017-04-19 | 衢州市鼎盛化工科技有限公司 | Method and device for preparing fluorine-containing polymer under micro-emulsion form |
| CN105037410A (en) * | 2015-06-18 | 2015-11-11 | 天津市安正电力高分子材料有限公司 | Equipment for producing silane materials through one-step method |
| CN108014741B (en) * | 2016-10-31 | 2020-06-09 | 中国石油化工股份有限公司 | Polymer continuous reaction method and polymer continuous reaction device |
| CN115738985A (en) * | 2022-10-27 | 2023-03-07 | 黄山邦森新材料有限公司 | Tubular reaction system for producing ultra-low molecular weight povidone |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3412779A (en) * | 1966-12-05 | 1968-11-26 | Phillips Petroleum Co | Solvent and polymer recovery in a solution polymerization process |
| GB1229156A (en) * | 1968-02-03 | 1971-04-21 | ||
| US4209436A (en) * | 1977-12-15 | 1980-06-24 | Stamicarbon, B.V. | Process for the removal of non-converted monomers from a copolymer of acrylonitrile |
| US5602216A (en) * | 1995-07-26 | 1997-02-11 | Sulzer Chemtech Ag | Process and apparatus for performing a polymerisation in a tube reactor |
| CN1186077A (en) * | 1996-12-26 | 1998-07-01 | 三井化学株式会社 | Polymerization process using separated flow |
| CN102281943A (en) * | 2009-01-16 | 2011-12-14 | 巴塞尔聚烯烃股份有限公司 | Ethylene polymerization in a high pressure reactor with improved initiator feeding |
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| EP1231194B1 (en) * | 2001-02-10 | 2003-11-12 | Oxeno Olefinchemie GmbH | Preparation of 1-olefins |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3412779A (en) * | 1966-12-05 | 1968-11-26 | Phillips Petroleum Co | Solvent and polymer recovery in a solution polymerization process |
| GB1229156A (en) * | 1968-02-03 | 1971-04-21 | ||
| US4209436A (en) * | 1977-12-15 | 1980-06-24 | Stamicarbon, B.V. | Process for the removal of non-converted monomers from a copolymer of acrylonitrile |
| US5602216A (en) * | 1995-07-26 | 1997-02-11 | Sulzer Chemtech Ag | Process and apparatus for performing a polymerisation in a tube reactor |
| CN1186077A (en) * | 1996-12-26 | 1998-07-01 | 三井化学株式会社 | Polymerization process using separated flow |
| CN102281943A (en) * | 2009-01-16 | 2011-12-14 | 巴塞尔聚烯烃股份有限公司 | Ethylene polymerization in a high pressure reactor with improved initiator feeding |
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