CN207498311U - A kind of polysulfones series macromolecular industrial production of material device - Google Patents
A kind of polysulfones series macromolecular industrial production of material device Download PDFInfo
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- CN207498311U CN207498311U CN201721560660.0U CN201721560660U CN207498311U CN 207498311 U CN207498311 U CN 207498311U CN 201721560660 U CN201721560660 U CN 201721560660U CN 207498311 U CN207498311 U CN 207498311U
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Abstract
The utility model is related to a kind of polysulfones series macromolecular industrial production of material devices, which solve a large amount of high temperature washings, discharge waste water is needed to need in existing method production process, processing, finished product drying time is long, purity is not high, solvent recovering rate is low and technical problem the problem of needing second dehydration, is equipped with the technical solution of the utility model:A kind of polysulfones series macromolecular industrial production of material device, equipped with polymerization reaction kettle, continuous centrifugal filter, accurate filter, granulating system, pelleter and the packing machine coupled successively.Granulating system includes comminutor, temperature regulating device, de- liquid mouth, solvent tank, condenser and vacuum pump set.The utility model is mainly used for the production of the high molecular materials such as polysulfones, polyether sulfone, polyphenylsulfone.
Description
Technical field
The utility model is related to polymeric material field, it is contour to be related to polysulfones, polyether sulfone, polyphenylsulfone for specifically one kind
Molecular material process units.
Background technology
Polysulfones series of products are high molecular polymers, predominantly polysulfones, polyether sulfone, polyphenylsulfone, are a kind of amorphous, thermoplastics
Property resin.Its characteristic is:Excellent in mechanical performance, big, the wear-resisting, high intensity of rigidity etc., due to its good characteristic, the production of polysulfones series
Product have been widely used in the high-end fields such as medical instrument, space flight and aviation, electronics.
Polysulfones series of products polymerization process primary raw material includes 4,4'- dichloro diphenyl sulfones, bisphenol-A, bisphenol S, 4,4 '-biphenyl
Diphenol, sodium hydroxide, potassium carbonate or saleratus etc., polymerize in a solvent, and common solvent has dimethyl sulfoxide (DMSO), N, N- dimethyl
The conducts such as toluene, dimethylbenzene, chlorobenzene may be selected in formamide, n,N-dimethylacetamide, N-Methyl pyrrolidone, sulfolane etc.
Dehydrating agent is blocked with monomer or chloromethanes, and the post processing of polymer is carried out after polymerization.
The post-processing approach of polysulfones high molecular material production at present is water-boiling method.Publication date is on 06 22nd, 2016 patent Shens
Please number:The Chinese invention patent of CN201610141437.6 discloses a kind of polyether sulfone high molecular material production method:Polyether sulfone
After the completion of high molecular material polymerization, pressurizeed with nitrogen polyethers sulfolane solution is pressed directly into fill aqueous solution closed heat partition it is pure
Change in device.Polyethers sulfolane solution is entered with the thread of certain diameter in water by distributor, is distributed in aqueous solution polyether sulfone because molten
Agent is dissolved in aqueous solution and becomes elongated solid, and the particle of certain length is then split by the blender with crushing function.
The inorganic salt particle still wrapped up in the particle of certain length, removing inorganic salt particle need to be through the high temperature of 4 times or more, a large amount of water
It washes, causes product purity not high, high energy consumption wastewater treatment can cause the pollution of environment again.Solvent through distillation can with recycling design,
But solvent recovering rate is low, and the moisture content of recycling design is higher, generally requires second dehydration rear enclosure use.Drying equipment is frequently with drum
Dry, vacuum drying, vacuum spiral belt drying are air-dried, drying process only removes moisture, can not improve the purity of product, water
Drying time is long, increases production cost.
Invention content
The utility model is exactly to solve to need a large amount of high temperature washings, discharge waste water to need to locate in existing method production process
Reason, finished product drying time is long, purity is not high, solvent recovering rate is low and the problem of needing second dehydration, proposes a kind of production process
In without high temperature washing, it is serial without drying, no wastewater discharge, solvent recovering rate is high, finished product purity is high, performance is stablized polysulfones
Macromolecular materials industry process units.
The technical solution of the utility model is:A kind of polysulfones series macromolecular industrial production of material device, equipped with successively
Polymerization reaction kettle, continuous centrifugal filter, accurate filter, granulating system, pelleter and the packing machine of connection.Granulating system packet
Include comminutor, temperature regulating device, de- liquid mouth, solvent tank, condenser and vacuum pump set.
Preferably, granulating system further includes deliming mouth, deliming tourie and water cooling plant.
Preferably, polymerization reaction kettle is enamel reaction still or stainless steel cauldron with Distallation systm.
Preferably, continuous centrifugal filter is that sleeping spiral shell tries sedimentation centrifuge, and horizontal screw unloading filter centrifugal machine is flat
Scraper discharging automatic centrifuge.
Preferably, accurate filter be stud filter, bag filter.
Preferably, comminutor is twin-screw or single screw rod comminutor.
Prior art crushing, washing, dry, solvent recovery manufacturing procedure can be reduced using the utility model device.It is molten
The agent rate of recovery is high, pollution-free, and solvent recovering rate is increased to 95% by existing 75% or so, and recovered solvent can be directly sharp again
With without recycling processing, and without pollutant discharge;Polysulfones high molecular material purity is high, ash content is few, polysulfones high molecular material ash
Point drop to 0.01~0.03% by the 0.2% of the prior art, heat distortion temperature higher, performance is more stable.
Description of the drawings
Fig. 1 is the process flow chart of the utility model;
Fig. 2 is the schematic diagram of the utility model granulating system.
Accompanying drawings symbol description:
1. drive system;2. comminutor;3. feed inlet;4. de- liquid mouth;5. condenser;6. solvent fills;7. vacuum pump set;8.
Deliming tourie;9. deliming mouth;10. water cooling plant;11. temperature-controlling system.
Specific embodiment
A kind of polysulfones series macromolecular industrial production of material device, equipped with polymerization reaction kettle, continuous centrifugal filter, salt
Drier, filtering surge tank, accurate filter, centrifugal pump, clear liquid surge tank, granulating system, pelleter and packing machine.It is granulated system
System includes comminutor 2, temperature regulating device 11, de- liquid mouth 4, solvent tank 6, condenser 5, deliming mouth 9, deliming tourie 8, water cooling plant
10 and vacuum pump set 7.
Polymerization reaction kettle is enamel reaction still or stainless steel cauldron with Distallation systm.
Continuous centrifugal filter is that sleeping spiral shell tries sedimentation centrifuge, horizontal screw unloading filter centrifugal machine, and flat scraper unloads
Expect automatic centrifuge.
Accurate filter be stud filter, bag filter.
Comminutor is twin-screw or single screw rod comminutor.
After the macromolecular material polymerization reactions such as polysulfones, the low water identical with polymerization solvent is added in into polymeric kettle
Divide solvent, for reducing reaction temperature, and terminate polymerisation.By diluted polymeric solution by bottom pipeline enter continuously from
Heart filter, using high-speed rotating centrifugal force, by-product, unreacted salt forming agent and the machinery that separating and filtering removal is reacted are miscellaneous
The large granular impurities such as matter;The polymeric solution tentatively filtered enters accurate filter by filtered fluid surge tank, filters out small miscellaneous
Matter finally obtains the polymer fluid of high-purity.The polymer fluid of high-purity enters after clear liquid surge tank to flow by centrifugal pump is granulated system
System, polymer fluid enter granulating system after de- liquid, deliming, and granulation machine squeezes out wire drawing, cooling solid into strips, strip solid
It is granulated into pelleter, finally completes packaging.
The de- liquid section of granulating system point, deliming are granulated section.De- liquid section includes comminutor 2, de- liquid mouth 4, condenser 5, solvent and fills
6th, vacuum pump set 7 and temperature-controlling system 11, de- liquid section temperature divide multistage, and temperature is incremented by step by step, temperature at 80-220 DEG C, evaporation it is molten
Agent is condensed into liquid through multiple de- liquid mouths 4 into condenser 5, and the solvent for being condensed into liquid enters solvent tank 6, and solvent tank 6 links
Vacuum pump set 7, solvent recovery process carry out under vacuum.Deliming is granulated section and includes comminutor 2, vacuum pump set 7, deliming tourie
8th, deliming mouth 9, water cooling plant 10, temperature-controlling system 11, deliming are granulated section temperature and divide multistage, and temperature is incremented by step by step, and temperature is in 220-
350 DEG C, deliming mouth 9 accesses deliming tourie 8 and vacuum pump set 7, takes off small molecule, unreacted monomer and oligomeric under vacuum
Object.
The utility model is described further with reference to embodiment.
Embodiment one:
4,210 kilograms of 4- dichloro diphenyl sulfones, 183 kilograms of bisphenol S, potassium hydroxide 80 are added in 2000L polymerization reaction kettles
Kilogram, solvent dimethyl sulfoxide (DMSO) 1200L, 150 kilograms of toluene is passed through nitrogen, heats up and start to flow back in 130 DEG C, with dehydrating amount
Increase, when temperature is gradually risen to 175 DEG C, water base removes thorough in polymerization system, and temperature rises to 180 in polymer fluid at this time
DEG C, and keep 180 DEG C of polyethers sulfolane solutions that molecular weight is needed to acquisition.When polyether sulfone polymeric solution reaches target molecular weight,
Dimethyl sulfoxide (DMSO) 150L is quickly added in into kettle, polyether sulfone solution temperature is down to 150 DEG C.Diluted polymer fluid is managed by bottom
Line enters continuous, closing, sedimentation-type centrifuge, by-product, unreacted salt forming agent and the mechanical admixture of filtering removal reaction etc.
Large granular impurity;Polymeric solution through accurate filter, filters out minute impurities again, finally obtains the polymer fluid of high-purity.
Polymer fluid enters screw extruder, and de- liquid section temperature is divided into four sections, and temperature is incremented by step by step, one section of 90 ± 5 DEG C of temperature,
Two sections of 120 ± 5 DEG C, three sections of temperature, 160 ± 5 DEG C, four sections of temperature, 180 ± 5 DEG C of temperature, the solvent of evaporation enter through multiple exhaust outlets
Condenser is condensed into liquid, and the solvent for being condensed into liquid enters solvent receiving tank.Deliming is granulated section temperature and is divided into eight sections, temperature by
Grade is incremented by, one section of 240 ± 5 DEG C, two sections of temperature 250 ± 5 DEG C, three sections of temperature temperature 260 ± 5 DEG C, four sections 270 ± 5 DEG C of temperature, five
280 ± 5 DEG C, six sections of Duan Wendu, 300 ± 5 DEG C, seven sections of temperature, 310 ± 5 DEG C, eight sections 320 ± 5 DEG C of temperature of temperature, the access of deliming mouth
Deliming tourie and vacuum pump take off small molecule, unreacted monomer and oligomer.Screw Extrusion wire drawing, cooling, granulation, packet
Dress.
Polyether sulfone ash content is 0.01% after testing, heat distortion temperature 203 DEG C (1.82MPa).
Embodiment two:
Chlorobenzene, dimethyl sulfoxide (DMSO) 1200L, 160 kilograms of bisphenol-A are added in 2000L polymerization reaction kettles, is passed through nitrogen, is risen
40 DEG C of 60 kilograms of sodium hydroxides of addition of temperature, heat up and start to flow back in 115 DEG C.With the increase of dehydrating amount, temperature gradually rise to
155 DEG C, water base removes thoroughly in polymerization system, cools down 120 DEG C, adds in 4,201 kilograms of 4- dichloro diphenyl sulfones, at this time polymer fluid
Interior temperature rises to 160 DEG C, is kept for 160 DEG C to polysulfones solution of the acquisition with certain molecular weight.Dimethyl sulfoxide (DMSO) 650L is rapidly joined,
Polysulfones solution temperature is down to 130 DEG C, and the ratio of product and total solvent is 28.5% at this time.Diluted polymer fluid is managed by bottom
Line enters continuous, closing, sedimentation-type centrifuge, by-product, unreacted salt forming agent and the mechanical admixture of filtering removal reaction etc.
Large granular impurity;Polymeric solution via the accurate filter under vacuum condition, filters out minute impurities, finally obtains high-purity again
Polymer fluid.
Polymer fluid enters screw extruder, and de- liquid section temperature is divided into four sections, and temperature is incremented by step by step, one section of 80 ± 5 DEG C of temperature,
Two sections of 100 ± 5 DEG C, three sections of temperature, 120 ± 5 DEG C, four sections of temperature, 160 ± 5 DEG C of temperature, the solvent of evaporation enter through multiple exhaust outlets
Condenser is condensed into liquid, and the solvent for being condensed into liquid enters solvent receiving tank.Deliming is granulated section temperature and is divided into eight sections, temperature by
Grade is incremented by, one section of 230 ± 5 DEG C, two sections of temperature 240 ± 5 DEG C, three sections of temperature temperature 250 ± 5 DEG C, four sections 255 ± 5 DEG C of temperature, five
255 ± 5 DEG C, six sections of Duan Wendu, 260 ± 5 DEG C, seven sections of temperature, 265 ± 5 DEG C, eight sections 270 ± 5 DEG C of temperature of temperature, the access of deliming mouth
Deliming tourie and vacuum pump take off small molecule, unreacted monomer and oligomer.Screw Extrusion wire drawing, cooling, granulation, packet
Dress.
Polysulfones ash content is 0.03% after testing, heat distortion temperature 175 DEG C (1.82MPa).
Embodiment three:
It is public that 4,210 kilograms of 4- dichloro diphenyl sulfones, 183 kilograms of bisphenol S, sodium carbonate 150 are added in 2000L polymerization reaction kettles
Jin, solvent N-methyl pyrilidone 1200L, 150 kilograms of toluene are passed through nitrogen, heat up and start to flow back in 120 DEG C, with dehydration
The increase of amount, when temperature is gradually risen to 160 DEG C, water base removes thoroughly in polymerization system, and temperature rises to 180 in polymer fluid at this time
DEG C, kept for 180 DEG C to polyethers sulfolane solution of the acquisition with certain molecular weight.Rapidly join N-Methyl pyrrolidone 240L, polyethers
Sulfolane solution temperature is down to 140 DEG C, and the ratio of product and solvent is 25.7% at this time.By diluted polymer fluid by bottom pipeline into
Enter big of continuous, closing, sedimentation-type centrifuge, by-product, unreacted salt forming agent and the mechanical admixture of filtering removal reaction etc.
Grain impurity;Polymeric solution via the filter under vacuum condition, filters out minute impurities again, finally obtains the polymerization of high-purity
Liquid.
Polymer fluid enters screw extruder, and de- liquid section temperature is divided into four sections, and temperature is incremented by step by step, one section of temperature 100 ± 5
DEG C, two sections of 160 ± 5 DEG C, three sections of temperature, 180 ± 5 DEG C, four sections of temperature, 200 ± 5 DEG C of temperature, the solvent of evaporation is through multiple exhaust outlets
Liquid is condensed into condenser, the solvent for being condensed into liquid enters solvent receiving tank.Deliming is granulated section temperature and is divided into eight sections, temperature
Degree is incremented by step by step, one section of 250 ± 5 DEG C, two sections of temperature, 270 ± 5 DEG C, three sections of temperature, 280 ± 5 DEG C, four sections temperature 290 ± 5 of temperature
DEG C, five sections of 300 ± 5 DEG C, six sections of temperature, 320 ± 5 DEG C, seven sections of temperature, 330 ± 5 DEG C, eight sections 350 ± 5 DEG C of temperature of temperature, deliming mouth
Deliming tourie and vacuum pump are accessed, takes off small molecule, unreacted monomer and oligomer.Screw Extrusion wire drawing is cooled down, is made
Grain, packaging.
Polyether sulfone ash content is 0.02% after testing, heat distortion temperature 203 DEG C (1.82MPa).
Only as described above, only specific embodiment of the utility model, when the utility model cannot be limited with this
The range of implementation, therefore the displacement of its equivalent assemblies or the equivalent variations made according to the utility model patent protection domain and modification,
It all should still belong to the scope that the utility model claims book is covered.
Claims (6)
1. a kind of polysulfones series macromolecular industrial production of material device, it is characterized in that:It is equipped with the polymerisation coupled successively
Kettle, continuous centrifugal filter, accurate filter, granulating system, pelleter and packing machine;The granulating system include comminutor,
Temperature regulating device, de- liquid mouth, solvent tank, condenser and vacuum pump set.
2. polysulfones series macromolecular industrial production of material device according to claim 1, it is characterised in that:The granulation
System further includes deliming mouth, deliming tourie and water cooling plant.
3. polysulfones series macromolecular industrial production of material device according to claim 1 or 2, it is characterised in that:It is described
Polymerization reaction kettle is enamel reaction still or stainless steel cauldron with Distallation systm.
4. polysulfones series macromolecular industrial production of material device according to claim 1 or 2, it is characterised in that:It is described
Continuous centrifugal filter for horizontal helical type sedimentation centrifuge, horizontal screw unloading filter centrifugal machine or flat scraper discharging automatically from
Scheming.
5. polysulfones series macromolecular industrial production of material device according to claim 1 or 2, it is characterised in that:It is described
Accurate filter is stud filter or bag filter.
6. polysulfones series macromolecular industrial production of material device according to claim 1 or 2, it is characterised in that:It is described
Comminutor is twin-screw or single screw rod comminutor.
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Publication number | Priority date | Publication date | Assignee | Title |
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CN114292401A (en) * | 2021-12-14 | 2022-04-08 | 山东科院天力节能工程有限公司 | Synthesis method and system of polysulfone series resin |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114292401A (en) * | 2021-12-14 | 2022-04-08 | 山东科院天力节能工程有限公司 | Synthesis method and system of polysulfone series resin |
CN114292401B (en) * | 2021-12-14 | 2024-03-08 | 山东科院天力节能工程有限公司 | Synthesis method and system of polysulfone series resin |
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