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 PDF

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Publication number
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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temperature
industrial production
polysulfones
filter
material device
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张艳丽
王成
李家旺
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Weihai Pasifeng New Materials Co Ltd
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Weihai Pasifeng New Materials Co Ltd
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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

A kind of polysulfones series macromolecular industrial production of material device
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.
CN201721560660.0U 2017-11-21 2017-11-21 A kind of polysulfones series macromolecular industrial production of material device Active CN207498311U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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