CN106220853A - A kind of polysulfone resin industrialized producing technology - Google Patents
A kind of polysulfone resin industrialized producing technology Download PDFInfo
- Publication number
- CN106220853A CN106220853A CN201610818935.XA CN201610818935A CN106220853A CN 106220853 A CN106220853 A CN 106220853A CN 201610818935 A CN201610818935 A CN 201610818935A CN 106220853 A CN106220853 A CN 106220853A
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- Prior art keywords
- temperature
- polyreaction
- reaction kettle
- polymerization reaction
- polysulfone resin
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- 229920002492 poly(sulfone) Polymers 0.000 title claims abstract description 156
- 229920005989 resin Polymers 0.000 title claims abstract description 125
- 239000011347 resin Substances 0.000 title claims abstract description 125
- 238000005516 engineering process Methods 0.000 title claims abstract description 44
- 239000000463 material Substances 0.000 claims abstract description 81
- 238000004519 manufacturing process Methods 0.000 claims abstract description 20
- 238000002203 pretreatment Methods 0.000 claims abstract description 13
- 238000006116 polymerization reaction Methods 0.000 claims description 228
- 238000006243 chemical reaction Methods 0.000 claims description 79
- 238000001514 detection method Methods 0.000 claims description 79
- 238000000034 method Methods 0.000 claims description 48
- 239000002904 solvent Substances 0.000 claims description 42
- 239000003153 chemical reaction reagent Substances 0.000 claims description 41
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims description 37
- 239000003960 organic solvent Substances 0.000 claims description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- 229910001868 water Inorganic materials 0.000 claims description 37
- 239000007788 liquid Substances 0.000 claims description 36
- 239000004020 conductor Substances 0.000 claims description 35
- 239000011229 interlayer Substances 0.000 claims description 28
- 230000004907 flux Effects 0.000 claims description 27
- 239000007789 gas Substances 0.000 claims description 27
- 238000001816 cooling Methods 0.000 claims description 23
- 239000011259 mixed solution Substances 0.000 claims description 22
- 238000001704 evaporation Methods 0.000 claims description 18
- 230000008020 evaporation Effects 0.000 claims description 18
- 150000003254 radicals Chemical class 0.000 claims description 17
- 229910052756 noble gas Inorganic materials 0.000 claims description 16
- 238000000926 separation method Methods 0.000 claims description 16
- 238000000746 purification Methods 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 14
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 13
- 238000001125 extrusion Methods 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 11
- 238000005649 metathesis reaction Methods 0.000 claims description 11
- 238000012805 post-processing Methods 0.000 claims description 11
- 230000007062 hydrolysis Effects 0.000 claims description 10
- 238000006460 hydrolysis reaction Methods 0.000 claims description 10
- 238000009835 boiling Methods 0.000 claims description 9
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 8
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 125000001174 sulfone group Chemical group 0.000 claims description 2
- MCZQGJXPPZHLTG-UHFFFAOYSA-N C.[Cl] Chemical group C.[Cl] MCZQGJXPPZHLTG-UHFFFAOYSA-N 0.000 claims 1
- 239000004215 Carbon black (E152) Substances 0.000 abstract description 8
- 229930195733 hydrocarbon Natural products 0.000 abstract description 8
- 238000009826 distribution Methods 0.000 abstract description 6
- 150000002430 hydrocarbons Chemical class 0.000 abstract description 5
- 239000002861 polymer material Substances 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 description 20
- 239000000243 solution Substances 0.000 description 18
- 238000003756 stirring Methods 0.000 description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 14
- 238000005259 measurement Methods 0.000 description 14
- 239000012071 phase Substances 0.000 description 14
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 13
- 239000000376 reactant Substances 0.000 description 11
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 8
- 229920000642 polymer Polymers 0.000 description 8
- 239000012458 free base Substances 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 229940106691 bisphenol a Drugs 0.000 description 5
- 239000006228 supernatant Substances 0.000 description 5
- 239000010409 thin film Substances 0.000 description 5
- 230000000007 visual effect Effects 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 230000006872 improvement Effects 0.000 description 4
- 239000002952 polymeric resin Substances 0.000 description 4
- 239000001103 potassium chloride Substances 0.000 description 4
- 235000011164 potassium chloride Nutrition 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- 150000003457 sulfones Chemical class 0.000 description 4
- 229920003002 synthetic resin Polymers 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- -1 hydrocarbon free radical Chemical class 0.000 description 3
- 230000000977 initiatory effect Effects 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 102000004895 Lipoproteins Human genes 0.000 description 2
- 108090001030 Lipoproteins Proteins 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000004308 accommodation Effects 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 210000003746 feather Anatomy 0.000 description 2
- 244000144992 flock Species 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 210000002784 stomach Anatomy 0.000 description 2
- 229920005992 thermoplastic resin Polymers 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- IBRQUKZZBXZOBA-UHFFFAOYSA-N 1-chloro-3-(3-chlorophenyl)sulfonylbenzene Chemical compound ClC1=CC=CC(S(=O)(=O)C=2C=C(Cl)C=CC=2)=C1 IBRQUKZZBXZOBA-UHFFFAOYSA-N 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 239000004811 fluoropolymer Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 229940050176 methyl chloride Drugs 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- RAYLUPYCGGKXQO-UHFFFAOYSA-N n,n-dimethylacetamide;hydrate Chemical compound O.CN(C)C(C)=O RAYLUPYCGGKXQO-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000002896 organic halogen compounds Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000002151 riboflavin Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 238000005829 trimerization reaction Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
- C08G75/20—Polysulfones
- C08G75/23—Polyethersulfones
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Other Resins Obtained By Reactions Not Involving Carbon-To-Carbon Unsaturated Bonds (AREA)
Abstract
The present invention relates to field of polymer material preparing technology, be specifically related to a kind of polysulfone resin industrialized producing technology, comprise the following steps: step one: polyreaction pre-treatment；Step 2: polyreaction；Step 3: polyreaction terminates.The polysulfone resin industrialized producing technology that the present invention provides solves the problem that polysulfones macromolecular material polymeric hydrocarbon molecular weight distribution span is big.The industrialized producing technology that the present invention improves makes the polysulfones macromolecular material purity produced high, and molecular weight distribution is concentrated, and production efficiency is higher, and quality is more stable.
Description
Technical field
The present invention relates to field of polymer material preparing technology, be specifically related to a kind of polysulfone resin industrialized producing technology.
Background technology
Polysulfones is containing alkyl-SO in molecular backbone2The thermoplastic resin of-alkyl chain link, polysulfone resin is slightly succinum
The armorphous transparent or semitransparent polymer of color, excellent in mechanical performance, rigidity is big, and wear-resisting, high intensity, even if the most also keeping
Excellent mechanical performance is the advantage that it is prominent, can make precise measure goods, may be adapted to make heat-resistant piece, insulating part, subtract
Mill wearing piece, instrument and meter part and medical apparatus and instruments part.Specifically be mainly used in electric, food and article of everyday use, automobile with,
The departments such as aviation, medical treatment and general industry, make various catalyst, connector, insulating part of transformer, controllable silicon cap, insulation sleeve
Pipe, coil rack, binding post, printed circuit board (PCB), axle sleeve, cover, television system part, capacitor film, brushgear housing, alkalescence electric power storage
Pond box, electric wire are coated with.PSF also can do protective cover element, electric gear, battery cap, aircraft inside and outside spare and accessory parts, aerospace
Device exterior protection cover, device plate washer of taking a picture, lamp part, sensor.Glass and rustless steel is replaced to make steam service plate, coffee vessel,
Cooking apparatus using microwave, milk vessel, milker parts, drink and food allotter.Health and medical apparatus and instruments aspect have surgical operation
Dish, aerosol apparatus, humidifier, dental instruments, flow controller, grooving device and laboratory apparatus, it may also be used for have a denture made, adhesive strength
Height, also can make chemical industry equipment (pump outer housing, tower external protection, acidproof nozzle, pipeline, valve pack), food processing equipment, dairy
Product process equipment, environment protection control infect equipment.For the optimization of the industrialized process for preparing of polysulfone resin, to become this area skill
The focus of attention of art personnel.
In currently available technology, for traditional production process of polysulfone resin can be divided into into salt, concentration, isolation of purified,
The process such as solvent recovery and pelletize, polycondensating process is divided into again one-step method and two-step method.The one-step method i.e. sodium salt of bisphenol-A or potassium salt are
Initiation material, with DDS in the presence of sulfone kind solvent, polycondensation synthesis PSF successively.Two steps are i.e. become salt by bisphenol-A, are concentrated two groups
Become.In order to increase recycled solvent degree further, improve preparation efficiency, reduce discharge of wastewater, for above-mentioned production technology
Having done corresponding improvement technology, such as application publication number in prior art is the patent of invention of CN 104629055 A, discloses work
Industry metaplasia produce polysulfones macromolecular material method, comprise the steps of after (1) polysulfones macromolecule material solution polyreaction terminates
Polymeric kettle adds the low moisture content solvent identical with polymerization solvent and stirs；(2) stirring, static separation 10～90 points are stopped
Clock；(3) supernatant is extracted when unreacted catalyst, the by-product inorganic salts of reaction and mechanical admixture sink to bottom reactor
In solvent kettle；With the product in low moisture content solvent extraction settled layer, again settle, with first in extraction supernatant to solvent kettle
Secondary clear liquid merges；(4) squeezing in thin film evaporation unit quantitatively, continuously by the solution of solvent kettle, solution is in the thin film evaporation of heating
Device stomach wall forms thin film and rapid steaming sends solvent；(5) the condensed device of solvent evaporated enters in solvent output device, reclaims
Solvent can be directly used for next time polyreaction in, it is not necessary to process；(6) polymer after evaporation solvent is at thin film evaporation unit
Stomach wall forms solid, and solid forms powder under the stirring action of wall built-up form；(7) polymer powders is through thin film evaporation unit still
Bottom pipeline enters granulator granulation to be terminated.
But in above-mentioned improvement technique and equipment, when polymer material reacts, due to polysulfones macromolecular material polymeric hydrocarbon
Molecular weight distribution span is big, does not carry out effective temperature control process for response system, thus improves what preparation of industrialization produced
Dangerous；Simultaneously after polyreaction terminates, employing interpolation is dripped after part solvent bank sedimentation, extracts supernatant, simultaneously will be again
Sedimentation, extraction supernatant both sides supernatant, the method step is complicated, and can not effectively be washed out by organic solvent, reduces life
Produce efficiency.
As can be seen here, can be based on the not enough polysulfone resin industrialized production work providing a kind of improvement of the prior art
Skill so that it is can effectively solve the problem that above-mentioned technical problem, reduces industrially prepared danger, makes to prepare the operation of polysulfone resin simultaneously
More convenient and efficient, improves production efficiency, becomes the technical barrier that those skilled in the art are urgently to be resolved hurrily.
Summary of the invention
The present invention is to solve above-mentioned technical problem, it is provided that a kind of polysulfone resin industrialized producing technology so that polysulfones tree
The preparation process of fat effectively controls polymerization rate, makes whole polymerization process more controllable, reduce industrialized production
Danger, make the polysulfone resin molecular weight distribution of preparation concentrate, production efficiency more high-quality is more stable.
In order to reach above-mentioned technique effect, the present invention includes techniques below scheme:
A kind of polysulfone resin industrialized producing technology, comprises the following steps:
Step one: polyreaction pre-treatment: add the polymerization reactant for preparing polysulfone resin in polymerization reaction kettle
Material, opens agitator in polymeric kettle, is passed through noble gas, gas-phase space gas in metathesis polymerizable reactor in polymerization reaction kettle
After, it is passed through high-temperature heat-conductive material to the interlayer of polymerization reaction kettle, makes the polyreaction material in polymerization reaction kettle reach polymerization anti-
Answer temperature；
Step 2: polyreaction: continue the interlayer to polymerization reaction kettle and be passed through high-temperature heat-conductive material, filled by viscosity measurements
Put the viscosity in detection polymerization reaction kettle, by the temperature in temperature-detecting device detection polymerization reaction kettle, when temperature detection fills
Conveying high-temperature heat-conductive material is stopped when putting the temperature information of detection less than 10～50 DEG C of polymeric reaction temperature；When temperature detection fills
When putting the temperature value of detection more than polymeric reaction temperature scope, then in polymerization reaction kettle, it is passed through cooling solvent, controls polymerization anti-
Answer the temperature in still in the range of polymeric reaction temperature；
Step 3: polyreaction terminates: when the viscosity number of viscosity detecting device detection reaches target viscosities, terminate polymerization
Reaction, reduces polyreaction temperature in the kettle and obtains polysulfone resin through separating out with purification processes.
Wherein the temperature of high-temperature heat-conductive material depends on the reaction temperature of polyreaction, and generates product and the physics of solvent
Character.Those skilled in the art, can directly determine the temperature model of high-temperature heat-conductive material based on present invention and prior art
Enclose value.Described high-temperature heat-conductive material can be conduction oil, in art technology, every can be passed through interlayer and play intensification make
Heat Conduction Material the most within the scope of the present invention.Simultaneously because exothermic reaction when preparing the reaction of polysulfone resin, this
The method conservative control of bright offer stops the time of conveying high-temperature heat-conductive material, carries out effectively for the temperature in polymerization reaction kettle
Control, when reacting, it is possible to persistently ensure that the temperature in polymerization reaction kettle is positioned in the range of reaction temperature.
Further, when the viscosity number of viscosity detecting device detection reaches target viscosities, it is passed through in polymerization reaction kettle
Capping reagent, makes polymeric hydrocarbon free radical replace, and after in reactor to be polymerized, organic solvent viscosity is stationary value, stops being passed through end-blocking
Reagent, terminates polyreaction.
Described viscosity detecting device can be viscometer；Can be in the case of voltage stabilization, the real-time current of stirring paddle
Conversion；It can also be the moment of torsion conversion of output in real time of converter.Those skilled in the art can select most suitable as required
Viscosity detecting device.
Known polyreaction middle and late stage starts, and according to reaction principle, its polyreaction is between long chain hydrocarbon and long chain hydrocarbon
Polyreaction, the molecular weight after polymerization is multiplied.Therefore controlling the polymerization in later stage well, the control to the degree of polymerization is favourable.This
After bright polysulfones macromolecular material reaches targeted degree of polymerization, add capping reagent, replace polysulfone resin end free base, employingization
Learn reactive mode and terminate polymerization, effectively control the polymerization of polymerization reaction late stage, make degree of polymerization reaction more controllable.
Further, described polyreaction material is the polyreaction material with free radical, described polymerization reaction kettle
The capping reagent being inside passed through makes the polysulfone resin free radical displacement of preparation in polyreaction.Capping reagent can replace polysulfone resin
End free base, makes chemical reaction terminate polymerization.
Further, described capping reagent is chloromethanes；Described noble gas is nitrogen or carbon dioxide.The present invention adopts
With chloromethanes as capping reagent, effectively making polyreaction terminate, owing to chloromethanes is flammable explosive gas, the present invention rationally sets
Count each step, effectively decompose for chloromethanes and discharge, improve efficiency and safety prepared by polysulfone resin, with existing skill
Art is compared, and it prepares better.
Further, described polysulfone resin industrialized producing technology also includes step 4: polyreaction post processing, general is polymerized
The mixed solution obtained after polymerization reaction terminating in reactor is emitted in water by drainage line, makes residual in organic solvent
Chloromethanes hydrolyzes, and dissolves polysulfone resin in organic solvent and separates out, described drainage line is provided with switch valve.
Further, the outfan of described drainage line connects nozzle；The temperature of described water is 55～59 DEG C；To in water
The polysulfone resin separated out uses water-boiling method to carry out purification processes；Purified process after heat expressing technique extrusion obtains polysulfones bar；
The temperature of described hot-extrudable technique is 170～175 DEG C.
It is further preferred that the temperature of described hot-extrudable technique is 174 DEG C.
When 174 DEG C of hot-extrudable bars of polysulfone resin, add the visual clarity of the polysulfones bar of capping reagent chloromethanes
More preferably, add the polysulfones of capping reagent chloromethanes, cross dimeric molecule less, be suitable for injection and hot melting temperature is stable；It is not added with end-blocking
The polysulfones of reagent is under same extrusion temperature, and the visual clarity of polysulfones bar is not so good as the former, when promoting suitable extrusion temperature
After, transparency improves, and part high polymer does not melt, and affects transparency during extrusion, and high polymer was dimeric molecule.
Drainage line nozzle design bottom polymerization reaction kettle, the polysulfone resin solution that can make precipitation is steady, controlled.
The hydrolysis temperature of chloromethanes 60 DEG C, actively promotes the temperature of water so that the water temperature in pond is positioned at about 58 DEG C, can
Hydrolyze in the contact of same water being effectively dissolved in the chloromethanes of organic solvent simultaneously, generate methanol and hydrochloric acid, hydrochloric acid simultaneously with
Excess carbonic acid nak response generates potassium bicarbonate and potassium chloride, improves safety when separating out polysulfones.
Further, in described drainage line, mixed solution is delivered in pure water by switch valve discontinuity；
The method using the discontinuous discharge mixed solution containing polysulfone resin, during can improving organic solvent emission
Dilution effect, reduce the risk producing line clogging in subsequent wash operation, it is little, all that the resin in pond separates out volume
Even, facilitate water-boiling method post processing.
Further, a length of 5s when switch valve is opened every time, a length of 10s during closedown, open and close and alternately control.
Those skilled in the art can select to open duration and closedown according to concrete industrialized production quantity and equipment situation
Duration.
Further, in step 2, it is passed through in the flow-control polymerization reaction kettle of high-temperature heat-conductive material by regulation
Temperature；In described step 3, polymerization reaction kettle is 60～70 DEG C obtains mixed solution through being naturally cooling to temperature, and described mixing is molten
Liquid obtains polysulfone resin through separating out with purification processes.
Owing to polysulfones macromolecular material polymerization process is exothermic reaction, suitable control polymeric reaction temperature, can make to gather
Conjunction process is more steady.Simultaneously as the kind of the i.e. polysulfones of polyreaction material is different, its temperature control point is according to polysulfones
Good reaction temperature scene adjusts, and wherein bisphenol-A class polysulfones control temperature is at 150～165 DEG C, then, when reacting, need to keep
Temperature in polymerization reaction kettle is 150～165 DEG C.The most too high by the temperature in suitably control reactor, can control to gather
Sulfone reacts at about 160 DEG C, makes polyreaction excessively acutely will not reduce evaporation capacity, reduces energy consumption.
Further, described polyreaction material includes bisphenol-A class polysulfones.
Further, described polymerization reaction kettle top connects polymerization tower, and described polymerization tower top connects condenser, institute
The outfan connection stating condenser has gas-liquid separator, described gas-liquid separator to be connected to chilling flux bath and output dress
Put；
In polyreaction starts the time period being completely exhausted out to polymeric reaction product, continue open cold condenser and polymerization tower
Between valve, control condenser inner condensat liquid temperature be less than 63 DEG C, make the solvent of evaporation and the condensed device of gas of evaporation
Inputting to gas-liquid separation tower, the liquid flux of separation is passed through chilling flux bath by described gas-liquid separation tower, and by separation
Gas is passed through output device and discharges；
Described chilling flux bath is connected by switch valve with polymerization reaction kettle, when in polymerization stage, if temperature inspection
The temperature value surveying device detection is more than range of reaction temperature, then open the switch valve between chilling flux bath and polymerization reaction kettle,
Cooling solvent is made to be passed through in polymerization reaction kettle；After polyreaction terminates, collect course of reaction is evaporated and condensed device and
Gas-liquid separator processes the organic solvent obtained.
When polyreaction is carried out, in its raw material, intermediate and finished product, flash-point minimum organic solvent N, N-dimethyl second
Amide, flash-point value is 66 DEG C.The organic solvent that the setting of condenser can make response system export is in less than 63 DEG C (i.e. at it
Below flash-point) in the environment of export, by the design of this structure, make full polymerization process be in all process materials flash-points with
Exterior domain, reduces it dangerous.
Further, after terminating polyreaction, stop being passed through noble gas, and open chilling flux bath and polymerization reaction kettle
Between valve, cooling solvent discharge is entered in polymerization reaction kettle, then reduce polyreaction temperature in the kettle through separate out and purify
Process obtains polysulfone resin.
Production technology of the present invention is suitable for the preparation of all polysulfones macromolecular materials and produces, and polyreaction material can
To select the most accordingly, production technology of the present invention is the most applicable.
Use technique scheme, including following beneficial effect: a kind of polysulfone resin industrialized production that the present invention provides
Technique, solves the problem that polysulfones macromolecular material polymeric hydrocarbon molecular weight distribution span is big.The industrialized production that the present invention improves
Technique makes the polysulfones macromolecular material purity produced high, and molecular weight distribution is concentrated, and production efficiency is higher, and quality is more stable.
Accompanying drawing explanation
Fig. 1 is device structure schematic diagram used in polysulfone resin industrialized producing technology of the present invention；
Fig. 2 is polysulfone resin embodiment one of the present invention and embodiment trimerization course of reaction viscosity measurements schematic diagram.
In figure,
1, polymerization reaction kettle；11, chuck；12, cylinder；2, polymerization tower；3, condenser；4, nozzle；5, cooling oil conveying dress
Put；6, capping reagent tank；7, gas-liquid separator；8, glass regards bucket；9, chilling flux bath；101, pond；102, solvent tank.
Detailed description of the invention
Below by specific embodiment, the present invention is described in further detail.
Embodiment one: a kind of polysulfone resin industrialized producing technology, comprises the following steps:
Step one: polyreaction pre-treatment: add the polymerization reactant for preparing polysulfone resin in polymerization reaction kettle
Material, opens agitator in polymeric kettle, is passed through noble gas, gas-phase space gas in metathesis polymerizable reactor in polymerization reaction kettle
Body, is passed through high-temperature heat-conductive material to the interlayer of polymerization reaction kettle, makes the polyreaction material in polymerization reaction kettle reach polymerization anti-
Answer temperature.
Step 2: polyreaction: continue the interlayer to polymerization reaction kettle and be passed through high-temperature heat-conductive material, filled by viscosity measurements
Put the viscosity in detection polymerization reaction kettle, by the temperature in temperature-detecting device detection polymerization reaction kettle, when temperature detection fills
Conveying high-temperature heat-conductive material is stopped when putting the temperature information of detection less than 10～50 DEG C of polymeric reaction temperature；When temperature detection fills
When putting the temperature value of detection more than polymeric reaction temperature scope, then in polymerization reaction kettle, it is passed through cooling solvent, controls polymerization anti-
Answer the temperature in still in the range of polymeric reaction temperature；
Step 3: polyreaction terminates: when the viscosity number of viscosity detecting device detection reaches target viscosities, terminate polymerization
Reaction, reduces polyreaction temperature in the kettle and obtains polysulfone resin through separating out with purification processes.
Embodiment two: a kind of polysulfone resin industrialized producing technology, comprises the following steps:
Step one: polyreaction pre-treatment: add the polymerization reactant for preparing polysulfone resin in polymerization reaction kettle
Material, described polyreaction material is the polyreaction material with free radical, opens agitator in polymeric kettle, to polyreaction
Noble gas it is passed through in still, gas-phase space gas in metathesis polymerizable reactor, it is passed through high-temperature heat-conductive to the interlayer of polymerization reaction kettle
Material, makes the polyreaction material in polymerization reaction kettle reach polymeric reaction temperature；
Step 2: polyreaction: continue the interlayer to polymerization reaction kettle and be passed through high-temperature heat-conductive material, filled by viscosity measurements
Put the viscosity in detection polymerization reaction kettle, by the temperature in temperature-detecting device detection polymerization reaction kettle, when temperature detection fills
Conveying high-temperature heat-conductive material is stopped when putting the temperature information of detection less than 10～50 DEG C of polymeric reaction temperature；When temperature detection fills
When putting the temperature value of detection more than polymeric reaction temperature scope, then in polymerization reaction kettle, it is passed through cooling solvent, controls polymerization anti-
Answer the temperature in still in the range of polymeric reaction temperature；
Step 3: polyreaction terminates: when the viscosity number of viscosity detecting device detection reaches target viscosities, anti-to polymerization
Be passed through capping reagent in answering still, the capping reagent being passed through in described polymerization reaction kettle make in polyreaction the polysulfone resin of preparation from
Replaced by base, after organic solvent viscosity is stationary value in reactor to be polymerized, stop being passed through capping reagent, terminate polyreaction,
Reduce polyreaction temperature in the kettle and obtain polysulfone resin through separating out with purification processes.
Embodiment three: a kind of polysulfone resin industrialized producing technology, comprises the following steps:
Step one: polyreaction pre-treatment: add the polymerization reactant for preparing polysulfone resin in polymerization reaction kettle
Material, described polyreaction material is the polyreaction material with free radical, and it includes bisphenol-A class polysulfones, opens polymeric kettle
Interior agitator, is passed through noble gas in polymerization reaction kettle, and gas-phase space gas in metathesis polymerizable reactor, to polymerization reaction kettle
Interlayer be passed through high-temperature heat-conductive material, make the polyreaction material in polymerization reaction kettle reach polymeric reaction temperature；Described inertia
Gas is nitrogen or carbon dioxide.
Step 2: polyreaction: continue the interlayer to polymerization reaction kettle and be passed through high-temperature heat-conductive material, filled by viscosity measurements
Put the viscosity in detection polymerization reaction kettle, by the temperature in temperature-detecting device detection polymerization reaction kettle, when temperature detection fills
Conveying high-temperature heat-conductive material is stopped when putting the temperature information of detection less than 10～50 DEG C of polymeric reaction temperature；When temperature detection fills
When putting the temperature value of detection more than polymeric reaction temperature scope, then in polymerization reaction kettle, it is passed through cooling solvent, controls polymerization anti-
Answer the temperature in still in the range of polymeric reaction temperature；
Step 3: polyreaction terminates: when the viscosity number of viscosity detecting device detection reaches target viscosities, anti-to polymerization
It is passed through chloromethanes in answering still, makes polymeric hydrocarbon free radical replace, after organic solvent viscosity is stationary value in reactor to be polymerized, stop
Being passed through capping reagent, the capping reagent being passed through in described polymerization reaction kettle makes the polysulfone resin free radical of preparation in polyreaction put
Change, terminate polyreaction, reduce polyreaction temperature in the kettle and obtain polysulfone resin through separating out with purification processes.
When preparing polysulfone resin, there is the viscosity measurements in polyreaction as shown in Figure 2 in embodiment one and embodiment three.
Curve A be embodiment one when preparing polysulfone resin, there is the viscosity measurements curve in polyreaction, curve B is embodiment three
When preparing polysulfone resin, there is the viscosity measurements curve in polyreaction.
Polysulfones is a kind of thermoplastic resin, and when dissolving in organic solvent, the viscosity of its organic solution promotes with the degree of polymerization
And it is linearly increasing.Therefore can be by its degree of polymerization of viscosity indirect reaction of organic solution.The viscosity of organic solution can be by viscous
Degree meter, the load current value of stirring slurry, stirring paddle converter output torque value directly or indirectly reflect.Use in the detection
Stirring paddle load current value is as the qualitative reference of the degree of polymerization (viscosity).
In fig. 2, each letter implication is as follows:
T1: be warming up to start polymeric reaction temperature time point；
T2: polyreaction arrives target needs end time point；
T3: add chloromethanes, all block time point；
T4: be cooled to stop polymeric reaction temperature time point；
L1: be warming up to start polymeric reaction temperature current value；
Current value at the end of L2: polyreaction needs；
L3: be passed through chloromethanes and blocked current value；
L4: be cooled to stop polymeric reaction temperature current value.
As shown in Figure 2, before T2 time point (being i.e. initially added into chloromethanes time point), two curves represent respectively and are passed through
Two curves are consistent, but after arriving target viscosities, even if starting the external world to intervene cooling, its polyreaction is the most persistently entered
OK, until during less than polyreaction initiation temperature.Visual data reflection is exactly that the load current value of its stirring paddle persistently increases
Being added to temperature when being reduced to polyreaction initiation temperature, electric current starts to stablize constant.
After arriving target viscosities, adding chloromethanes reagent, after continuing 3～5 minutes, stirring paddle load current value will not
Increase the most in time and increase.Analyzing reason is in 3～5 minutes, and polysulfone resin there occurs that end capping reaction, free radical are set to
Changing, polyreaction passes through chemical means force termination.
As shown in Figure 2, embodiment one, in the experiment not using terminal reagent, is terminated reaction and is carried out by cooling,
Owing to temperature-fall period is slow release process, polyreaction was persistently carried out within considerable time, and the polysulfone resin finally obtained gathers
The right targeted degree of polymerization that will be greater than, or rule of thumb, carry out in advance terminating converging operationJu Hecaozuo, be limited by the impact of operating experience factor
Greatly, the degree of polymerization controls more extensive.When embodiment three uses chloromethanes as end-capping reagent, reaction will terminate rapidly, the degree of polymerization
Control more accurate.
Embodiment four: a kind of polysulfone resin industrialized producing technology, comprises the following steps:
Step one: polyreaction pre-treatment: add the polymerization reactant for preparing polysulfone resin in polymerization reaction kettle
Material, described polyreaction material is the polyreaction material with free radical, opens agitator in polymeric kettle, to polyreaction
Noble gas it is passed through in still, gas-phase space gas in metathesis polymerizable reactor, it is passed through high-temperature heat-conductive to the interlayer of polymerization reaction kettle
Material, makes the polyreaction material in polymerization reaction kettle reach polymeric reaction temperature；
Step 2: polyreaction: continue the interlayer to polymerization reaction kettle and be passed through high-temperature heat-conductive material, filled by viscosity measurements
Put the viscosity in detection polymerization reaction kettle, by the temperature in temperature-detecting device detection polymerization reaction kettle, when temperature detection fills
Conveying high-temperature heat-conductive material is stopped when putting the temperature information of detection less than 10～50 DEG C of polymeric reaction temperature；When temperature detection fills
When putting the temperature value of detection more than polymeric reaction temperature scope, then in polymerization reaction kettle, it is passed through cooling solvent, controls polymerization anti-
Answer the temperature in still in the range of polymeric reaction temperature；
Step 3: polyreaction terminates: when the viscosity number of viscosity detecting device detection reaches target viscosities, anti-to polymerization
Being passed through chloromethanes in answering still, the capping reagent being passed through in described polymerization reaction kettle makes the polysulfone resin of preparation in polyreaction free
Base is replaced, and after organic solvent viscosity is stationary value in reactor to be polymerized, stops being passed through capping reagent, terminates polyreaction,
To mixed solution, reduce polyreaction temperature in the kettle；
Step 4: polyreaction post processing, the mixed solution obtained after being polymerized reaction terminating in polymerization reaction kettle passes through
Drainage line is emitted in water, makes the chloromethanes hydrolysis of residual in organic solvent, dissolves polysulfone resin analysis in organic solvent
Go out, described drainage line is provided with switch valve.
Embodiment five: a kind of polysulfone resin industrialized producing technology, comprises the following steps:
Step one: polyreaction pre-treatment: add the polymerization reactant for preparing polysulfone resin in polymerization reaction kettle
Material, described polyreaction material is the polyreaction material with free radical, opens agitator in polymeric kettle, to polyreaction
Noble gas it is passed through in still, gas-phase space gas in metathesis polymerizable reactor, it is passed through high-temperature heat-conductive to the interlayer of polymerization reaction kettle
Material, makes the polyreaction material in polymerization reaction kettle reach polymeric reaction temperature；
Step 2: polyreaction: continue the interlayer to polymerization reaction kettle and be passed through high-temperature heat-conductive material, filled by viscosity measurements
Put the viscosity in detection polymerization reaction kettle, by the temperature in temperature-detecting device detection polymerization reaction kettle, when temperature detection fills
Conveying high-temperature heat-conductive material is stopped when putting the temperature information of detection less than 10～50 DEG C of polymeric reaction temperature；When temperature detection fills
When putting the temperature value of detection more than polymeric reaction temperature scope, then in polymerization reaction kettle, it is passed through cooling solvent, controls polymerization anti-
Answer the temperature in still in the range of polymeric reaction temperature；
Step 3: polyreaction terminates: when the viscosity number of viscosity detecting device detection reaches target viscosities, anti-to polymerization
Being passed through chloromethanes in answering still, the capping reagent being passed through in described polymerization reaction kettle makes the polysulfone resin of preparation in polyreaction free
Base is replaced, and after organic solvent viscosity is stationary value in reactor to be polymerized, stops being passed through capping reagent, terminates polyreaction and obtains
Containing the mixed solution of polysulfone resin, reduce polyreaction temperature in the kettle.
Step 4: polyreaction post processing, the mixed solution obtained after being polymerized reaction terminating in polymerization reaction kettle passes through
Drainage line is emitted in water, makes the chloromethanes hydrolysis of residual in organic solvent, dissolves polysulfone resin analysis in organic solvent
Going out, described drainage line is provided with switch valve, the outfan of described drainage line connects nozzle；The temperature of described water is 55
℃。
Embodiment six: a kind of polysulfone resin industrialized producing technology, comprises the following steps:
Step one: polyreaction pre-treatment: add the polymerization reactant for preparing polysulfone resin in polymerization reaction kettle
Material, described polyreaction material is the polyreaction material with free radical, opens agitator in polymeric kettle, to polyreaction
Noble gas it is passed through in still, gas-phase space gas in metathesis polymerizable reactor, it is passed through high-temperature heat-conductive to the interlayer of polymerization reaction kettle
Material, makes the polyreaction material in polymerization reaction kettle reach polymeric reaction temperature；
Step 2: polyreaction: continue the interlayer to polymerization reaction kettle and be passed through high-temperature heat-conductive material, filled by viscosity measurements
Put the viscosity in detection polymerization reaction kettle, by the temperature in temperature-detecting device detection polymerization reaction kettle, when temperature detection fills
Conveying high-temperature heat-conductive material is stopped when putting the temperature information of detection less than 10～50 DEG C of polymeric reaction temperature；When temperature detection fills
When putting the temperature value of detection more than polymeric reaction temperature scope, then in polymerization reaction kettle, it is passed through cooling solvent, controls polymerization anti-
Answer the temperature in still in the range of polymeric reaction temperature；
Step 3: polyreaction terminates: when the viscosity number of viscosity detecting device detection reaches target viscosities, anti-to polymerization
Being passed through chloromethanes in answering still, the capping reagent being passed through in described polymerization reaction kettle makes the polysulfone resin of preparation in polyreaction free
Base is replaced, and after organic solvent viscosity is stationary value in reactor to be polymerized, stops being passed through capping reagent, terminates polyreaction and obtains
Mixed solution,；
Step 4: polyreaction post processing, the mixed solution obtained after being polymerized reaction terminating in polymerization reaction kettle passes through
Drainage line is emitted in water, makes the chloromethanes hydrolysis of residual in organic solvent, dissolves polysulfone resin analysis in organic solvent
Going out, described drainage line is provided with switch valve, in described drainage line, mixed solution is delivered to pure by switch valve discontinuity
In water, until polymer resin solution exports completely to pure water.The outfan of described drainage line connects nozzle；Described
The temperature of water is 60 DEG C.
Embodiment seven: a kind of polysulfone resin industrialized producing technology, comprises the following steps:
Step one: polyreaction pre-treatment: add the polymerization reactant for preparing polysulfone resin in polymerization reaction kettle
Material, described polyreaction material is the polyreaction material with free radical, and described polyreaction material is for having freedom
The polyreaction material of base, opens agitator in polymeric kettle, is passed through noble gas, metathesis polymerizable reactor in polymerization reaction kettle
Interior gas-phase space gas, is passed through high-temperature heat-conductive material to the interlayer of polymerization reaction kettle, makes the polymerization reactant in polymerization reaction kettle
Material reaches polymeric reaction temperature；
Step 2: polyreaction: continue the interlayer to polymerization reaction kettle and be passed through high-temperature heat-conductive material, filled by viscosity measurements
Put the viscosity in detection polymerization reaction kettle, by the temperature in temperature-detecting device detection polymerization reaction kettle, when temperature detection fills
Conveying high-temperature heat-conductive material is stopped when putting the temperature information of detection less than 10～50 DEG C of polymeric reaction temperature；When temperature detection fills
When putting the temperature value of detection more than polymeric reaction temperature scope, then in polymerization reaction kettle, it is passed through cooling solvent, controls polymerization anti-
Answer the temperature in still in the range of polymeric reaction temperature；
Step 3: polyreaction terminates: when the viscosity number of viscosity detecting device detection reaches target viscosities, anti-to polymerization
Being passed through chloromethanes in answering still, the capping reagent being passed through in described polymerization reaction kettle makes the polysulfone resin of preparation in polyreaction free
Base is replaced, and after in reactor to be polymerized, organic solvent viscosity is stationary value, stops being passed through capping reagent, in described polymerization reaction kettle
The capping reagent being passed through makes the polysulfone resin free radical displacement of preparation in polyreaction, terminates polyreaction, reduces polyreaction
Temperature in the kettle obtains polysulfone resin through separating out with purification processes；
Step 4: polyreaction post processing, the mixed solution obtained after being polymerized reaction terminating in polymerization reaction kettle passes through
Drainage line is emitted in water, makes the chloromethanes hydrolysis of residual in the organic solvent in mixed solution, dissolves in organic solvent
Polysulfone resin separate out, described drainage line is provided with switch valve, in described drainage line, switch valve discontinuity will mix molten
Liquid is delivered in pure water, a length of 5s when specially switch valve is opened every time, a length of 10s during closedown, opens and closes alternately control
System, until polymer resin solution exports completely to pure water.The outfan of described drainage line connects nozzle；Described water
Temperature be 55～60 DEG C.
Example five and embodiment seven through the polymer resin solution of nozzle discharge, detect the polysulfones tree of discharge respectively
The uniformity of lipoprotein solution and diameter, result is as shown in table 1.
Table 1 embodiment five and the polymer resin solution state-detection of embodiment seven discharge
| Component | Diameter | The uniformity |
| Embodiment five | More than 200mm | Uneven |
| Embodiment seven | Less than 100mm | Uniformly |
From the data in table 1, it can be seen that wherein the diameter of the polysulfone resin solution that embodiment five is discharged is more than 200mm, will obtain
Polysulfone resin solution when carrying out follow-up water-boiling method purification processes, need manual operation manually to export to macerator pump, increase
Add manpower and materials, and manual hand manipulation has too increased the danger of work.And the polysulfone resin solution that embodiment seven is discharged
Diameter less than 100mm, and good evenness, it is possible to automatically export to macerator pump, import the equipment of postprocessing working procedures.
Save trouble and labor, adds production efficiency.
Embodiment eight: a kind of polysulfone resin industrialized producing technology, comprises the following steps:
Step one: polyreaction pre-treatment: add the polymerization reactant for preparing polysulfone resin in polymerization reaction kettle
Material, described polyreaction material is the polyreaction material with free radical, and described polyreaction material includes that bisphenol-A is birdsed of the same feather flock together
Sulfone, described polyreaction material is the polyreaction material with free radical, opens agitator in polymeric kettle, to polyreaction
Noble gas it is passed through in still, gas-phase space gas in metathesis polymerizable reactor, it is passed through high-temperature heat-conductive to the interlayer of polymerization reaction kettle
Material；
Step 2: polyreaction: continue the interlayer to polymerization reaction kettle and be passed through high-temperature heat-conductive material, filled by viscosity measurements
Put the viscosity in detection polymerization reaction kettle, by the temperature in temperature-detecting device detection polymerization reaction kettle, when temperature detection fills
Conveying high-temperature heat-conductive material is stopped when putting the temperature information of detection less than 10 DEG C of polymeric reaction temperature；In keeping polymerization reaction kettle
Temperature be 150～165 DEG C, when the temperature value of temperature-detecting device detection is more than 165 DEG C, be then passed through cold in polymerization reaction kettle
But solvent, controls the temperature in polymerization reaction kettle in the range of polymeric reaction temperature；
Step 3: polyreaction terminates: when the viscosity number of viscosity detecting device detection reaches target viscosities, anti-to polymerization
Being passed through chloromethanes in answering still, the capping reagent being passed through in described polymerization reaction kettle makes the polysulfone resin of preparation in polyreaction free
Base is replaced, and after in reactor to be polymerized, organic solvent viscosity is stationary value, stops being passed through capping reagent, in described polymerization reaction kettle
The capping reagent being passed through makes the polysulfone resin free radical displacement of preparation in polyreaction, terminates polyreaction, obtains mixed solution,
Maintaining current state to 20min, be passed through cooling conduction oil to the interlayer of polymerization reaction kettle, reducing polyreaction temperature in the kettle is 60
～70 DEG C obtain polysulfone resin solution；
Step 4: polyreaction post processing, the mixed solution obtained after being polymerized reaction terminating in polymerization reaction kettle passes through
Drainage line is emitted in water, makes the chloromethanes hydrolysis of residual in organic solvent, dissolves polysulfone resin analysis in organic solvent
Going out, described drainage line is provided with switch valve, in described drainage line, mixed solution is delivered to pure by switch valve discontinuity
In water；A length of 5s when switch valve is opened every time, a length of 10s during closedown, open and close and alternately control, until fluoropolymer resin is molten
Liquid exports completely to pure water.The outfan of described drainage line connects nozzle；The temperature of described water is 58 DEG C；
Step 5: purification processes: the polysulfone resin using water-boiling method to separate out step 4 purifies；
Step 6: extrusion: hot-extrudable technique extrusion obtains polysulfones bar, and the temperature of hot-extrudable technique is 175 DEG C.
Embodiment nine: a kind of polysulfone resin industrialized producing technology, comprises the following steps:
Step one: polyreaction pre-treatment: add the polymerization reactant for preparing polysulfone resin in polymerization reaction kettle
Material, described polyreaction material is the polyreaction material with free radical, and described polyreaction material includes that bisphenol-A is birdsed of the same feather flock together
Sulfone, opens agitator in polymeric kettle, is passed through noble gas, gas-phase space gas in metathesis polymerizable reactor in polymerization reaction kettle
Body, is passed through high-temperature heat-conductive material to the interlayer of polymerization reaction kettle；
Step 2: polyreaction: continue the interlayer to polymerization reaction kettle and be passed through high-temperature heat-conductive material, filled by viscosity measurements
Put the viscosity in detection polymerization reaction kettle, by the temperature in temperature-detecting device detection polymerization reaction kettle, by regulation high temperature
Temperature in the flow-control polymerization reaction kettle of Heat Conduction Material, when the temperature information of temperature-detecting device detection is less than polyreaction
Conveying high-temperature heat-conductive material is stopped during 50 DEG C of temperature；It is exothermic reaction owing to preparing the polyreaction of polysulfone resin, then stops
After conveying high-temperature heat-conductive material, keeping the temperature in polymerization reaction kettle is 150～165 DEG C, when the temperature of temperature-detecting device detection
Angle value is more than 165 DEG C, then be passed through cooling solvent in polymerization reaction kettle, controls the temperature in polymerization reaction kettle in polyreaction temperature
In the range of degree；
Described polymerization reaction kettle top connects polymerization tower, and described polymerization tower top connects condenser, described condenser
Outfan connect have gas-liquid separator, described gas-liquid separator to be connected to chilling flux bath and output device, work as polymerization
Reaction started to the time period that polymeric reaction product is completely exhausted out, and continued the valve between open cold condenser and polymerization tower, controlled
The temperature of condenser inner condensat liquid is less than 63 DEG C, makes the solvent of evaporation and the condensed device of gas of evaporation input to gas-liquid separation
In tower, the liquid flux of separation is passed through chilling flux bath by described gas-liquid separation tower, and the gas of separation is passed through output dress
Put and discharge；When the temperature value of temperature-detecting device detection is more than 165 DEG C, then chilling flux bath is passed through cooling in reactor
Solvent, controls the temperature in polymerization reaction kettle in the range of polymeric reaction temperature, due to chilling flux bath, for aggregated tower, cold
But the organic solvent of institute's evaporated in the polyreaction that device and gas-liquid separator are recovered to, the most described cooling solvent be polymerized
In reactor, organic solvent is identical；
Step 3: polyreaction terminates: when the viscosity number of viscosity detecting device detection reaches target viscosities, anti-to polymerization
It is passed through chloromethanes in answering still, makes polymeric hydrocarbon free radical replace, after organic solvent viscosity is stationary value in reactor to be polymerized, stop
It is passed through capping reagent, terminates polyreaction, maintain current state to 40min, after terminating polyreaction, obtain mixed solution, stop
It is passed through noble gas, and opens the valve between chilling flux bath and polymerization reaction kettle, cooling solvent discharge is entered polyreaction
In still, reduction polyreaction temperature in the kettle is 60～70 DEG C and obtains polysulfone resin solution.
Step 4: polyreaction post processing, the mixed solution obtained after being polymerized reaction terminating in polymerization reaction kettle passes through
Drainage line is emitted in water, makes the chloromethanes hydrolysis of residual in organic solvent, dissolves polysulfone resin analysis in organic solvent
Go out；Valve between open cold condenser and polymerization tower, the temperature controlling condenser inner condensat liquid is less than 63 DEG C, makes the solvent of evaporation
Inputting to gas-liquid separation tower with the condensed device of gas of evaporation, the liquid flux of separation is passed through urgency by described gas-liquid separation tower
Cold solvent groove, and the gas of separation is passed through output device discharges, described chilling flux bath and polymerization reaction kettle are by opening
Pass valve connects；
Being provided with switch valve in described drainage line, in described drainage line, mixed solution is delivered to by switch valve discontinuity
In pure water；A length of 5s when switch valve is opened every time, a length of 10s during closedown, open and close and alternately control, until polymer tree
Lipoprotein solution exports completely to pure water.The outfan of described drainage line connects nozzle；The temperature of described water is 58 DEG C；
Step 5: purification processes: the polysulfone resin using water-boiling method to separate out step 4 purifies；
Step 6: extrusion: hot-extrudable technique extrusion obtains polysulfones bar, and the temperature of hot-extrudable technique is 170 DEG C.
Polysulfone resin industrialized producing technology described in above-described embodiment one to embodiment nine can be applicable to all polysulfones
The preparation of family macromolecule material produces, and polyreaction material can select the most accordingly, production of the present invention
Technique is the most applicable.
For a kind of polysulfone resin industrialized producing technology described in embodiment nine, use polysulfone resin as shown in Figure 1
Industrialized production equipment, including the polymerization reaction kettle 1 being sequentially connected with, polymerization tower 2, condenser 3 and output device, described polymerization is anti-
Answering still to include chuck 11 and cylinder 12, be formed with interlayer between described chuck and cylinder, described interlayer is connected by switch valve to be had
Heat Conduction Material conveyer device 4, described cylinder body bottom connects nozzle 5.Bottom and the top of described interlayer are respectively connected with heat conduction material
Material conveying device.Viscosity detecting device and temperature-detecting device it is provided with in described polymerization reaction kettle.Described polymerization reaction kettle
Top is connected by valve capping reagent tank 6.Described capping reagent tank is methyl chloride gas tank.Described output device includes depending on
The gas-liquid separator 7 of secondary connection and glass regard bucket 8, and the fluid output port of described gas/liquid separator device is connected with cylinder.Described
The fluid output port of gas-liquid separator by switch valve connect have chilling flux bath 9, described chilling flux bath by switch valve with
Cylinder connects.Described polymerization reaction kettle bottom is communicated with pond 101 by nozzle.It is connected between described cylinder and nozzle and has discharge
Pipeline, described drainage line is provided with switch valve.Described polymerization reaction kettle top is connected by valve solvent tank 102, institute
The driving means connection stating the switch valve in drainage line has intervalometer, by the switch in described Timer Controlling drainage line
Valve opens fixing duration and cuts out fixing duration.This device is suitable for the preparation of all polysulfones macromolecular materials and produces.
Embodiment ten: a kind of polysulfone resin industrialized producing technology, comprises the following steps:
A kind of polysulfone resin industrialized producing technology, comprises the following steps:
Step one: polyreaction pre-treatment: use 500L chuck glassed steel reaction vessels is as polymerization reaction kettle, by metering
Tank quantitatively adds the organic solvent N,N-dimethylacetamide of 400L in polymerization reaction kettle；Low rate start anchor formula stirring paddle, turns
Speed is 2r/min；Manual weighing, adds 70kg44 dichloro diphenyl sulfone, 160kg bisphenol-A, 110kg carbonic acid in polymerization reaction kettle
Potassium, then closes batching hole.In still, it is passed through low-pressure nitrogen, continues 5min.In making polymerization reaction kettle, oxygen all displaces.Throw
Material process is complete.Temperature controls to start to enable, temperature control settings point 63 DEG C, range of accommodation 61～64 DEG C；
Step 2: polyreaction: step up the rotating speed of anchor formula stirring paddle to 45r/min, settle out, monitors that polymerization is anti-
Answer the temperature curve value in still, stirring paddle motor inverter torque value and power current flow valuve；200 DEG C of heat conduction it are passed through in interlayer
Oil, slowly promotes polymerization reaction kettle temperature, and temperature promotes unsuitable too fast, it is to avoid burst porcelain；When polyreaction temperature in the kettle rises to
When about 120 DEG C, stirring paddle motor inverter torque value and power current flow valuve in polymerization reaction kettle start gradually to promote, mark
Polyreaction has begun to.Reaction generates polysulfones, potassium chloride, water, CO2, a small amount of N,N-dimethylacetamide is decomposed into CO2With
NH3.Wherein gaseous component CO2、NH3, evaporation N,N-dimethylacetamide, the water of evaporation and protection gas nitrogen pass through polymerization tower
Once enter condenser after condensation.Owing to controlling condenser temperature, temperature control settings point 63 DEG C, range of accommodation 61～64 DEG C,
By after gas-liquid separator separates gas phase after water and N,N-dimethylacetamide condensation, collect chilling flux bath gives over to follow-up
Use；Residue gas phase CO2、NH3It is delivered to output device with nitrogen；
Keeping high-temperature hot oil to continue conveying, polyreaction is slow exothermic polymerization reaction, when temperature rises to 135 DEG C,
Stop sending into high-temperature hot oil；Along with proceeding of reaction, temperature slowly promotes；Optimal reaction temperature is 160 DEG C.When polymerization is anti-
When answering temperature in the kettle more than 160 DEG C, suitably open the switch valve between chilling flux bath and polymerization reaction kettle, make polymerization reaction kettle
Interior temperature maintains 160 ± 1 DEG C；Maintain polyreaction；Because the boiling point of N,N-dimethylacetamide 165 DEG C, below boiling point
Reaction temperature can effectively reduce evaporation, reduces energy consumption；
Step 3: polyreaction terminates: due to the most corresponding different viscosity of the polysulfones of different polymerization degree, its
Real time viscosity value can be with the converter torque value of anchor formula stirring paddle and the indirect nominal of power current flow valuve.Change when anchor formula stirring paddle
Frequently device torque value and power current flow valuve reach desired value, and mark extent of polymerization meets requirement, starts to terminate reaction；
Chloromethanes is delivered to below polymerization reaction kettle liquid level, the converter torque value of anchor formula stirring paddle and power current flow valuve
Trend eases up, and starts constant after 5min, closes the valve between chloromethanes and polymerization reaction kettle；Terminate reaction to complete；Anchor afterwards
The converter torque value of formula stirring paddle and power current flow valuve continue the most in time and change；
Because chloromethanes is colourless flammable toxic gas, belong to organohalogen compounds.It is slightly soluble in water, is soluble in ether, benzene etc..
There is combustibility, explosive mixture, explosion limit 8.1%～17.2% (volume) can be formed with air；Chloromethanes 60 DEG C with
Methanol is generated during upper hydrolysis.After terminating reaction, chloromethanes is that excess is added, and the chloromethanes of excess is in the environment of 160 DEG C
Evaporation, meets water, hydrolysis in the condenser E101 of 63 DEG C, generates hydrochloric acid and methanol, and methanol discharge vaporization to glass regards in bucket, molten
Yu Shui；Remaining liq (comprising trace hydrochloric acid) is collected in chilling flux bath；Stop being passed through nitrogen, open chilling flux bath with poly-
Closing the valve between reactor, enter in polymerization reaction kettle by cooling solvent discharge, the hydrochloric acid in polymerization reaction kettle is with excess carbonic acid
Nak response, generates potassium chloride and CO2；
Step 4: polyreaction post processing: cooling polymerization reaction kettle, to 63 DEG C, in cycle time switch drainage line
Valve (5s opens, and 10s closes), to polymerization reaction kettle, material is all released in pure water (58 DEG C), is dissolved in N, N-dimethyl second
Polysulfone resin in amide starts to separate out fluffy solid resin；Dissolving chloromethanes in a solvent is continued in water if had simultaneously
Being hydrolyzed into methanol and hydrochloric acid, hydrochloric acid generates potassium chloride and CO with potassium carbonate reaction2；63 DEG C of temperature of gas phase and liquid phase section set,
The chloromethanes that can make micro-excess is fully hydrolyzed, and reduces danger；
Step 5: purify: the polysulfone resin using water-boiling method to separate out step 4 carries out purification processes.
Step 6: extrusion: in 174 DEG C by hot-extrudable for polysulfone resin bar.
Whole reaction produces about 120kg polysulfone resin.According to the difference of the degree of polymerization, the different trades mark, quality can be distinguished
Constant.When 174 degrees Celsius of hot-extrudable bars of polysulfone resin, the visual clarity of the polysulfones bar adding capping reagent is more preferable,
Analyze reason, add polysulfone resin prepared by capping reagent, cross dimeric molecule less, be suitable for injection and hot melting temperature is stable；Do not add
Adding the polysulfones of capping reagent under same extrusion temperature, the visual clarity of polysulfones bar is not so good as the former, suitably squeezes when promoting
After going out temperature, transparency improves, and analyzes reason, and part high polymer does not melt, and affects transparency during extrusion, and high polymer was
Dimeric molecule.
As a example by the polyreaction material selected by embodiment ten, it is respectively adopted gathering described in embodiment one to embodiment nine
Sulphone resin industrialized producing technology, prepares the polysulfone resin of corresponding polysulfone resin and embodiment ten preparation as test group one He
Test group ten, the polysulfone resin performance of detection embodiment one to embodiment ten preparation, at the bar choosing same polyreaction material
Under part, preparing the purity of polysulfone resin, selection application publication number is the patent of invention of CN 104629055 A simultaneously, disclosed
Polysulfone resin prepared by industrialized production polysulfones macromolecular material method as a control group, carries out performance test experience.Detection
Method and detection are shown in Table 2.
Test group and matched group polysulfone resin performance test experience:
Table 2 polysulfone resin performance test experience
Detecting through method and the feature of data shown in table 2, obtaining most preferred embodiment is the life described in embodiment ten
Production. art, the technical program, wherein embodiment nine is consistent method with embodiment ten, by embodiment one in embodiment nine phase
Contrast, the embodiment of the present invention nine is most preferred embodiment, and the polysulfone resin physical and chemical parameter that it is prepared is optimal, and with right in preparation
Compare according to group, in hgher efficiency.Embodiment one to embodiment nine use the polyreaction material described in embodiment ten prepare simultaneously
Polysulfone resin and embodiment ten prepared by polysulfone resin, compare its performance of matched group more excellent.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, that is made any repaiies
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (10)
1. a polysulfone resin industrialized producing technology, it is characterised in that comprise the following steps:
Step one: polyreaction pre-treatment: add the polyreaction material for preparing polysulfone resin in polymerization reaction kettle, open
Open agitator in polymeric kettle, in polymerization reaction kettle, be passed through noble gas, in metathesis polymerizable reactor after gas-phase space gas, to
The interlayer of polymerization reaction kettle is passed through high-temperature heat-conductive material, makes the polyreaction material in polymerization reaction kettle reach polyreaction temperature
Degree；
Step 2: polyreaction: continue the interlayer to polymerization reaction kettle and be passed through high-temperature heat-conductive material, examined by viscosity detecting device
Survey the viscosity in polymerization reaction kettle, by the temperature in temperature-detecting device detection polymerization reaction kettle, when temperature-detecting device is examined
The temperature information surveyed stops conveying high-temperature heat-conductive material when being less than 10～50 DEG C of polymeric reaction temperature；When temperature-detecting device is examined
When the temperature value surveyed is more than polymeric reaction temperature scope, then in polymerization reaction kettle, it is passed through cooling solvent, controls polymerization reaction kettle
Interior temperature is in the range of polymeric reaction temperature；
Step 3: polyreaction terminates: when the viscosity number of viscosity detecting device detection reaches target viscosities, terminate polymerization anti-
Should, reduce polyreaction temperature in the kettle and obtain polysulfone resin through separating out with purification processes.
Polysulfone resin industrialized producing technology the most according to claim 1, it is characterised in that when viscosity detecting device detects
Viscosity number when reaching target viscosities, in polymerization reaction kettle, be passed through capping reagent, organic solvent viscosity in reactor to be polymerized
After stationary value, stop being passed through capping reagent, terminate polyreaction.
Polysulfone resin industrialized producing technology the most according to claim 2, it is characterised in that described polyreaction material
For having the polyreaction material of free radical, the capping reagent being passed through in described polymerization reaction kettle makes for preparing in polyreaction to gather
Sulphone resin free radical is replaced.
Polysulfone resin industrialized producing technology the most according to claim 2, it is characterised in that described capping reagent is chlorine
Methane；Described noble gas is nitrogen or carbon dioxide.
Polysulfone resin industrialized producing technology the most according to claim 1, it is characterised in that described polysulfone resin industrialization
Production technology also includes step 4: polyreaction post processing, the mixing obtained after being polymerized reaction terminating in polymerization reaction kettle is molten
Liquid is emitted in water by drainage line, makes the chloromethanes hydrolysis of residual in organic solvent, dissolves polysulfones in organic solvent
Resin separates out, and described drainage line is provided with switch valve.
Polysulfone resin industrialized producing technology the most according to claim 5, it is characterised in that the output of described drainage line
End connection has nozzle；The temperature of described water is 55～60 DEG C；
Water-boiling method is used to carry out purification processes the polysulfone resin separated out in water；Purified process after heat expressing technique extrusion obtains
Polysulfones bar；The temperature of described hot-extrudable technique is 170～175 DEG C.
Polysulfone resin industrialized producing technology the most according to claim 5, it is characterised in that switch in described drainage line
Mixed solution is delivered in pure water by valve discontinuity；A length of 5s when switch valve is opened every time, a length of 10s during closedown, open and
Close and alternately control.
Polysulfone resin industrialized producing technology the most according to claim 1, it is characterised in that in step 2, by adjusting
Joint is passed through the temperature in the flow-control polymerization reaction kettle of high-temperature heat-conductive material；In described step 3, polymerization reaction kettle is through nature
Being cooled to temperature be 60～70 DEG C and obtain mixed solution, described mixed solution is through separating out and purification processes obtains polysulfone resin.
Polysulfone resin industrialized producing technology the most according to claim 1, it is characterised in that described polymerization reaction kettle top
Connecting and have polymerization tower, described polymerization tower top connects condenser, and the outfan of described condenser connects gas-liquid separator, institute
State gas-liquid separator and be connected to chilling flux bath and output device；
In polyreaction starts the time period being completely exhausted out to polymeric reaction product, continue between open cold condenser and polymerization tower
Valve, the temperature controlling condenser inner condensat liquid is less than 63 DEG C, makes the solvent of evaporation and the gas condensed device input of evaporation
To gas-liquid separation tower, the liquid flux of separation is passed through chilling flux bath, and the gas that will separate by described gas-liquid separation tower
It is passed through output device to discharge；
Described chilling flux bath is connected by switch valve with polymerization reaction kettle, when in polymerization stage, if temperature detection dress
The temperature value putting detection is more than range of reaction temperature, then open the switch valve between chilling flux bath and polymerization reaction kettle, make cold
But in solvent is passed through polymerization reaction kettle；After polyreaction terminates, collect that course of reaction is evaporated and condensed device and gas-liquid
Separator processes the organic solvent obtained.
Polysulfone resin industrialized producing technology the most according to claim 9, it is characterised in that after terminating polyreaction, stop
Stop-pass enters noble gas, and opens the valve between chilling flux bath and polymerization reaction kettle, cooling solvent discharge is entered polymerization anti-
In answering still, then reduce polyreaction temperature in the kettle and obtain polysulfone resin through separating out with purification processes.
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