CN106220853B - A kind of polysulfone resin industrialized producing technology - Google Patents
A kind of polysulfone resin industrialized producing technology Download PDFInfo
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- CN106220853B CN106220853B CN201610818935.XA CN201610818935A CN106220853B CN 106220853 B CN106220853 B CN 106220853B CN 201610818935 A CN201610818935 A CN 201610818935A CN 106220853 B CN106220853 B CN 106220853B
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- 229920002492 poly(sulfone) Polymers 0.000 title claims abstract description 155
- 229920005989 resin Polymers 0.000 title claims abstract description 124
- 239000011347 resin Substances 0.000 title claims abstract description 124
- 238000005516 engineering process Methods 0.000 title claims abstract description 43
- 239000000463 material Substances 0.000 claims abstract description 80
- 238000004519 manufacturing process Methods 0.000 claims abstract description 25
- 238000002203 pretreatment Methods 0.000 claims abstract description 13
- 238000006116 polymerization reaction Methods 0.000 claims description 229
- 238000006243 chemical reaction Methods 0.000 claims description 107
- 238000001514 detection method Methods 0.000 claims description 70
- 238000000034 method Methods 0.000 claims description 51
- 239000002904 solvent Substances 0.000 claims description 42
- 239000003153 chemical reaction reagent Substances 0.000 claims description 41
- 239000003960 organic solvent Substances 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- 229910001868 water Inorganic materials 0.000 claims description 37
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims description 36
- 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 17
- 230000008020 evaporation Effects 0.000 claims description 17
- 150000003254 radicals Chemical class 0.000 claims description 17
- 238000000926 separation method Methods 0.000 claims description 17
- 239000011261 inert gas Substances 0.000 claims description 16
- 238000000746 purification Methods 0.000 claims description 16
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 14
- 238000001192 hot 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
- 238000009835 boiling Methods 0.000 claims description 9
- 230000007062 hydrolysis Effects 0.000 claims description 9
- 238000006460 hydrolysis reaction Methods 0.000 claims description 9
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 6
- 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
- 229930195733 hydrocarbon Natural products 0.000 abstract description 8
- 239000004215 Carbon black (E152) Substances 0.000 abstract description 6
- 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
- 239000000243 solution Substances 0.000 description 18
- 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 11
- 239000000376 reactant Substances 0.000 description 11
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 229920000642 polymer Polymers 0.000 description 8
- 239000012458 free base Substances 0.000 description 7
- 238000004458 analytical method Methods 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
- 238000001125 extrusion Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 239000001103 potassium chloride Substances 0.000 description 5
- 235000011164 potassium chloride Nutrition 0.000 description 5
- 239000006228 supernatant Substances 0.000 description 5
- 230000000007 visual effect Effects 0.000 description 5
- 229940106691 bisphenol a Drugs 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000002952 polymeric resin Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 150000003457 sulfones Chemical class 0.000 description 4
- 229920003002 synthetic resin Polymers 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- -1 hydrocarbon free radical Chemical class 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000007789 sealing Methods 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
- 150000001408 amides Chemical class 0.000 description 2
- 239000002585 base 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
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 210000003746 feather Anatomy 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 244000144992 flock Species 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 238000001746 injection moulding Methods 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
- 239000000843 powder Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000004062 sedimentation Methods 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
- XOMKZKJEJBZBJJ-UHFFFAOYSA-N 1,2-dichloro-3-phenylbenzene Chemical group ClC1=CC=CC(C=2C=CC=CC=2)=C1Cl XOMKZKJEJBZBJJ-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-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
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 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
- 125000000217 alkyl group Chemical group 0.000 description 1
- 229920002892 amber Polymers 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005253 cladding Methods 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
- 238000004880 explosion Methods 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 239000004811 fluoropolymer Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000006872 improvement Effects 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
- 238000012544 monitoring process Methods 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
- 238000011056 performance test Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000008439 repair process 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
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 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, and in particular to a kind of polysulfone resin industrialized producing technology includes the following steps：Step 1：Polymerisation pre-treatment；Step 2：Polymerisation；Step 3：Polymerisation terminates.Polysulfone resin industrialized producing technology provided by the invention solves the problems, such as that polysulfones high molecular material polymeric hydrocarbon molecular weight distribution span is big.The improved industrialized producing technology of the present invention makes the polysulfones high molecular material purity of production high, and molecular weight distribution is concentrated, production efficiency higher, and quality is more stable.
Description
Technical field
The present invention relates to field of polymer material preparing technology, and in particular to a kind of polysulfone resin industrialized producing technology.
Background technology
Polysulfones is to contain alkyl-SO in molecular backbone2The thermoplastic resin of alkyl chain link, polysulfone resin are slightly ambers
The armorphous transparent or semitransparent polymer of color, excellent in mechanical performance, rigidity is big, and wear-resisting, high intensity is kept at high temperature
Excellent mechanical performance is the advantage that it is protruded, and can make precise measure product, may be adapted to make heat-resistant piece, insulating part, subtract
Grind wearing piece, instrument and meter part and medical instrument part.Specifically be mainly used for electric, food and daily necessities, automobile,
The departments such as aviation, medical treatment and general industry make various contactors, connector, insulating part of transformer, silicon-controlled cap, insulation sleeve
Pipe, coil rack, binding post, printed circuit board, axle sleeve, cover, television system part, capacitor film, brushgear housing, alkaline electric power storage
Pond box, electric wire cladding.PSF can also do protection 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.Steam service plate is made instead of glass and stainless steel, coffee vessel,
Cooking apparatus using microwave, milk vessel, milker component, drink and food distributor.There is surgical operation in terms of health and medical instrument
Disk, sprayer, humidifier, dental appliance, flow controller, grooving device and laboratory apparatus, it may also be used for it has a denture made, adhesive strength
Height can also make chemical industry equipment (pump outer cover, 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 field skill
The focus of attention of art personnel.
In currently available technology, for polysulfone resin traditional production process can be divided into salt, concentration, isolation of purified,
The processes such as solvent recovery and granulation, polycondensating process are divided into as one-step method and two-step method.The sodium salt or sylvite of one-step method, that is, bisphenol-A be
Starting material, with DDS in the presence of sulfone class solvent, polycondensation successively synthesizes PSF.Two steps are i.e. by bisphenol-A at two salt, concentration groups
At.Recycled solvent degree in order to further increase improves preparation efficiency, discharge of wastewater is reduced, for above-mentioned production technology
Corresponding improved technology has been done in the prior art, such as the patent of invention that application publication number is 104629055 A of CN, disclose work
Industry metaplasia produces polysulfones high molecular material method, comprises the steps of：(1) after polysulfones macromolecule material solution polymerisation
Low moisture content solvent identical with polymerization solvent is added in polymeric kettle and stirs；(2) stop stirring, static 10~90 points of separation
Clock；(3) supernatant is extracted when unreacted catalyst, the by-product inorganic salts of reaction and mechanical admixture sink to reactor bottom
Into solvent kettle；It with the product in low moisture content solvent extraction settled layer, settles, is extracted in supernatant to solvent kettle with first again
Secondary clear liquid merges；(4) solution of solvent kettle quantified, continuously squeezed into thin film evaporation unit, thin film evaporation of the solution in heating
Device stomach wall forms film and rapid steaming sends out solvent；(5) the condensed device of solvent evaporated enters in solvent output device, recycles
Solvent can be directly used for next time polymerisation in, without processing；(6) polymer after solvent is evaporated in thin film evaporation unit
Stomach wall forms solid, and solid forms powder under the stirring action of wall built-up form；(7) polymer powders are through thin film evaporation unit kettle
Bottom pipeline, which enters comminutor granulation, to be terminated.
But in above-mentioned modified technique and equipment, when polymer material is reacted, due to polysulfones high molecular material polymeric hydrocarbon
Molecular weight distribution span is big, is not directed to reaction system and carries out effective temperature control processing, to improve preparation of industrialization production
It is dangerous；Simultaneously after polymerisation, is dripped after the sedimentation of part solvent bank using addition, extract supernatant, while will be again
Supernatant and both sides supernatant are extracted in sedimentation, and this method step is complicated, and cannot effectively wash out organic solvent, reduces life
Produce efficiency.
It can be seen that insufficient a kind of improved polysulfone resin industrialized production work of offer in the prior art can be based on
Skill can effectively solve above-mentioned technical problem, reduce industrially prepared danger, while make the process for preparing polysulfone resin
More convenient and efficient improves production efficiency, becomes those skilled in the art's technical barrier urgently to be resolved hurrily.
Invention content
In order to solve the above-mentioned technical problem the present invention, provides a kind of polysulfone resin industrialized producing technology so that polysulfones tree
Polymerization rate is effectively controlled in the preparation process of fat, keeps entire polymerization process more controllable, reduces industrialized production
Danger, so that the polysulfone resin molecular weight distribution of preparation is concentrated, production efficiency higher quality is more stable.
In order to reach above-mentioned technique effect, the present invention includes following technical scheme：
A kind of polysulfone resin industrialized producing technology, includes the following steps：
Step 1：Polymerisation pre-treatment：Into polymerization reaction kettle, addition is used to prepare the polymerization reactant of polysulfone resin
Material opens blender in polymeric kettle, is passed through inert gas into polymerization reaction kettle, gas-phase space gas in metathesis polymerizable reaction kettle
Afterwards, it is passed through high-temperature heat-conductive material to the interlayer of polymerization reaction kettle, so that the polymerisation material in polymerization reaction kettle is reached polymerization anti-
Answer temperature；
Step 2：Polymerisation：Continue to be passed through high-temperature heat-conductive material to the interlayer of polymerization reaction kettle, be filled by viscosity measurements
The viscosity in detection polymerization reaction kettle is set, the temperature in polymerization reaction kettle is detected by temperature-detecting device, when temperature detection fills
It sets when the temperature information of detection is less than 10~50 DEG C of polymeric reaction temperature and stops conveying high-temperature heat-conductive material；When temperature detection fills
When setting the temperature value of detection more than polymeric reaction temperature range, then cooling solvent is passed through into polymerization reaction kettle, control polymerization is anti-
Answer the temperature in kettle within the scope of polymeric reaction temperature；
Step 3：Polymerisation terminates：When the viscosity number of viscosity detecting device detection reaches target viscosities, polymerization is terminated
Reaction reduces polymerisation temperature in the kettle and obtains polysulfone resin with purification processes through being precipitated.
Wherein the temperature of high-temperature heat-conductive material depends on the reaction temperature of polymerisation, and generates the physics of product and solvent
Property.Those skilled in the art can directly determine the temperature model of high-temperature heat-conductive material based on the content of present invention and the prior art
Enclose value.The high-temperature heat-conductive material can be conduction oil, in art technology, it is every can be passed through interlayer and play heating make
Heat Conduction Material is within the scope of the invention.Simultaneously because exothermic reaction when preparing the reaction of polysulfone resin, this hair
The method of bright offer rationally controls the time for stopping conveying high-temperature heat-conductive material, is carried out for the temperature in polymerization reaction kettle effective
Control can continue to ensure that the temperature in polymerization reaction kettle is located in the range of reaction temperature when being reacted.
Further, it when the viscosity number of viscosity detecting device detection reaches target viscosities, is passed through into polymerization reaction kettle
Capping reagent makes polymeric hydrocarbon free radical replace, and after organic solvent viscosity is stationary value in reaction kettle to be polymerized, stopping is passed through sealing end
Reagent terminates polymerisation.
The viscosity detecting device can be viscosimeter；Can be in voltage stabilization, the real-time current of agitating paddle
Conversion；Or the real-time output torque conversion of frequency converter.Those skilled in the art can select most suitable as needed
Viscosity detecting device.
The known polymerisation middle and later periods, according to reaction principle, polymerisation is between long chain hydrocarbons and long chain hydrocarbons
Polymerisation, the molecular weight after polymerization are multiplied.Therefore the polymerization in later stage is controlled, it is advantageous to the control of the degree of polymerization.This hair
After bright polysulfones high molecular material reaches targeted degree of polymerization, capping reagent is added, polysulfone resin end free base is replaced, using change
It learns reactive mode and terminates polymerization, effectively control the polymerization of polymerization reaction late stage, keep degree of polymerization reaction more controllable.
Further, the polymerisation material is the polymerisation material with free radical, the polymerization reaction kettle
The capping reagent being inside passed through makes the polysulfone resin free radical prepared in polymerisation replace.Capping reagent can replace polysulfone resin
End free base, to make chemical reaction terminate polymerization.
Further, the capping reagent is chloromethanes；The inert gas is nitrogen or carbon dioxide.The present invention adopts
It uses chloromethanes as capping reagent, effectively polymerisation is made to terminate, since chloromethanes is flammable explosive gas, the present invention is rationally set
Each step is counted, is effectively decomposed and is discharged for chloromethanes, efficiency and safety prepared by polysulfone resin is improved, with existing skill
Art is compared, and is prepared better.
Further, the polysulfone resin industrialized producing technology further includes step 4：Polymerisation post-processes, and will polymerize
The mixed solution obtained after polymerization reaction terminating in reaction kettle is emitted by drainage line in water, is made remaining in organic solvent
Chloromethanes hydrolyzes, and the polysulfone resin dissolved in organic solvent is precipitated, and switch valve is provided in the drainage line.
Further, the output end of the drainage line is connected with nozzle；The temperature of the water is 55~59 DEG C；To in water
The polysulfone resin of precipitation carries out purification processes using water-boiling method；Hot extrusion technique squeezes out to obtain polysulfones bar after purified processing；
The temperature of the hot extrusion technique is 170~175 DEG C.
It is further preferred that the temperature of the hot extrusion technique is 174 DEG C.
In 174 DEG C of polysulfone resin hot extrusion bars, the visual clarity of the polysulfones bar of capping reagent chloromethanes is added
More preferably, add capping reagent chloromethanes polysulfones, cross dimeric molecule it is less, be suitble to injection molding and hot melting temperature stablize；It is not added with sealing end
For the polysulfones of reagent under same extrusion temperature, the visual clarity of polysulfones bar is not so good as the former, when the appropriate extrusion temperature of promotion
Afterwards, transparency improves, and part high polymer do not melt, and when extrusion influences transparency, and high polymer was dimeric molecule.
The drainage line nozzle of polymerization reaction kettle bottom designs, and the polysulfone resin solution of precipitation can be made steady, controllable.
60 DEG C of the hydrolysis temperature of chloromethanes, actively promotes the temperature of water so that the water temperature in pond is located at 58 DEG C or so, can
Chloromethanes to be effectively dissolved in organic solvent is contacted while being hydrolyzed in same water, generates methanol and hydrochloric acid, and hydrochloric acid is same simultaneously
Excessive carbonic acid nak response generates saleratus and potassium chloride, improves safety when polysulfones is precipitated.
Further, mixed solution is delivered in pure water by the drainage line upper switch valve discontinuity；
The method that mixed solution containing polysulfone resin is discharged using discontinuous, during can improving organic solvent emission
Dilution effect, reduce the risk of the generation line clogging in subsequent wash process, the resin in pond be precipitated it is small,
It is even, facilitate water-boiling method to post-process.
Further, each opening time of switch valve is 5s, when closing a length of 10s, open and close and alternately control.
Those skilled in the art can be according to specific industrialized production quantity and equipment situation selection opening time and closing
Duration.
Further, it in step 2, is passed through in the flow control polymerization reaction kettle of high-temperature heat-conductive material by adjusting
Temperature；In the step 3, polymerization reaction kettle obtains mixed solution through being naturally cooling to temperature for 60~70 DEG C, and the mixing is molten
Liquid obtains polysulfone resin through being precipitated with purification processes.
Since polysulfones high molecular material polymerization process is exothermic reaction, control polymeric reaction temperature appropriate can make to gather
Conjunction process is more steady.Simultaneously as the type of polymerisation material, that is, polysulfones is different, temperature control point according to polysulfones most
Good reaction temperature scene adjustment, wherein bisphenol-A class polysulfones control temperature at 150~165 DEG C, then when being reacted, need to keep
Temperature in polymerization reaction kettle is 150~165 DEG C.Should not be excessively high by the temperature in suitable control reaction kettle, it can control poly-
Sulfone is reacted at 160 DEG C or so, so that polymerisation excessively acutely will not be reduced evaporation capacity, is reduced energy consumption.
Further, the polymerisation material includes bisphenol-A class polysulfones.
Further, it is connected with polymerization tower at the top of the polymerization reaction kettle, is connected with condenser at the top of the polymerization tower, institute
The output end for stating condenser is connected with gas-liquid separator, and the gas-liquid separator is connected separately with chilling flux bath and output fills
It sets；
When polymerisation started in the period being completely exhausted out to polymeric reaction product, condenser and polymerization tower are persistently opened
Between valve, control condenser inner condensat liquid temperature be 63 DEG C hereinafter, making the condensed device of gas of the solvent and evaporation of evaporation
It is input in gas-liquid separation tower, the liquid flux of separation is passed through chilling flux bath by the gas-liquid separation tower, and by separation
Gas is passed through output device and is discharged；
The chilling flux bath is connect with polymerization reaction kettle by switch valve, in polymerization stage, if temperature is examined
The temperature value for surveying device detection is more than range of reaction temperature, then opens the switch valve between chilling flux bath and polymerization reaction kettle,
Cooling solvent is set to be passed through in polymerization reaction kettle；After polymerisation, collect reaction process is evaporated and condensed device and
The organic solvent that gas-liquid separator is handled.
When polymerisation carries out, in raw material, intermediate and finished product, the minimum organic solvent N of flash-point, N- dimethyl second
Amide, flash-point value are 66 DEG C.The organic solvent that the setting of condenser can be such that reaction system exports is in 63 DEG C or less (i.e. at it
Below flash-point) in the environment of export, design with this configuration, make full polymerization process be in all process materials flash-points with
Exterior domain reduces its danger.
Further, after terminating polymerisation, stopping is passed through inert gas, and opens chilling flux bath and polymerization reaction kettle
Between valve, cooling solvent discharge is entered in polymerization reaction kettle, then reduces polymerisation temperature in the kettle through being precipitated and purifying
Processing obtains polysulfone resin.
Production technology of the present invention is suitble to the preparation of all polysulfones high molecular materials to produce, and polymerisation material can
Accordingly to be selected as needed, production technology of the present invention is applicable in.
Using above-mentioned technical proposal, including following advantageous effect：A kind of polysulfone resin industrialized production provided by the invention
Technique solves the problems, such as that polysulfones high molecular material polymeric hydrocarbon molecular weight distribution span is big.The improved industrialized production of the present invention
Technique makes the polysulfones high molecular material purity of production high, and molecular weight distribution is concentrated, production efficiency higher, and quality is more stable.
Description of the drawings
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 reaction process 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
It sets；6, capping reagent tank；7, gas-liquid separator；8, glass regards bucket；9, chilling flux bath；101, pond；102, solvent tank.
Specific implementation mode
The present invention is described in further detail below by specific embodiment.
Embodiment one：A kind of polysulfone resin industrialized producing technology, includes the following steps：
Step 1：Polymerisation pre-treatment：Into polymerization reaction kettle, addition is used to prepare the polymerization reactant of polysulfone resin
Material opens blender in polymeric kettle, is passed through inert gas into polymerization reaction kettle, gas-phase space gas in metathesis polymerizable reaction kettle
Body is passed through high-temperature heat-conductive material to the interlayer of polymerization reaction kettle, so that the polymerisation material in polymerization reaction kettle is reached polymerization anti-
Answer temperature.
Step 2：Polymerisation：Continue to be passed through high-temperature heat-conductive material to the interlayer of polymerization reaction kettle, be filled by viscosity measurements
The viscosity in detection polymerization reaction kettle is set, the temperature in polymerization reaction kettle is detected by temperature-detecting device, when temperature detection fills
It sets when the temperature information of detection is less than 10~50 DEG C of polymeric reaction temperature and stops conveying high-temperature heat-conductive material；When temperature detection fills
When setting the temperature value of detection more than polymeric reaction temperature range, then cooling solvent is passed through into polymerization reaction kettle, control polymerization is anti-
Answer the temperature in kettle within the scope of polymeric reaction temperature；
Step 3：Polymerisation terminates：When the viscosity number of viscosity detecting device detection reaches target viscosities, polymerization is terminated
Reaction reduces polymerisation temperature in the kettle and obtains polysulfone resin with purification processes through being precipitated.
Embodiment two：A kind of polysulfone resin industrialized producing technology, includes the following steps：
Step 1：Polymerisation pre-treatment：Into polymerization reaction kettle, addition is used to prepare the polymerization reactant of polysulfone resin
Material, the polymerisation material are the polymerisation material with free radical, blender in polymeric kettle are opened, to polymerisation
It is passed through inert gas in kettle, gas-phase space gas in metathesis polymerizable reaction kettle is passed through high-temperature heat-conductive to the interlayer of polymerization reaction kettle
Material makes the polymerisation material in polymerization reaction kettle reach polymeric reaction temperature；
Step 2：Polymerisation：Continue to be passed through high-temperature heat-conductive material to the interlayer of polymerization reaction kettle, be filled by viscosity measurements
The viscosity in detection polymerization reaction kettle is set, the temperature in polymerization reaction kettle is detected by temperature-detecting device, when temperature detection fills
It sets when the temperature information of detection is less than 10~50 DEG C of polymeric reaction temperature and stops conveying high-temperature heat-conductive material；When temperature detection fills
When setting the temperature value of detection more than polymeric reaction temperature range, then cooling solvent is passed through into polymerization reaction kettle, control polymerization is anti-
Answer the temperature in kettle within the scope of polymeric reaction temperature；
Step 3：Polymerisation terminates：It is anti-to polymerization when the viscosity number of viscosity detecting device detection reaches target viscosities
It answers and is passed through capping reagent in kettle, the capping reagent being passed through in the polymerization reaction kettle makes the polysulfone resin prepared in polymerisation certainly
It is replaced by base, after organic solvent viscosity is stationary value in reaction kettle to be polymerized, stopping is passed through capping reagent, terminates polymerisation,
It reduces polymerisation temperature in the kettle and obtains polysulfone resin with purification processes through being precipitated.
Embodiment three：A kind of polysulfone resin industrialized producing technology, includes the following steps：
Step 1：Polymerisation pre-treatment：Into polymerization reaction kettle, addition is used to prepare the polymerization reactant of polysulfone resin
Material, the polymerisation material are the polymerisation material with free radical comprising bisphenol-A class polysulfones opens polymeric kettle
Interior blender, is passed through inert gas into polymerization reaction kettle, gas-phase space gas in metathesis polymerizable reaction kettle, to polymerization reaction kettle
Interlayer be passed through high-temperature heat-conductive material, so that the polymerisation material in polymerization reaction kettle is reached polymeric reaction temperature；The inertia
Gas is nitrogen or carbon dioxide.
Step 2：Polymerisation：Continue to be passed through high-temperature heat-conductive material to the interlayer of polymerization reaction kettle, be filled by viscosity measurements
The viscosity in detection polymerization reaction kettle is set, the temperature in polymerization reaction kettle is detected by temperature-detecting device, when temperature detection fills
It sets when the temperature information of detection is less than 10~50 DEG C of polymeric reaction temperature and stops conveying high-temperature heat-conductive material；When temperature detection fills
When setting the temperature value of detection more than polymeric reaction temperature range, then cooling solvent is passed through into polymerization reaction kettle, control polymerization is anti-
Answer the temperature in kettle within the scope of polymeric reaction temperature；
Step 3：Polymerisation terminates：It is anti-to polymerization when the viscosity number of viscosity detecting device detection reaches target viscosities
It answers and is passed through chloromethanes in kettle, polymeric hydrocarbon free radical is made to replace, after organic solvent viscosity is stationary value in reaction kettle to be polymerized, stop
It is passed through capping reagent, the capping reagent being passed through in the polymerization reaction kettle makes the polysulfone resin free radical prepared in polymerisation set
It changes, terminates polymerisation, reduce polymerisation temperature in the kettle and obtain polysulfone resin with purification processes through being precipitated.
When preparing polysulfone resin, the viscosity measurements occurred in polymerisation are as shown in Figure 2 for embodiment one and embodiment three.
Curve A be embodiment one when preparing polysulfone resin, occur polymerisation in viscosity measurements curve, curve B be embodiment three
When preparing polysulfone resin, the viscosity measurements curve in polymerisation occurs.
Polysulfones is a kind of thermoplastic resin, and when dissolving in organic solvent, the viscosity of organic solution is promoted with the degree of polymerization
And it is linearly increasing.Therefore its degree of polymerization of the viscosity indirect reaction of organic solution can be used.The viscosity of organic solution can be by viscous
Meter, the load current value of stirring slurry, agitating paddle frequency converter output torque value are spent directly or indirectly to reflect.It uses in the detection
Qualitative reference of the agitating paddle load current value as the degree of polymerization (viscosity).
In fig. 2, each alphabetical meaning is as follows：
T1：It is warming up to and polymeric reaction temperature time point takes place；
T2：Polymerisation reaches target and needs end time point；
T3：Chloromethanes is added, all blocks time point；
T4：It is cooled to and stops polymeric reaction temperature time point；
L1：It is warming up to and polymeric reaction temperature current value takes place；
L2：Current value at the end of polymerisation needs；
L3：It is passed through chloromethanes sealing end and completes current value；
L4：It is cooled to and stops polymeric reaction temperature current value.
As shown in Figure 2, before T2 time points (being initially added into chloromethanes time point), two curves are respectively represented and are passed through
Two curves are consistent, but after reaching target viscosities, though start it is extraneous intervene cooling, polymerisation still continue into
Row, until when being less than polymerisation initiation temperature.Visual data reflection is exactly that the load current value of its agitating paddle persistently increases
When being added to temperature and being reduced to polymerisation initiation temperature, electric current starts to stablize constant.
After reaching target viscosities, chloromethanes reagent is added, after continuing 3~5 minutes, agitating paddle load current value will not
Increase increase with time again.Analysis is the reason is that in 3~5 minutes, and end capping reaction has occurred in polysulfone resin, and free radical is set to
It changes, polymerisation passes through chemical means force termination.
As shown in Figure 2, for embodiment one in the experiment without using terminal reagent, terminating reaction is carried out by cooling down,
Since temperature-fall period is sustained release process, polymerisation persistently carries out within considerable time, and the polysulfone resin finally obtained is poly-
It is right to will be greater than targeted degree of polymerization, or rule of thumb, termination converging operation is carried out in advance, it is limited by the influence of operating experience factor
Greatly, degree of polymerization control is more extensive.When embodiment three uses chloromethanes as end-capping reagent, reaction will be terminated rapidly, the degree of polymerization
Control is more accurate.
Example IV：A kind of polysulfone resin industrialized producing technology, includes the following steps：
Step 1：Polymerisation pre-treatment：Into polymerization reaction kettle, addition is used to prepare the polymerization reactant of polysulfone resin
Material, the polymerisation material are the polymerisation material with free radical, blender in polymeric kettle are opened, to polymerisation
It is passed through inert gas in kettle, gas-phase space gas in metathesis polymerizable reaction kettle is passed through high-temperature heat-conductive to the interlayer of polymerization reaction kettle
Material makes the polymerisation material in polymerization reaction kettle reach polymeric reaction temperature；
Step 2：Polymerisation：Continue to be passed through high-temperature heat-conductive material to the interlayer of polymerization reaction kettle, be filled by viscosity measurements
The viscosity in detection polymerization reaction kettle is set, the temperature in polymerization reaction kettle is detected by temperature-detecting device, when temperature detection fills
It sets when the temperature information of detection is less than 10~50 DEG C of polymeric reaction temperature and stops conveying high-temperature heat-conductive material；When temperature detection fills
When setting the temperature value of detection more than polymeric reaction temperature range, then cooling solvent is passed through into polymerization reaction kettle, control polymerization is anti-
Answer the temperature in kettle within the scope of polymeric reaction temperature；
Step 3：Polymerisation terminates：It is anti-to polymerization when the viscosity number of viscosity detecting device detection reaches target viscosities
It answers and is passed through chloromethanes in kettle, the capping reagent being passed through in the polymerization reaction kettle keeps the polysulfone resin prepared in polymerisation free
Base is replaced, and after organic solvent viscosity is stationary value in reaction kettle to be polymerized, stopping is passed through capping reagent, terminates polymerisation, obtains
To mixed solution, polymerisation temperature in the kettle is reduced；
Step 4：Polymerisation post-processes, and the mixed solution obtained after reaction terminating will be polymerize in polymerization reaction kettle and is passed through
Drainage line is emitted into water, is made remaining chloromethanes hydrolysis in organic solvent, is dissolved polysulfone resin analysis in organic solvent
Go out, switch valve is provided in the drainage line.
Embodiment five：A kind of polysulfone resin industrialized producing technology, includes the following steps：
Step 1：Polymerisation pre-treatment：Into polymerization reaction kettle, addition is used to prepare the polymerization reactant of polysulfone resin
Material, the polymerisation material are the polymerisation material with free radical, blender in polymeric kettle are opened, to polymerisation
It is passed through inert gas in kettle, gas-phase space gas in metathesis polymerizable reaction kettle is passed through high-temperature heat-conductive to the interlayer of polymerization reaction kettle
Material makes the polymerisation material in polymerization reaction kettle reach polymeric reaction temperature；
Step 2：Polymerisation：Continue to be passed through high-temperature heat-conductive material to the interlayer of polymerization reaction kettle, be filled by viscosity measurements
The viscosity in detection polymerization reaction kettle is set, the temperature in polymerization reaction kettle is detected by temperature-detecting device, when temperature detection fills
It sets when the temperature information of detection is less than 10~50 DEG C of polymeric reaction temperature and stops conveying high-temperature heat-conductive material；When temperature detection fills
When setting the temperature value of detection more than polymeric reaction temperature range, then cooling solvent is passed through into polymerization reaction kettle, control polymerization is anti-
Answer the temperature in kettle within the scope of polymeric reaction temperature；
Step 3：Polymerisation terminates：It is anti-to polymerization when the viscosity number of viscosity detecting device detection reaches target viscosities
It answers and is passed through chloromethanes in kettle, the capping reagent being passed through in the polymerization reaction kettle keeps the polysulfone resin prepared in polymerisation free
Base is replaced, and after organic solvent viscosity is stationary value in reaction kettle to be polymerized, stopping is passed through capping reagent, is terminated polymerisation and is obtained
Mixed solution containing polysulfone resin reduces polymerisation temperature in the kettle.
Step 4：Polymerisation post-processes, and the mixed solution obtained after reaction terminating will be polymerize in polymerization reaction kettle and is passed through
Drainage line is emitted into water, is made remaining chloromethanes hydrolysis in organic solvent, is dissolved polysulfone resin analysis in organic solvent
Go out, switch valve is provided in the drainage line, the output end of the drainage line is connected with nozzle；The temperature of the water is 55
℃。
Embodiment six：A kind of polysulfone resin industrialized producing technology, includes the following steps：
Step 1：Polymerisation pre-treatment：Into polymerization reaction kettle, addition is used to prepare the polymerization reactant of polysulfone resin
Material, the polymerisation material are the polymerisation material with free radical, blender in polymeric kettle are opened, to polymerisation
It is passed through inert gas in kettle, gas-phase space gas in metathesis polymerizable reaction kettle is passed through high-temperature heat-conductive to the interlayer of polymerization reaction kettle
Material makes the polymerisation material in polymerization reaction kettle reach polymeric reaction temperature；
Step 2：Polymerisation：Continue to be passed through high-temperature heat-conductive material to the interlayer of polymerization reaction kettle, be filled by viscosity measurements
The viscosity in detection polymerization reaction kettle is set, the temperature in polymerization reaction kettle is detected by temperature-detecting device, when temperature detection fills
It sets when the temperature information of detection is less than 10~50 DEG C of polymeric reaction temperature and stops conveying high-temperature heat-conductive material；When temperature detection fills
When setting the temperature value of detection more than polymeric reaction temperature range, then cooling solvent is passed through into polymerization reaction kettle, control polymerization is anti-
Answer the temperature in kettle within the scope of polymeric reaction temperature；
Step 3：Polymerisation terminates：It is anti-to polymerization when the viscosity number of viscosity detecting device detection reaches target viscosities
It answers and is passed through chloromethanes in kettle, the capping reagent being passed through in the polymerization reaction kettle keeps the polysulfone resin prepared in polymerisation free
Base is replaced, and after organic solvent viscosity is stationary value in reaction kettle to be polymerized, stopping is passed through capping reagent, is terminated polymerisation and is obtained
Mixed solution,；
Step 4：Polymerisation post-processes, and the mixed solution obtained after reaction terminating will be polymerize in polymerization reaction kettle and is passed through
Drainage line is emitted into water, is made remaining chloromethanes hydrolysis in organic solvent, is dissolved polysulfone resin analysis in organic solvent
Go out, switch valve is provided in the drainage line, mixed solution is delivered to pure by the drainage line upper switch valve discontinuity
In water, until in polymer resin solution output to pure water completely.The output end of the drainage line is connected with nozzle；It is described
The temperature of water is 60 DEG C.
Embodiment seven：A kind of polysulfone resin industrialized producing technology, includes the following steps：
Step 1：Polymerisation pre-treatment：Into polymerization reaction kettle, addition is used to prepare the polymerization reactant of polysulfone resin
Material, the polymerisation material are the polymerisation material with free radical, and the polymerisation material is with freedom
The polymerisation material of base opens blender in polymeric kettle, inert gas, metathesis polymerizable reaction kettle is passed through into 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：Polymerisation：Continue to be passed through high-temperature heat-conductive material to the interlayer of polymerization reaction kettle, be filled by viscosity measurements
The viscosity in detection polymerization reaction kettle is set, the temperature in polymerization reaction kettle is detected by temperature-detecting device, when temperature detection fills
It sets when the temperature information of detection is less than 10~50 DEG C of polymeric reaction temperature and stops conveying high-temperature heat-conductive material；When temperature detection fills
When setting the temperature value of detection more than polymeric reaction temperature range, then cooling solvent is passed through into polymerization reaction kettle, control polymerization is anti-
Answer the temperature in kettle within the scope of polymeric reaction temperature；
Step 3：Polymerisation terminates：It is anti-to polymerization when the viscosity number of viscosity detecting device detection reaches target viscosities
It answers and is passed through chloromethanes in kettle, the capping reagent being passed through in the polymerization reaction kettle keeps the polysulfone resin prepared in polymerisation free
Base is replaced, and after organic solvent viscosity is stationary value in reaction kettle to be polymerized, stopping is passed through capping reagent, in the polymerization reaction kettle
The capping reagent being passed through makes the polysulfone resin free radical prepared in polymerisation replace, and terminates polymerisation, reduces polymerisation
Temperature in the kettle obtains polysulfone resin through being precipitated with purification processes；
Step 4：Polymerisation post-processes, and the mixed solution obtained after reaction terminating will be polymerize in polymerization reaction kettle and is passed through
Drainage line is emitted into water, makes remaining chloromethanes hydrolysis in the organic solvent in mixed solution, dissolving is in organic solvent
Polysulfone resin be precipitated, be provided with switch valve in the drainage line, the drainage line upper switch valve discontinuity will mix molten
Liquid is delivered in pure water, and the specially each opening time of switch valve is 5s, when closing a length of 10s, open and close and alternately control
System, until in polymer resin solution output to pure water completely.The output end of the drainage line is connected with nozzle；The water
Temperature be 55~60 DEG C.
Example five and embodiment seven the polymer resin solution through nozzle discharge, detect the polysulfones tree of discharge respectively
The uniformity and diameter of lipoprotein solution, the results are shown in Table 1.
The polymer resin solution state-detection that 1 embodiment five of table and embodiment seven are discharged
| Component | Diameter | The uniformity |
| Embodiment five | More than 200mm | It is uneven |
| Embodiment seven | Less than 100mm | Uniformly |
From the data in table 1, it can be seen that the diameter for the polysulfone resin solution that wherein 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 to carry out output manually in macerator pump, increase
Manpower and materials are added, and manual hand manipulation also increases the danger of work.And the polysulfone resin solution that embodiment seven is discharged
Diameter be less than 100mm, and good evenness can carry out exporting to macerator pump automatically, import the equipment of postprocessing working procedures.
Save trouble and labor increases production efficiency.
Embodiment eight：A kind of polysulfone resin industrialized producing technology, includes the following steps：
Step 1：Polymerisation pre-treatment：Into polymerization reaction kettle, addition is used to prepare the polymerization reactant of polysulfone resin
Material, the polymerisation material are the polymerisation material with free radical, and the polymerisation material includes that bisphenol-A is birdsed of the same feather flock together
Sulfone, the polymerisation material are the polymerisation material with free radical, blender in polymeric kettle are opened, to polymerisation
It is passed through inert gas in kettle, gas-phase space gas in metathesis polymerizable reaction kettle is passed through high-temperature heat-conductive to the interlayer of polymerization reaction kettle
Material；
Step 2：Polymerisation：Continue to be passed through high-temperature heat-conductive material to the interlayer of polymerization reaction kettle, be filled by viscosity measurements
The viscosity in detection polymerization reaction kettle is set, the temperature in polymerization reaction kettle is detected by temperature-detecting device, when temperature detection fills
It sets when the temperature information of detection is less than 10 DEG C of polymeric reaction temperature and stops conveying high-temperature heat-conductive material；It keeps in polymerization reaction kettle
Temperature be 150~165 DEG C, when temperature-detecting device detection temperature value be more than 165 DEG C, then be passed through into polymerization reaction kettle cold
But solvent controls the temperature in polymerization reaction kettle within the scope of polymeric reaction temperature；
Step 3：Polymerisation terminates：It is anti-to polymerization when the viscosity number of viscosity detecting device detection reaches target viscosities
It answers and is passed through chloromethanes in kettle, the capping reagent being passed through in the polymerization reaction kettle keeps the polysulfone resin prepared in polymerisation free
Base is replaced, and after organic solvent viscosity is stationary value in reaction kettle to be polymerized, stopping is passed through capping reagent, in the polymerization reaction kettle
The capping reagent being passed through makes the polysulfone resin free radical prepared in polymerisation replace, and terminates polymerisation, obtains mixed solution,
It maintains current state to 20min, cooling conduction oil is passed through to the interlayer of polymerization reaction kettle, it is 60 to reduce polymerisation temperature in the kettle
~70 DEG C obtain polysulfone resin solution；
Step 4：Polymerisation post-processes, and the mixed solution obtained after reaction terminating will be polymerize in polymerization reaction kettle and is passed through
Drainage line is emitted into water, is made remaining chloromethanes hydrolysis in organic solvent, is dissolved polysulfone resin analysis in organic solvent
Go out, switch valve is provided in the drainage line, mixed solution is delivered to pure by the drainage line upper switch valve discontinuity
In water；The each opening time of switch valve is 5s, when closing a length of 10s, open and close and alternately control, until fluoropolymer resin is molten
In liquid output to pure water completely.The output end of the drainage line is connected with nozzle；The temperature of the water is 58 DEG C；
Step 5：Purification processes：The polysulfone resin that step 4 is precipitated using water-boiling method is purified；
Step 6：It squeezes out：Hot extrusion technique squeezes out to obtain polysulfones bar, and the temperature of hot extrusion technique is 175 DEG C.
Embodiment nine：A kind of polysulfone resin industrialized producing technology, includes the following steps：
Step 1：Polymerisation pre-treatment：Into polymerization reaction kettle, addition is used to prepare the polymerization reactant of polysulfone resin
Material, the polymerisation material are the polymerisation material with free radical, and the polymerisation material includes that bisphenol-A is birdsed of the same feather flock together
Sulfone opens blender in polymeric kettle, is passed through inert gas into polymerization reaction kettle, gas-phase space gas in metathesis polymerizable reaction kettle
Body is passed through high-temperature heat-conductive material to the interlayer of polymerization reaction kettle；
Step 2：Polymerisation：Continue to be passed through high-temperature heat-conductive material to the interlayer of polymerization reaction kettle, be filled by viscosity measurements
The viscosity in detection polymerization reaction kettle is set, the temperature in polymerization reaction kettle is detected by temperature-detecting device, by adjusting 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 polymerisation
Stop conveying high-temperature heat-conductive material at 50 DEG C of temperature；Polymerisation due to preparing polysulfone resin is exothermic reaction, then stops
After conveying high-temperature heat-conductive material, it is 150~165 DEG C to keep the temperature in polymerization reaction kettle, when the temperature of temperature-detecting device detection
Angle value is more than 165 DEG C, then cooling solvent is passed through into polymerization reaction kettle, controls the temperature in polymerization reaction kettle in polymerisation temperature
It spends in range；
It is connected with polymerization tower at the top of the polymerization reaction kettle, condenser, the condenser are connected at the top of the polymerization tower
Output end be connected with gas-liquid separator, the gas-liquid separator is connected separately with chilling flux bath and output device, works as polymerization
Reaction started in the period being completely exhausted out to polymeric reaction product, persistently opened the valve between condenser and polymerization tower, control
The temperature of condenser inner condensat liquid is 63 DEG C hereinafter, the condensed device of gas of the solvent and evaporation of evaporation is made to be input to gas-liquid separation
In tower, the liquid flux of separation is passed through chilling flux bath by the gas-liquid separation tower, and the gas of separation is passed through output dress
It sets and is discharged；When the temperature value of temperature-detecting device detection is more than 165 DEG C, then chilling flux bath is passed through cooling into reaction kettle
Solvent controls the temperature in polymerization reaction kettle within the scope of polymeric reaction temperature, is aggregated tower, cold due to chilling flux bath
But the organic solvent of institute's evaporated in the polymerisation that device and gas-liquid separator are recovered to, thus the cooling solvent with polymerize
Organic solvent is identical in reaction kettle；
Step 3：Polymerisation terminates：It is anti-to polymerization when the viscosity number of viscosity detecting device detection reaches target viscosities
It answers and is passed through chloromethanes in kettle, polymeric hydrocarbon free radical is made to replace, after organic solvent viscosity is stationary value in reaction kettle to be polymerized, stop
It is passed through capping reagent, terminates polymerisation, maintains current state to 40min, mixed solution is obtained after terminating polymerisation, stop
It is passed through inert gas, and opens the valve between chilling flux bath and polymerization reaction kettle, cooling solvent discharge is entered into polymerisation
In kettle, reduces polymerisation temperature in the kettle and obtain polysulfone resin solution for 60~70 DEG C.
Step 4：Polymerisation post-processes, and the mixed solution obtained after reaction terminating will be polymerize in polymerization reaction kettle and is passed through
Drainage line is emitted into water, is made remaining chloromethanes hydrolysis in organic solvent, is dissolved polysulfone resin analysis in organic solvent
Go out；The valve between condenser and polymerization tower is opened, the temperature for controlling condenser inner condensat liquid is 63 DEG C hereinafter, making the solvent of evaporation
It is input in gas-liquid separation tower with the condensed device of gas of evaporation, the liquid flux of separation is passed through urgency by the gas-liquid separation tower
Cold solvent slot, and the gas of separation is passed through output device and is discharged, the chilling flux bath is with polymerization reaction kettle by opening
Close valve connection；
Switch valve is provided in the drainage line, mixed solution is delivered to by the drainage line upper switch valve discontinuity
In pure water；The each opening time of switch valve is 5s, when closing a length of 10s, open and close and alternately control, until polymer tree
In lipoprotein solution output to pure water completely.The output end of the drainage line is connected with nozzle；The temperature of the water is 58 DEG C；
Step 5：Purification processes：The polysulfone resin that step 4 is precipitated using water-boiling method is purified；
Step 6：It squeezes out：Hot extrusion technique squeezes out to obtain polysulfones bar, and the temperature of hot extrusion technique is 170 DEG C.
Polysulfone resin industrialized producing technology described in above-described embodiment one to embodiment nine can be suitable for all polysulfones
The preparation of family macromolecule material produces, and polymerisation material can be selected accordingly as needed, production of the present invention
Technique is applicable in.
For a kind of polysulfone resin industrialized producing technology described in embodiment nine, using polysulfone resin as shown in Figure 1
Industrialized production equipment, including sequentially connected polymerization reaction kettle 1, polymerization tower 2, condenser 3 and output device, the polymerization are anti-
It includes chuck 11 and cylinder 12 to answer kettle, and interlayer is formed between the chuck and cylinder, and the interlayer is connected with by switch valve
Heat Conduction Material conveying device 4, the cylinder body bottom are connected with nozzle 5.The bottom and top of the interlayer are respectively connected with heat conduction material
Material conveying device.It is provided with viscosity detecting device and temperature-detecting device in the polymerization reaction kettle.The polymerization reaction kettle
Top is connected with capping reagent tank 6 by valve.The capping reagent tank is methyl chloride gas tank.The output device include according to
The gas-liquid separator 7 and glass of secondary connection regard bucket 8, and the fluid output port of the gas/liquid separator device is connect with cylinder.It is described
The fluid output port of gas-liquid separator is connected with chilling flux bath 9 by switch valve, the chilling flux bath by switch valve with
Cylinder connects.The polymerization reaction kettle bottom end is communicated with pond 101 by nozzle.It is connected with discharge between the cylinder and nozzle
Pipeline is provided with switch valve in the drainage line.Solvent tank 102, institute are connected with by valve at the top of the polymerization reaction kettle
The driving device for stating the switch valve in drainage line is connected with timer, passes through the switch in the Timer Controlling drainage line
Valve opens fixed duration and closes fixed duration.The device is suitble to the preparation of all polysulfones high molecular materials to produce.
Embodiment ten：A kind of polysulfone resin industrialized producing technology, includes the following steps：
A kind of polysulfone resin industrialized producing technology, includes the following steps：
Step 1：Polymerisation pre-treatment：Using 500L chucks glassed steel reaction vessels as polymerization reaction kettle, pass through metering
The quantitative organic solvent n,N-dimethylacetamide that 400L is added into polymerization reaction kettle of tank；Low rate start anchor formula agitating paddle turns
Speed is 2r/min；Manual weighing adds 70kg44 dichloro diphenyl sulfones, 160kg bisphenol-As, 110kg carbonic acid into polymerization reaction kettle
Then potassium closes batching hole.It is passed through low-pressure nitrogen into kettle, continues 5min.Oxygen in polymerization reaction kettle is set all to displace.It throws
Material process finishes.Temperature control starts to enable, 63 DEG C of temperature control settings point, 61~64 DEG C of adjustable range；
Step 2：Polymerisation：The rotating speed of anchor formula agitating paddle is stepped up to 45r/min, is settled out, monitoring polymerization is anti-
Answer the temperature curve value in kettle, agitating paddle motor inverter torque value and power electric flow valuve；200 DEG C of heat conduction are passed through into interlayer
Oil slowly promotes polymerization reaction kettle temperature, and temperature is promoted should not be too fast, avoids burst porcelain；When the promotion of polymerisation temperature in the kettle is arrived
At 120 DEG C or so, agitating paddle motor inverter torque value and power electric flow valuve in polymerization reaction kettle start gradually to be promoted, mark
Polymerisation has begun.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
Enter condenser after primary condensation.Due to control condenser temperature, 63 DEG C of temperature control settings point, 61~64 DEG C of adjustable range,
After water and n,N-dimethylacetamide condensation by gas-liquid separator separates gas phase after, be collected into chilling flux bath give over to it is follow-up
It uses；Remaining gas phase CO2、NH3It is delivered to output device with nitrogen；
High-temperature hot oil is kept to continue to convey, polymerisation is slow exothermic polymerization reaction, when temperature is promoted to 135 DEG C,
Stop being sent into high-temperature hot oil；With continuing for reaction, temperature is slowly promoted；Optimal reaction temperature is 160 DEG C.When polymerization is anti-
When temperature in the kettle being answered to be more than 160 DEG C, the appropriate switch valve opened between chilling flux bath and polymerization reaction kettle makes polymerization reaction kettle
Interior temperature maintains 160 ± 1 DEG C；Maintain polymerisation；Because of 165 DEG C of the boiling point of n,N-dimethylacetamide, boiling point is below
Reaction temperature can effectively reduce evaporation, reduce energy consumption；
Step 3：Polymerisation terminates：Since the polysulfones of different polymerization degree corresponds to different viscosity in organic solvent,
Real time viscosity value can use the frequency converter torque value of anchor formula agitating paddle and power electric flow valuve indirectly nominal.When the change of anchor formula agitating paddle
Frequency device torque value and power electric flow valuve reach desired value, and mark extent of polymerization is met the requirements, and starts to terminate reaction；
Chloromethanes is delivered to polymerization reaction kettle liquid level hereinafter, anchor formula agitating paddle frequency converter torque value and power electric flow valuve
Trend eases up, and starts constant, the valve between closing chloromethanes and polymerization reaction kettle after 5min；Reaction is terminated to complete；Anchor later
The frequency converter torque value and power electric flow valuve of formula agitating paddle no longer continue at any time to 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 when upper hydrolysis.After terminating reaction, chloromethanes is to be excessively added, and excessive chloromethanes is in the environment of 160 DEG C
Evaporation, water is met in 63 DEG C of condenser E101, is hydrolyzed, and generates hydrochloric acid and methanol, methanol discharge vaporization to glass regards in bucket, molten
Yu Shui；Remaining liq (including micro hydrochloric acid) is collected in chilling flux bath；Stopping is passed through nitrogen, opens chilling flux bath and gathers
The valve between reaction kettle is closed, cooling solvent discharge is entered in polymerization reaction kettle, the hydrochloric acid in polymerization reaction kettle is the same as excessive carbonic acid
Nak response generates potassium chloride and CO2；
Step 4：Polymerisation post-processes：Cooling polymerization reaction kettle, to 63 DEG C, in period time switch drainage line
Valve (5s is opened, and 10s is closed), until material is all released in pure water (58 DEG C) in polymerization reaction kettle, is dissolved in N, N- dimethyl second
Polysulfone resin in amide starts that fluffy solid resin is precipitated；Simultaneously if there is continuing the chloromethanes of dissolving in a solvent in water
It is hydrolyzed into methanol and hydrochloric acid, hydrochloric acid generates potassium chloride and CO with carbonic acid nak response2；63 DEG C of temperature of gas phase and liquid phase section are set,
Micro- excessive chloromethanes can be made to be fully hydrolyzed, reduced dangerous；
Step 5：Purification：Purification processes are carried out to the polysulfone resin that step 4 is precipitated using water-boiling method.
Step 6：It squeezes out：In 174 DEG C by polysulfone resin hot extrusion bar.
Entire reaction production about 120kg polysulfone resins.According to the difference of the degree of polymerization, the different trades mark, quality can be distinguished
It is constant.In 174 degrees Celsius of polysulfone resin hot extrusion bars, the visual clarity for adding the polysulfones bar of capping reagent is more preferable,
Analyze reason, addition capping reagent prepare polysulfone resin, cross dimeric molecule it is less, be suitble to injection molding and hot melting temperature stablize；Do not add
Add the polysulfones of capping reagent under same extrusion temperature, the visual clarity of polysulfones bar is not so good as the former, appropriate crowded when being promoted
After going out temperature, transparency improves, and analyzes reason, and part high polymer do not melt, and when extrusion influences transparency, and high polymer was
Dimeric molecule.
By taking the polymerisation material selected by embodiment ten as an example, it is respectively adopted poly- described in embodiment one to embodiment nine
Sulphone resin industrialized producing technology prepares the polysulfone resin of corresponding polysulfone resin and the preparation of embodiment ten as one He of test group
Test group ten, the polysulfone resin performance that detection embodiment one is prepared to embodiment ten, in the item for choosing same polymerisation material
Under part, the purity of polysulfone resin is prepared, while it is the patent of invention of 104629055 A of CN to select application publication number, it is disclosed
Polysulfone resin prepared by industrialized production polysulfones high molecular material method as a control group, carries out performance test experience.Detection
Method and detection are shown in Table 2.
Test group and the experiment of control group polysulfone resin performance detection：
2 polysulfone resin performance detection of table is tested
It is detected through the method for data and feature shown in table 2, it is the life described in embodiment ten to obtain most preferred embodiment
Production. art, the technical program, wherein embodiment nine and embodiment ten are consistent method, by embodiment one in nine phase of embodiment
Comparison, the embodiment of the present invention nine be most preferred embodiment, prepare polysulfone resin physical and chemical parameter it is best, and in preparation with it is right
It is compared according to group, it is more efficient.Embodiment one to embodiment nine is prepared using the polymerisation material described in embodiment ten simultaneously
Polysulfone resin and embodiment ten prepared by polysulfone resin, its performance is more excellent compared to the control group.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of polysulfone resin industrialized producing technology, which is characterized in that include the following steps：
Step 1：Polymerisation pre-treatment：Into polymerization reaction kettle, addition is used to prepare the polymerisation material of polysulfone resin, opens
Blender in polymeric kettle is opened, is passed through inert gas into polymerization reaction kettle, in metathesis polymerizable reaction kettle after gas-phase space gas, to
The interlayer of polymerization reaction kettle is passed through high-temperature heat-conductive material, and the polymerisation material in polymerization reaction kettle is made to reach polymerisation temperature
Degree；
Step 2：Polymerisation：Continue to be passed through high-temperature heat-conductive material to the interlayer of polymerization reaction kettle, be examined by viscosity detecting device
The viscosity in polymerization reaction kettle is surveyed, the temperature in polymerization reaction kettle is detected by temperature-detecting device, when temperature-detecting device is examined
The temperature information of survey 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 of survey is more than polymeric reaction temperature range, then it is passed through cooling solvent into polymerization reaction kettle, controls polymerization reaction kettle
Interior temperature is within the scope of polymeric reaction temperature；
Step 3：Polymerisation terminates：When the viscosity number of viscosity detecting device detection reaches target viscosities, to polymerization reaction kettle
It is inside passed through capping reagent, organic solvent viscosity terminates polymerization for after stationary value, stopping is passed through capping reagent in reaction kettle to be polymerized
Reaction reduces polymerisation temperature in the kettle and obtains polysulfone resin with purification processes through being precipitated.
2. polysulfone resin industrialized producing technology according to claim 1, which is characterized in that the polymerisation material
For the polymerisation material with free radical, the capping reagent that is passed through in the polymerization reaction kettle makes to prepare in polymerisation poly-
Sulphone resin free radical is replaced.
3. polysulfone resin industrialized producing technology according to claim 1, which is characterized in that the capping reagent is chlorine
Methane；The inert gas is nitrogen or carbon dioxide.
4. polysulfone resin industrialized producing technology according to claim 1, which is characterized in that the polysulfone resin industrialization
Production technology further includes step 4：Polymerisation post-processes, and the mixing obtained after polymerization reaction terminating in polymerization reaction kettle is molten
Liquid is emitted by drainage line in water, is made remaining chloromethanes hydrolysis in organic solvent, is dissolved polysulfones in organic solvent
Resin is precipitated, and switch valve is provided in the drainage line.
5. polysulfone resin industrialized producing technology according to claim 4, which is characterized in that the output of the drainage line
End is connected with nozzle；The temperature of the water is 55~60 DEG C；
Purification processes are carried out using water-boiling method to the polysulfone resin being precipitated in water；Hot extrusion technique squeezes out to obtain after purified processing
Polysulfones bar；The temperature of the hot extrusion technique is 170~175 DEG C.
6. polysulfone resin industrialized producing technology according to claim 4, which is characterized in that the drainage line upper switch
Mixed solution is delivered in pure water by valve discontinuity；The each opening time of switch valve is 5s, when closing a length of 10s, open and
It closes and alternately controls.
7. polysulfone resin industrialized producing technology according to claim 1, which is characterized in that in step 2, pass through tune
Section is passed through the temperature in the flow control polymerization reaction kettle of high-temperature heat-conductive material；In the step 3, polymerization reaction kettle is through nature
It is cooled to temperature and obtains mixed solution for 60~70 DEG C, the mixed solution obtains polysulfone resin through being precipitated with purification processes.
8. polysulfone resin industrialized producing technology according to claim 1, which is characterized in that at the top of the polymerization reaction kettle
It is connected with polymerization tower, is connected with condenser at the top of the polymerization tower, the output end of the condenser is connected with gas-liquid separator, institute
It states gas-liquid separator and is connected separately with chilling flux bath and output device；
When polymerisation started in the period being completely exhausted out to polymeric reaction product, persistently open between condenser and polymerization tower
The temperature of valve, control condenser inner condensat liquid is 63 DEG C hereinafter, making the condensed device input of gas of the solvent and evaporation of evaporation
Into gas-liquid separation tower, the liquid flux of separation is passed through chilling flux bath by the gas-liquid separation tower, and by the gas of separation
Output device is passed through to be discharged；
The chilling flux bath is connect with polymerization reaction kettle by switch valve, in polymerization stage, if temperature detection fills
The temperature value for setting detection is more than range of reaction temperature, then opens the switch valve between chilling flux bath and polymerization reaction kettle, make cold
But solvent is passed through in polymerization reaction kettle；After polymerisation, device that reaction process is evaporated and condensed and gas-liquid are collected
The organic solvent that separator is handled.
9. polysulfone resin industrialized producing technology according to claim 8, which is characterized in that after terminating polymerisation, stop
It is only passed through inert gas, and opens the valve between chilling flux bath and polymerization reaction kettle, it is anti-that cooling solvent discharge is entered polymerization
It answers in kettle, then reduces polymerisation temperature in the kettle and obtain polysulfone resin with purification processes through being precipitated.
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| CN112239540B (en) * | 2020-12-21 | 2021-03-19 | 富海(东营)新材料科技有限公司 | Industrial purification process and purification device for polysulfone resin material |
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| JP2012211290A (en) * | 2011-03-31 | 2012-11-01 | Sumitomo Chemical Co Ltd | Method for producing polysulfone with reduced halogen content |
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