CN103865266A - Polysulfone engineering plastic production method and equipment - Google Patents
Polysulfone engineering plastic production method and equipment Download PDFInfo
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- CN103865266A CN103865266A CN201210541415.0A CN201210541415A CN103865266A CN 103865266 A CN103865266 A CN 103865266A CN 201210541415 A CN201210541415 A CN 201210541415A CN 103865266 A CN103865266 A CN 103865266A
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Abstract
The present invention discloses a polysulfone engineering plastic production method, which comprises: 1, carrying out a normal pressure polymerization reaction of chlorophenyl sulfone, bisphenol A, potassium carbonate and a dimethyl acetamide solvent at a certain reaction temperature; 2, adding purified water to the product obtained in the step 1, and crushing to obtain a mother liquor and a solid material; 3, distilling the mother liquor obtained in the step 2 to recover the dimethyl acetamide solvent, and washing the solid material obtained in the step 2 with purified water; and 4, drying the washed solid material in the step 3 to obtain the final product. The present invention further discloses polysulfone engineering plastic production equipment.
Description
Technical field
The present invention relates to organic high molecular compound preparation and processing technique field, relate in particular to a kind of polysulfones engineering plastics production method and equipment.
Background technology
Polysulfones is the thermoplastic resin that contains chain link in molecular backbone chain.Polysulfones mechanical property excellence, rigidity is large, wear-resisting, high strength, due to its good characteristic, polysulfones has been widely used in multiple technical fields such as mechanical industry, electronic apparatus, communications and transportation, medicine equipment.
The polysulfones production method using in prior art, its solvent adopts dimethyl sulfoxide (DMSO).Not only the smell is awful for dimethyl sulfoxide solvent, but also have toxicity.In polysulfones manufacture process, easily endanger the healthy of staff, when overflowing, smell also can cause environmental pollution.
Meanwhile, the polysulfones production unit moisture eliminator using in prior art is dry by drainage, causes humidity of materials larger, has extended time of drying, has increased production cost.The polysulfones production unit moisture eliminator using in prior art is in addition roundabout drier, and in vacuum, fine powder easily overflows, therefore need to install cyclonic separator.
Summary of the invention
In order to overcome the defect existing in prior art, the invention provides a kind of polysulfones engineering plastics production method and equipment, harmless environmental friendliness, and finished product processing performance can effectively improve.
A kind of polysulfones engineering plastics production method, comprising: step 1, by the polymerization under atmospheric pressure reaction 12 hours under the temperature of reaction of 150 ℃ ~ 170 ℃ of sulphenone, dihydroxyphenyl propane, salt of wormwood and dimethylacetamide solvent; Step 2, add pure water to pulverize as mother liquor and solid materials products therefrom in step 1; Step 3, dimethylacetamide solvent will be reclaimed after the mother liquor distillation in this step 2; Solid materials in this step 2 is washed with pure water; Step 4, by dry the solid materials after pure water washing in the step 3 final product that obtains.
Further, in this step 1, sulphenone is 58.6 parts, and dihydroxyphenyl propane is 49.8 parts, and salt of wormwood is 45.7 parts, and the final product generating in described step 4 is 100 parts.
Further, this mother liquor comprises water, N,N-DIMETHYLACETAMIDE and Repone K.
Further, in this step 4, solid materials is dry before through centrifuge dripping.
Further, in this step 1, the time of polymerization under atmospheric pressure reaction is at least 12 hours.In this step 1, the time of polymerization under atmospheric pressure reaction is 12 to 16 hours.In this step 1, the temperature of reaction of polymerization under atmospheric pressure reaction is 150 ℃ ~ 155 ℃.
Further, in this step 3, mother liquor distillation time is 10 hours.In this step 3, solid materials is through pure water washing 3 to 6 times.In this step 3, solid materials is through pure water washing 4 times.
Further, in this step 4, the dry time of solid materials is 8 hours.
The present invention discloses a kind of polysulfones engineering plastics production unit simultaneously, comprising: a polymeric kettle, for dropping into sulphenone, dihydroxyphenyl propane, salt of wormwood and dimethylacetamide solvent and normal pressure generation polyreaction under the temperature of reaction of 150 ℃ ~ 170 ℃; One pulverizer, this pulverizer is connected with this polymeric kettle, for the resultant of polymeric kettle being pulverized for mother liquor and solid materials; One still kettle, this still kettle is connected with this pulverizer, for distilling mother liquor and reclaiming dimethylacetamide solvent; One washing kettle, this washing kettle is connected with this pulverizer, for washing this solid materials; One drying kettle, this drying kettle is connected with this washing kettle, obtains final product for dry this solid materials after washing.
Further, the temperature of reaction in polymeric kettle is 150 ℃ ~ 155 ℃.
Further, this polymeric kettle is a glassed steel reaction vessels, and the stirring arm of this glassed steel reaction vessels is anchor formula, and rotating speed is 65 revs/min, and this glassed steel reaction vessels is through the heat-conducting oil heating of 250 ℃.This still kettle is chuck heating, and thermophore is superheated vapour, and the temperature of this hot steam is 150 ℃, and pressure is 6kg/cm
2.This washing kettle is chuck heating, and thermophore is superheated vapour, and the temperature of this hot steam is 110 ℃, and pressure is 4kg/cm
2.This drying kettle is helical-ribbon type drying kettle, and this helical-ribbon type drying kettle overlaps interior 250 ℃ of thermal oils circulation, vacuum tightness maximum-0.1Mpa in still, and ribbon Revolution Per Minute 15 turns.Baiting valve is Worm-gear type.This polysulfones engineering plastics production unit also comprises a whizzer, and this whizzer is connected with drying kettle with this washing kettle.
Compared with prior art, polysulfones engineering plastics production method provided by the present invention and production unit, do not need dimethyl sulfoxide (DMSO) as solvent, solved dimethylacetamide solvent in prior art and easily cause the defect of health threat and environmental pollution.Polysulfones engineering plastics production unit provided by the present invention adopts helical-ribbon type moisture eliminator, and not only drying efficiency is high, also can save the cyclonic separator that must use in prior art, makes Whole Equipment cost, and the product each side index of production is all significantly increased.
Accompanying drawing explanation
Can be by following detailed Description Of The Invention and appended graphic being further understood about the advantages and spirit of the present invention.
Fig. 1 be shown in the present go out polysulfones engineering plastics production method schema;
Fig. 2 be shown in the present go out polysulfones engineering plastics production method device structure schematic diagram.
Embodiment
Describe a kind of polysulfones engineering plastics production method and the equipment of a kind of specific embodiment of the present invention in detail below in conjunction with accompanying drawing.But, the present invention should be understood as and be not limited to this embodiment described below, and technical concept of the present invention can be implemented with other known technologies or the combination of function other technologies identical with those known technologies.
In the following description, for clear structure of the present invention and the mode of operation of showing, to be described by all multidirectional words, but should by 'fornt', 'back', " left side ", " right side ", " outward ", " interior ", " outwards ", " inwardly ", " on ", the Word Understanding such as D score is for convenience of term, and not should be understood to word of limitation.
As shown in fig. 1, technical scheme provided by the present invention specifically comprises:
S1, sulphenone, dihydroxyphenyl propane, salt of wormwood and dimethylacetamide solvent are carried out to polymerization under atmospheric pressure reaction at a certain temperature.Typically, polymeric reaction temperature can be set between 150 ℃ to 170 ℃, and the viscosity of the final product polysulfones that different temperature of reaction obtains is different.In the present embodiment, preferably the temperature of reaction of 150 ℃ ~ 155 ℃ as optimal reaction temperature.By sulphenone, dihydroxyphenyl propane, salt of wormwood and dimethylacetamide solvent polymerization under atmospheric pressure reaction at a certain temperature at least 12 hours.According to different viscosity requirements, this polymerization under atmospheric pressure reaction times can be between 12 hours to 16 hours.
S2, add pure water to pulverize as mother liquor and solid materials products therefrom in S1.
S3, dimethylacetamide solvent will be reclaimed after the mother liquor distillation in this S2.Solid materials in this S2 is washed with pure water.
S4, by dry the solid materials after pure water washing in the S3 final product that obtains.
To in detail production technique operating process and the equipment that uses be described below:
The first step, raw material drop into polymeric kettle:
Sulphenone (58.6%), dihydroxyphenyl propane (49.8%), salt of wormwood (45.7%), dimethylacetamide solvent (volume 1500ml).Wherein, the per-cent proportioning of sulphenone, dihydroxyphenyl propane, salt of wormwood is to produce the charging capacity that 100 parts of polysulfones products are foundation calculating.The raw material total amount of now throwing is 154.1 parts, wherein 58.6 parts of sulphenones, and 49.8 parts of dihydroxyphenyl propanes, 45.7 parts, salt of wormwood, resultant polysulfones is 100 parts, another 54.1 parts is byproduct discharge.Approximately 40 parts, Repone K in byproduct, all the other are water and carbonic acid gas.In the present embodiment, the polymeric kettle volume 3000ml using.This polymeric kettle is glassed steel reaction vessels, and its stirring arm is anchor formula, 65 revs/min of rotating speeds, and chuck heating, by heat-conducting oil heating, 250 ℃ of oil temperatures.The polyreaction of raw material in polymeric kettle is normal pressure, and at least 12 hours reaction times, material reaction temperature is controlled at 150 ℃ ~ 170 ℃ left and right.The viscosity of the final product polysulfones that different temperature of reaction and different reaction times obtain is different.In order to reach best-of-breed technology effect, the material reaction temperature using in present embodiment is 150 ℃ ~ 155 ℃, and polymerization reaction time is 12-16 hour.
Second step, pulverizing:
Polyreaction finishes post polymerization thing and must add pure water to pulverize.After pulverizing, the liquid of gained claims mother liquor, containing solvent N,N-DIMETHYLACETAMIDE, water, Repone K, mother liquor is delivered to distillation plant and carry out solvent recuperation, and solid materials is delivered to washing plant and is washed in mother liquor.
The 3rd step, distillation and washing:
Mother liquor enters still kettle.Still kettle is chuck heating.Thermophore is superheated vapour, the about 150 ℃ of left and right of pressure 6kg/cm2(temperature).Utilize water different from solvent boiling point, layering distillation.Dimethylacetamide solvent after recovery can use in the time that feed intake next time.Water is as discharge of wastewater, through the qualified water drain that enters of wastewater treatment.Distillation approximately needs 10 hours, and byproduct is Repone K crystallization, can provide the factory of other needs to use.
Washing must be used pure water.The pure water unit production capacity being equipped with is 3 tons/hour, washing totally four times.Water after washing still needs distillation for the first time, described in its distilation steps sees above.Second and third, four washing water can be used for pulverizing after polyreaction water and next time production process wash for the first time.Before washing each time, must be broken through pulverizer band pigment, more carefully more to wash totally, the transparency of product is better.Wash and complete for approximately 10 hours.Washing kettle volume 10000L, chuck heating.Hot medium is superheated vapour, approximately 110 ℃ of left and right of pressure 4kg/cm2(temperature).In order to reach best technique effect, before dry materials, material can be dried with whizzer, then send into drying kettle with worm conveyor and enter next link.
The 4th step, dry:
Adopt 6000L helical-ribbon type drying kettle.Total approximately 8 hours time of drying, the about 500kg of the final powder product of drying kettle.250 ℃ of thermal oil circulations in drying kettle chuck, vacuum tightness maximum-0.1Mpa in still.The ribbon Revolution Per Minute 15 of this helical-ribbon type drying kettle turns, and its baiting valve adopts Worm-gear type, opens lightly, controls easily.Client needs powdery, i.e. check, pack, warehouse-in.
The 5th step, granulation (optional) are the step S5 in schema 1:
As client needs granularly, dry emit powder 10 and send to granulation.Equipment adopts single screw pelletizer.
The 6th step, the examination and test of products, be packaged as the step S6 in schema 1
The equal sampling Detection of each batch products factory quality supervision, qualified after i.e. packing warehouse-in, issue client.
The cod concentration that produces waste water in production is 1560PPM/L, and standard is cod<100PPM/L, available precipitation, charcoal absorption, and biochemical treatment tertiary treatment is up to standard.
The present invention also provides a kind of polysulfones engineering plastics production unit.As shown in Figure 2, this production unit comprises: polymeric kettle 101, be used for dropping into raw material 1(and comprise sulphenone, dihydroxyphenyl propane, salt of wormwood and dimethylacetamide solvent) and under certain temperature of reaction normal pressure produce polyreaction, typically, polymeric reaction temperature can be set between 150 ℃ to 170 ℃, and the viscosity of the final product polysulfones that different temperature of reaction obtains is different.In the present embodiment, preferably the temperature of reaction of 150 ℃ ~ 155 ℃ as optimal reaction temperature.By sulphenone, dihydroxyphenyl propane, salt of wormwood and dimethylacetamide solvent polymerization under atmospheric pressure reaction at a certain temperature at least 12 hours.According to different viscosity requirements, this polymerization under atmospheric pressure reaction times can be between 12 hours to 16 hours.Pulverizer 102, this pulverizer 102 is connected with this polymeric kettle 101, for the resultant of polymeric kettle 101 is pulverized as mother liquor and solid materials.Still kettle 103, this still kettle 103 is connected with this pulverizer 102, for distilling mother liquor and reclaiming dimethylacetamide solvent.Washing kettle 104, this washing kettle 104 is connected with this pulverizer 102, for washing this solid materials.Drying kettle 105, this drying kettle 105 is connected with this washing kettle 104, obtains final product for dry this solid materials after washing.In addition, this polysulfones engineering plastics production unit also comprises the chemical industry common equipments such as storage tanks, condenser, tower.
Following table is the test performance table of the finished product that manufactures through polysulfones engineering plastics production method provided by the present invention and equipment, from this table, and the product that its performance index of the product manufacturing according to the present invention are produced far above prior art.
The experiment condition of upper table and method explanation:
1, density/Density
Inspecting standard: GB/T 1033.1-2008;
2, tensile strength/Tensile Modulus
Inspecting standard: GB/T 1040.1-2008;
3, flexural strength/Flexural Strength
Inspecting standard: GB/T 9341-2008;
4, modulus in flexure/Flexural Modulus
Inspecting standard: GB/T 9341-2008;
5, simple beam impact strength (breach)/Charpy Impact Strength(Notch)
Inspecting standard: GB/T 1043.1-2008, the impact energy that wherein breach uses is 2J;
6, heat-drawn wire/HDT
Inspecting standard: GB/T 1634.1-2004;
7, dielectric strength/Dielectric Strength
Inspecting standard: GB/T 1408.1-2006;
8, volume resistivity/Volume Resistivity
Inspecting standard: GB/T 1410-2006;
9, linear expansivity/Linear Expansivity
Inspecting standard: GB/T 2572-2005.
Compared with prior art, polysulfones engineering plastics production method provided by the present invention and production unit, do not need dimethyl sulfoxide (DMSO) as solvent, solved dimethylacetamide solvent in prior art and easily cause the defect of health threat and environmental pollution.Polysulfones engineering plastics production unit provided by the present invention adopts helical-ribbon type moisture eliminator, and not only drying efficiency is high, also can save the cyclonic separator that must use in prior art, makes Whole Equipment cost, and the product each side index of production is all significantly increased.Simultaneously polysulfones engineering plastics production method provided by the present invention and production unit, its waste water producing in producing to environment without any pollution.
Described in this specification sheets is preferred embodiment of the present invention, and above embodiment is only in order to illustrate technical scheme of the present invention but not limitation of the present invention.All those skilled in the art, all should be within the scope of the present invention under this invention's idea by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (18)
1. a polysulfones engineering plastics production method, is characterized in that, comprising:
Step 1, by the polymerization under atmospheric pressure reaction under the temperature of reaction of 150 ℃ ~ 170 ℃ of sulphenone, dihydroxyphenyl propane, salt of wormwood and dimethylacetamide solvent;
Step 2, add pure water to pulverize as mother liquor and solid materials products therefrom in step 1;
Step 3, described dimethylacetamide solvent will be reclaimed after the mother liquor distillation in described step 2; Solid materials in described step 2 is washed with pure water;
Step 4, the solid materials drying after pure water washing in step 3 is obtained to final product.
2. polysulfones engineering plastics production method as described in claim 1, is characterized in that, in described step 1, sulphenone is 58.6 parts, and dihydroxyphenyl propane is 49.8 parts, and salt of wormwood is 45.7 parts, and the final product generating in described step 4 is 100 parts.
3. polysulfones engineering plastics production method as described in claim 1, is characterized in that, described mother liquor comprises water, N,N-DIMETHYLACETAMIDE and Repone K.
4. polysulfones engineering plastics production method as described in claim 1, is characterized in that, in described step 4 solid materials dry before through centrifuge dripping.
5. polysulfones engineering plastics production method as described in claim 1, is characterized in that, in described step 1, the time of polymerization under atmospheric pressure reaction is at least 12 hours.
6. polysulfones engineering plastics production method as described in claim 5, is characterized in that, in described step 1, the time of polymerization under atmospheric pressure reaction is 12 to 16 hours.
7. polysulfones engineering plastics production method as described in claim 1, is characterized in that, in described step 1, the temperature of reaction of polymerization under atmospheric pressure reaction is 150 ℃ ~ 155 ℃.
8. polysulfones engineering plastics production method as described in claim 1, is characterized in that, in described step 3, mother liquor distillation time is 10 hours.
9. polysulfones engineering plastics production method as described in claim 1, is characterized in that, in described step 3, solid materials is through pure water washing 3 to 6 times.
10. polysulfones engineering plastics production method as described in claim 9, is characterized in that, in described step 3, solid materials is through pure water washing 4 times.
11. polysulfones engineering plastics production methods as described in claim 1, is characterized in that, in described step 4, the dry time of solid materials is 8 hours.
12. 1 kinds of polysulfones engineering plastics production units, is characterized in that, comprising:
One polymeric kettle, for dropping into sulphenone, dihydroxyphenyl propane, salt of wormwood and dimethylacetamide solvent and normal pressure generation polyreaction under the temperature of reaction of 150 ℃ ~ 170 ℃;
One pulverizer, described pulverizer is connected with described polymeric kettle, for the resultant of polymeric kettle being pulverized for mother liquor and solid materials;
One still kettle, described still kettle is connected with described pulverizer, for distilling mother liquor and reclaiming described dimethylacetamide solvent;
One washing kettle, described washing kettle is connected with described pulverizer, for washing described solid materials;
One drying kettle, described drying kettle is connected with described washing kettle, obtains final product for dry described solid materials after washing.
13. polysulfones engineering plastics production units as claimed in claim 12, is characterized in that, the temperature of reaction in described polymeric kettle is 150 ℃ ~ 155 ℃.
14. polysulfones engineering plastics production units as claimed in claim 12, it is characterized in that, described polymeric kettle is a glassed steel reaction vessels, and the stirring arm of described glassed steel reaction vessels is anchor formula, rotating speed is 65 revs/min, and described glassed steel reaction vessels is through the heat-conducting oil heating of 250 ℃.
15. polysulfones engineering plastics production units as claimed in claim 12, is characterized in that, described still kettle is chuck heating, and thermophore is superheated vapour, and the temperature of described hot steam is 150 ℃, and pressure is 6kg/cm
2.
16. polysulfones engineering plastics production units as claimed in claim 12, is characterized in that, described washing kettle is chuck heating, and thermophore is superheated vapour, and the temperature of described hot steam is 110 ℃, and pressure is 4kg/cm
2.
17. polysulfones engineering plastics production units as claimed in claim 12, it is characterized in that, described drying kettle is helical-ribbon type drying kettle, described helical-ribbon type drying kettle overlaps interior 250 ℃ of thermal oils circulation, vacuum tightness maximum-0.1Mpa in still, ribbon Revolution Per Minute 15 turns, and the baiting valve of described helical-ribbon type drying kettle is Worm-gear type.
18. polysulfones engineering plastics production units as claimed in claim 12, is characterized in that, described polysulfones engineering plastics production unit also comprises a whizzer, and described whizzer is connected with drying kettle with described washing kettle.
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| CN201210541415.0A CN103865266A (en) | 2012-12-13 | 2012-12-13 | Polysulfone engineering plastic production method and equipment |
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| CN201210541415.0A CN103865266A (en) | 2012-12-13 | 2012-12-13 | Polysulfone engineering plastic production method and equipment |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106220853A (en) * | 2016-09-12 | 2016-12-14 | 李涛 | A kind of polysulfone resin industrialized producing technology |
| CN110272545A (en) * | 2019-06-12 | 2019-09-24 | 扬州清研高分子新材料有限公司 | A kind of processing method shortening the polysulfones production cycle |
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| US20020115791A1 (en) * | 2000-12-14 | 2002-08-22 | General Electric Company | Polysulfone/polysiloxane polycarbonate block copolymers |
| US6562935B1 (en) * | 1998-09-25 | 2003-05-13 | Sumitomo Chemical Company, Limited | Thermoplastic aromatic polysulfone resin composition |
| CN102482412A (en) * | 2009-09-29 | 2012-05-30 | 住友化学株式会社 | Aromatic polysulfone resin and membranes thereof |
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Patent Citations (4)
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| CN85101721A (en) * | 1985-04-01 | 1986-09-24 | 中国科学院长春应用化学研究所 | The synthetic polyether sulphone that has the phthalein side group of single stage method |
| US6562935B1 (en) * | 1998-09-25 | 2003-05-13 | Sumitomo Chemical Company, Limited | Thermoplastic aromatic polysulfone resin composition |
| US20020115791A1 (en) * | 2000-12-14 | 2002-08-22 | General Electric Company | Polysulfone/polysiloxane polycarbonate block copolymers |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106220853A (en) * | 2016-09-12 | 2016-12-14 | 李涛 | A kind of polysulfone resin industrialized producing technology |
| CN110272545A (en) * | 2019-06-12 | 2019-09-24 | 扬州清研高分子新材料有限公司 | A kind of processing method shortening the polysulfones production cycle |
| CN110272545B (en) * | 2019-06-12 | 2020-08-04 | 扬州清研高分子新材料有限公司 | Processing method for shortening polysulfone production period |
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