CN107304280A - A kind of preparation method of polyvinylidene fluoride material - Google Patents
A kind of preparation method of polyvinylidene fluoride material Download PDFInfo
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- CN107304280A CN107304280A CN201610235820.8A CN201610235820A CN107304280A CN 107304280 A CN107304280 A CN 107304280A CN 201610235820 A CN201610235820 A CN 201610235820A CN 107304280 A CN107304280 A CN 107304280A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/16—Homopolymers or copolymers or vinylidene fluoride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F114/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F114/18—Monomers containing fluorine
- C08F114/22—Vinylidene fluoride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical Kinetics & Catalysis (AREA)
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- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The invention discloses a kind of preparation method of polyvinylidene fluoride material, comprise the following steps;Step 1) prepare powdered Kynoar, 1) raw material is put into reactor, at a temperature of 4 10 DEG C, stirring reaction 20 40 minutes;2) polypropylene glycol solution, vinylidene fluoride monomers, methyl cyclopentane are passed through again, in 30 40 DEG C of stirring reactions, terminating reaction when pressure drops to 0.2 below 0.45MPa;3) by temperature drop to 5 10 DEG C, and kept for 20 35 minutes, then filter, wash, dry, produce powdered Kynoar;Step 2), powdered Kynoar, olefin(e) acid, benzophenone, Tissuemat E, zinc stearate and polyvinylpyrrolidone are added to comminutor, granulation operation is carried out, Kynoar plastic matrix is made;Step 3) Kynoar plastic matrix is added to injection machine, injection temperature is controlled at 280 330 DEG C, polyvinylidene fluoride material is made, product pressure resistance is good, more homogeneous without supporting layer, aperture, its vinylidene prepared has good heat endurance and machinability.
Description
Technical field
The present invention relates to plastics preparation field, more particularly to a kind of preparation method of polyvinylidene fluoride material.
Background technology
Kynoar (PVDF) is a kind of crystalline polymer of chain using-CH2-CF2- as construction unit,
In crystalline structure, the arrangement of carbochain indention, after hydrogen atom is replaced by the larger fluorine atom of electronegativity, with
Adjacent fluorine atom is mutually exclusive, so that fluorine atom is not in the same plane, and make spiral point along carbochain
Cloth, therefore surrounded in carbochain surrounding by the stable fluorine atom of a series of properties, this almost gapless space
Barrier prevents any atom or group to destroy carbochain from entering easily in its structure.Just because of this knot
Structure so that PVDF has the excellent chemical stability such as excellent acid and alkali resistance, oxidant.
It is more special a kind of in fluoro-containing plastic, plastics family, such as PVDF, PFA, PTFE, ETFE,
ECTFE ... possesses extremely strong corrosion resistance, heat endurance, is easy to processing.The sheet material that is made up of such material,
Bar, pipe part, plant equipment, be widely used in plating, photovoltaic, semiconductor, chemical industry, metallurgy,
Papermaking and pharmaceuticals industry, typical case such as printed substrate production equipment, silicon plate etching apparatus, also available for electricity
Sub- electrical equipment industry cable clad, sleeve pipe, collapsible tube, terminal plate, anode backplate, high-k electric capacity
Device film, ribbon heater, optical fiber sheath, external coating etc., and existing polyvinylidene fluoride, are used
In outdoor, easy quick aging.
We are by by material prescription, injection, the improvement of extrusion process condition, so as to change its molecule knot
Structure and physical property, such as tensile strength, modulus of elasticity, glass transition temperature index, make the material more severe
Still it can be played a role in the environment of quarter.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation method of polyvinylidene fluoride material, with
Solve caused above-mentioned multinomial defect in the prior art.
To achieve the above object, the present invention provides following technical scheme:A kind of polyvinylidene fluoride material
Preparation method, comprises the following steps
Step 1), prepare powdered Kynoar
1) 3-5 parts by weight hydrogen peroxide, 2-8 parts by weight of inorganic aqueous slkalis, are put into reactor, is well mixed,
The fluoro- 1,1,2- Separators of 10-13 parts by weight 1,2,2- tri-, the fluorine hexanoyl of 3-6 parts by weight 11 are put into again
Fluorine solution, 13-18 parts by weight dicholorodifluoromethane solvent, 1-3 parts by weight perfluoro butyl sulfonic acid fluoride solution,
At a temperature of -4-10 DEG C, stirring reaction 20-40 minutes;
2) 6-10 parts by weight polypropylene glycols solution, 15-23 parts by weight vinylidene fluoride monomers, 4-7 are passed through again
Parts by weight methyl cyclopentane, in 30-40 DEG C of stirring reaction, pressure drops to whole during below 0.2-0.45MPa
Only react;
3) by temperature drop to 5-10 DEG C, and kept for 20-35 minutes, then filter, wash, dry,
Produce powdered Kynoar;
Step 2), prepare Kynoar plastic matrix
By powdered Kynoar, olefin(e) acid, benzophenone, Tissuemat E, zinc stearate and polyethylene pyrrole
Pyrrolidone is added to comminutor, carries out granulation operation, is made Kynoar plastic matrix, comminutor with
100~500r/min speed operation;Its temperature control is at 18-25 DEG C;
Step 3), prepare polyvinylidene fluoride material
Kynoar plastic matrix is added to injection machine, injection temperature is controlled at 280-330 DEG C, is made
Polyvinylidene fluoride material, during toward fluorubber is added in injection machine, fluorubber is moulded relative to Kynoar
The weight ratio for expecting masterbatch is 1:900-950.
It is preferred that, the step 1) in, the fluorubber of 1-3 parts by weight, Huo Zhe are added in the first step
The fluorubber of 2-7 parts by weight is added in second step.
It is preferred that, the powdered Kynoar, olefin(e) acid, benzophenone, Tissuemat E, zinc stearate
Weight ratio with polyvinylpyrrolidone is 100:(10-12):(5-8):(3-7):(2-5):(8-12).
It is preferred that, the fluorubber preferred polyolefm class fluorubber, nitroso-fluoro-elastomers, 4 third fluorubber and
One or any two kinds of mixture in phosphonitrilic fluoro rubber.
It is preferred that, the TPO fluorubber, nitroso-fluoro-elastomers, 4 third fluorubber or phosphonitrilic fluoro rubber
Relative to Kynoar plastic matrix weight ratio respectively 1:920、1:932、1:928 and 1:948.
It is preferred that, the weight ratio of the fluorubber mixture is as follows:
TPO fluorubber:Nitroso-fluoro-elastomers is 2:3、
TPO fluorubber:4 third fluorubber are 1:2、
TPO fluorubber:Phosphonitrilic fluoro rubber is 2:3、
Nitroso-fluoro-elastomers:4 third fluorubber are 1:3、
Nitroso-fluoro-elastomers:Phosphonitrilic fluoro rubber is 3:2、
4 third fluorubber:Phosphonitrilic fluoro rubber is 2:1.
Beneficial effect using above technical scheme is:The polyvinylidene fluoride material that the present invention is processed, product
Pressure-resistant functional, more homogeneous without supporting layer, aperture, its vinylidene prepared has good heat
Stability and machinability, can meet the production technologies such as injection, extrusion and membrane, in addition, the side of the present invention
Method technique is simple and environmentally-friendly, is easy to industrializing implementation, has in fields such as food, medicine, chemical industry and widely should
With prospect, in the case that the material is used for outdoor, extends its service life, be particularly suitable in outdoor application.
Embodiment
The following detailed description of the preferred embodiment of the present invention.
Embodiment 1:
A kind of preparation method of polyvinylidene fluoride material, comprises the following steps
Step 1), prepare powdered Kynoar
1) 3 parts by weight hydrogen peroxide, 2 parts by weight of inorganic aqueous slkalis, are put into reactor, are well mixed, then
Put into the fluoro- 1,1,2- Separators of 10 parts by weight 1,2,2- tri-, the fluorine hexanoyl fluorine solution of 3 parts by weight 11,
13 parts by weight dicholorodifluoromethane solvents, 1 parts by weight perfluoro butyl sulfonic acid fluoride solution, then add 1 parts by weight
Fluorubber, the fluorubber is TPO fluorubber:4 third fluorubber ratios are 1:2 fluorubber mixing
Thing, at a temperature of -4 DEG C, stirring reaction 20 minutes;
2) 6 parts by weight polypropylene glycol solution, 15 parts by weight vinylidene fluoride monomers, 4 parts by weight methyl are passed through again
Pentamethylene, in 30 DEG C of stirring reactions, terminating reaction when pressure drops to below 0.2MPa;
3) by temperature drop to 5 DEG C, and kept for 20 minutes, then filter, wash, dry, produce powder
Last shape Kynoar;
Step 2), prepare Kynoar plastic matrix
By powdered Kynoar, olefin(e) acid, benzophenone, Tissuemat E, zinc stearate and polyethylene pyrrole
Pyrrolidone is added to comminutor, carries out granulation operation, and Kynoar plastic matrix is made, described powdered
Kynoar, olefin(e) acid, benzophenone, Tissuemat E, the weight of zinc stearate and polyvinylpyrrolidone
Than for 100:10:5:3:2:8, comminutor is run with 100r/min speed;Its temperature control is at 18 DEG C;
Step 3), prepare polyvinylidene fluoride material
Kynoar plastic matrix is added to injection machine, injection temperature is controlled at 280 DEG C, is made poly- inclined
Fluoride material, during toward fluorubber is added in injection machine, the fluorubber is TPO fluorubber, is gathered
Olefines fluorubber is relative to Kynoar plastic matrix weight ratio respectively 1:920.
Embodiment 2:
A kind of preparation method of polyvinylidene fluoride material, comprises the following steps
Step 1), prepare powdered Kynoar
1) 5 parts by weight hydrogen peroxide, 8 parts by weight of inorganic aqueous slkalis, are put into reactor, are well mixed, then
Put into the fluoro- 1,1,2- Separators of 13 parts by weight 1,2,2- tri-, the fluorine hexanoyl fluorine solution of 6 parts by weight 11,
18 parts by weight dicholorodifluoromethane solvents, 3 parts by weight perfluoro butyl sulfonic acid fluoride solution, at a temperature of 2 DEG C,
Stirring reaction 40 minutes;
2) 10 parts by weight polypropylene glycol solution, 15 parts by weight vinylidene fluoride monomers, 4 parts by weight first are passed through again
Cyclopentane, then the fluorubber of 7 parts by weight is added, the fluorubber is for TPO fluorubber:Phosphonitrile fluorine
Rubber ratio is 2:3 fluorubber mixture, in 40 DEG C of stirring reactions, pressure drops to below 0.45MPa
When terminating reaction;
3) by temperature drop to 10 DEG C, and kept for 35 minutes, then filter, wash, dry, produce powder
Last shape Kynoar;
Step 2), prepare Kynoar plastic matrix
By powdered Kynoar, olefin(e) acid, benzophenone, Tissuemat E, zinc stearate and polyethylene pyrrole
Pyrrolidone is added to comminutor, carries out granulation operation, and Kynoar plastic matrix is made, described powdered
Kynoar, olefin(e) acid, benzophenone, Tissuemat E, the weight of zinc stearate and polyvinylpyrrolidone
Than for 100:12:8:7:5:12, comminutor is run with 200r/min speed;Its temperature control exists
20℃;
Step 3), prepare polyvinylidene fluoride material
Kynoar plastic matrix is added to injection machine, injection temperature is controlled at 300 DEG C, is made poly- inclined
Fluoride material, during toward fluorubber is added in injection machine, the fluorubber is nitroso-fluoro-elastomers, nitrous
Base fluorubber is 1 relative to Kynoar plastic matrix weight ratio:932.
Embodiment 3:
A kind of preparation method of polyvinylidene fluoride material, comprises the following steps
Step 1), prepare powdered Kynoar
1) 4 parts by weight hydrogen peroxide, 6 parts by weight of inorganic aqueous slkalis, are put into reactor, are well mixed, then
Put into the fluoro- 1,1,2- Separators of 12 parts by weight 1,2,2- tri-, the fluorine hexanoyl fluorine solution of 5 parts by weight 11,
16 parts by weight dicholorodifluoromethane solvents, 2 parts by weight perfluoro butyl sulfonic acid fluoride solution, then add 2 parts by weight
Fluorubber, the fluorubber is nitroso-fluoro-elastomers:4 third fluorubber ratios are 1:3 fluorubber mixture,
At a temperature of 5 DEG C, stirring reaction 30 minutes;
2) 7 parts by weight polypropylene glycol solution, 18 parts by weight vinylidene fluoride monomers, 5 parts by weight methyl are passed through again
Pentamethylene, in 35 DEG C of stirring reactions, terminating reaction when pressure drops to below 0.35MPa;
3) by temperature drop to 8 DEG C, and kept for 30 minutes, then filter, wash, dry, produce powder
Last shape Kynoar;
Step 2), prepare Kynoar plastic matrix
By powdered Kynoar, olefin(e) acid, benzophenone, Tissuemat E, zinc stearate and polyethylene pyrrole
Pyrrolidone is added to comminutor, carries out granulation operation, and Kynoar plastic matrix is made, described powdered
Kynoar, olefin(e) acid, benzophenone, Tissuemat E, the weight of zinc stearate and polyvinylpyrrolidone
Than for 100:11:7:5:3:10, comminutor is run with 350r/min speed;Its temperature control exists
23℃;
Step 3), prepare polyvinylidene fluoride material
Kynoar plastic matrix is added to injection machine, injection temperature is controlled at 315 DEG C, is made poly- inclined
Fluoride material, during toward fluorubber is added in injection machine, the fluorubber is 4 third fluorubber, 4 third fluorine
Rubber is 1 relative to Kynoar plastic matrix weight ratio:928.
Embodiment 4:
A kind of preparation method of polyvinylidene fluoride material, comprises the following steps
Step 1), prepare powdered Kynoar
1) 4 parts by weight hydrogen peroxide, 6 parts by weight of inorganic aqueous slkalis, are put into reactor, are well mixed, then
Put into the fluoro- 1,1,2- Separators of 11 parts by weight 1,2,2- tri-, the fluorine hexanoyl fluorine solution of 5 parts by weight 11,
15 parts by weight dicholorodifluoromethane solvents, 2 parts by weight perfluoro butyl sulfonic acid fluoride solution, at a temperature of 8 DEG C,
Stirring reaction 25 minutes;
2) 7 parts by weight polypropylene glycol solution, 18 parts by weight vinylidene fluoride monomers, 6 parts by weight methyl are passed through again
Pentamethylene, then the fluorubber of 5 parts by weight is added, the fluorubber is TPO fluorubber:Nitroso fluorine rubber
Glue ratio is 2:3 fluorubber mixture, in 38 DEG C of stirring reactions, when pressure drops to below 0.33MPa
Terminating reaction;
3) by temperature drop to 7 DEG C, and kept for 28 minutes, then filter, wash, dry, produce powder
Last shape Kynoar;
Step 2), prepare Kynoar plastic matrix
By powdered Kynoar, olefin(e) acid, benzophenone, Tissuemat E, zinc stearate and polyethylene pyrrole
Pyrrolidone is added to comminutor, carries out granulation operation, and Kynoar plastic matrix is made, described powdered
Kynoar, olefin(e) acid, benzophenone, Tissuemat E, the weight of zinc stearate and polyvinylpyrrolidone
Than for 100:11:5:7:3:11, comminutor is run with 350r/min speed;Its temperature control exists
23℃;
Step 3), prepare polyvinylidene fluoride material
Kynoar plastic matrix is added to injection machine, injection temperature is controlled at 295 DEG C, is made poly- inclined
Fluoride material, during toward fluorubber is added in injection machine, the fluorubber is phosphonitrilic fluoro rubber, phosphonitrile fluorine
Rubber is 1 relative to Kynoar plastic matrix weight ratio:948.
Project | Index | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
Melt flow rate (MFR) (g/10min) | 6.6 | 7.8 | 7.3 | 6.9 | 4.2 |
Tensile strength (Mpa) | 36—50 | 63 | 68 | 66 | 72 |
Elongation (25 DEG C/%) | 50—70 | 72 | 78 | 74 | 81 |
Relative density (gcm-3) | 1.75—1.78 | 1.72 | 1.74 | 1.76 | 1.73 |
Fusing point (DEG C) | 144 | 168 | 178 | 181 | 172 |
Thermal stress ftractures | Do not split | Do not split | Do not split | Do not split | Do not split |
Water absorption rate (%) | 0.04 | 0.24 | 0.18 | 0.24 | 0.26 |
Glass transition temperature (DEG C) | -39 | -42 | -51 | -48 | -53 |
Brittle temperature (DEG C) | Below -62 | -81 | -72 | -89 | -76 |
Heat decomposition temperature (DEG C) | 320 | 415 | 395 | 420 | 380 |
Temperature (DEG C) is used for a long time | -40—125 | -60—160 | -50—145 | -55—165 | -60—140 |
Dielectric constant (60-106Hz) | 6.0—8.0 | 7.2 | 7.6 | 6.8 | 7.8 |
Specific insulation (Ω cm) | 3*1012 | 3*1012 | 3*1012 | 3*1012 | 3*1012 |
Tensile stress at yield (Mpa) | 80 | 90 | 102 | 93 | 108 |
Notch impact strength (KJ/cm2) | 11 | 14 | 18 | 17 | 15 |
Arc resistance (s) | 50—70 | 80 | 82 | 78 | 83 |
Anti-flammability | Self-extinguishment | Self-extinguishment | Self-extinguishment | Self-extinguishment | Self-extinguishment |
The polyvinylidene fluoride material that the present invention is processed, product pressure resistance is good, without supporting layer, aperture
It is more homogeneous, its prepare vinylidene there is good heat endurance and machinability, can meet injection,
The production technology such as extrusion and membrane, in addition, the method technique of the present invention is simple and environmentally-friendly, is easy to industrializing implementation,
It is with a wide range of applications in fields such as food, medicine, chemical industry, in the case that the material is used for outdoor,
Extend its service life, be particularly suitable in outdoor application.
Above-described is only the preferred embodiment of the present invention, it is noted that for the common skill of this area
For art personnel, without departing from the concept of the premise of the invention, various modifications and improvements can be made,
These belong to protection scope of the present invention.
Claims (6)
1. a kind of preparation method of polyvinylidene fluoride material, it is characterised in that comprise the following steps
Step 1), prepare powdered Kynoar
1) 3-5 parts by weight hydrogen peroxide, 2-8 parts by weight of inorganic aqueous slkalis, are put into reactor, is well mixed,
The fluoro- 1,1,2- Separators of 10-13 parts by weight 1,2,2- tri-, the fluorine hexanoyl of 3-6 parts by weight 11 are put into again
Fluorine solution, 13-18 parts by weight dicholorodifluoromethane solvent, 1-3 parts by weight perfluoro butyl sulfonic acid fluoride solution,
At a temperature of -4-10 DEG C, stirring reaction 20-40 minutes;
2) 6-10 parts by weight polypropylene glycols solution, 15-23 parts by weight vinylidene fluoride monomers, 4-7 are passed through again
Parts by weight methyl cyclopentane, in 30-40 DEG C of stirring reaction, pressure drops to whole during below 0.2-0.45MPa
Only react;
3) by temperature drop to 5-10 DEG C, and kept for 20-35 minutes, then filter, wash, dry,
Produce powdered Kynoar;
Step 2), prepare Kynoar plastic matrix
By powdered Kynoar, olefin(e) acid, benzophenone, Tissuemat E, zinc stearate and polyethylene pyrrole
Pyrrolidone is added to comminutor, carries out granulation operation, is made Kynoar plastic matrix, comminutor with
100~500r/min speed operation;Its temperature control is at 18-25 DEG C;
Step 3), prepare polyvinylidene fluoride material
Kynoar plastic matrix is added to injection machine, injection temperature is controlled at 280-330 DEG C, is made
Polyvinylidene fluoride material, during toward fluorubber is added in injection machine, fluorubber is moulded relative to Kynoar
The weight ratio for expecting masterbatch is 1:900-950.
2. the preparation method of polyvinylidene fluoride material according to claim 1, it is characterised in that institute
State step 1) in, the fluorubber of 1-3 parts by weight is added in the first step, or adds in second step 2-7
The fluorubber of parts by weight.
3. the preparation method of polyvinylidene fluoride material according to claim 1, it is characterised in that institute
State step 2) in, powdered Kynoar, olefin(e) acid, benzophenone, Tissuemat E, zinc stearate and
The weight ratio of polyvinylpyrrolidone is 100:(10-12):(5-8):(3-7):(2-5):(8-12).
4. the preparation method of polyvinylidene fluoride material according to claim 2, it is characterised in that institute
State in fluorubber preferred polyolefm class fluorubber, nitroso-fluoro-elastomers, 4 third fluorubber and phosphonitrilic fluoro rubber
One or any two kinds of mixture.
5. the preparation method of polyvinylidene fluoride material according to claim 4, it is characterised in that institute
TPO fluorubber, nitroso-fluoro-elastomers, 4 third fluorubber or phosphonitrilic fluoro rubber are stated relative to polyvinylidene fluoride
Alkene plastics master batch weight ratio respectively 1:920、1:932、1:928 and 1:948.
6. the preparation method of polyvinylidene fluoride material according to claim 4, it is characterised in that institute
The weight ratio for stating fluorubber mixture is as follows:
TPO fluorubber:Nitroso-fluoro-elastomers is 2:3、
TPO fluorubber:4 third fluorubber are 1:2、
TPO fluorubber:Phosphonitrilic fluoro rubber is 2:3、
Nitroso-fluoro-elastomers:4 third fluorubber are 1:3、
Nitroso-fluoro-elastomers:Phosphonitrilic fluoro rubber is 3:2、
4 third fluorubber:Phosphonitrilic fluoro rubber is 2:1.
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CN115028945A (en) * | 2022-07-26 | 2022-09-09 | 碧菲分离膜(大连)有限公司 | Synthetic method of polyvinylidene fluoride |
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