CN107090127B - A kind of reinforced polypropylene material with good microwave absorbing property - Google Patents
A kind of reinforced polypropylene material with good microwave absorbing property Download PDFInfo
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- CN107090127B CN107090127B CN201710429693.XA CN201710429693A CN107090127B CN 107090127 B CN107090127 B CN 107090127B CN 201710429693 A CN201710429693 A CN 201710429693A CN 107090127 B CN107090127 B CN 107090127B
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- glass fibre
- microwave absorbing
- absorbing property
- reinforced polypropylene
- polypropylene material
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- -1 polypropylene Polymers 0.000 title claims abstract description 72
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 59
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 59
- 239000000463 material Substances 0.000 title claims abstract description 43
- 239000003365 glass fiber Substances 0.000 claims abstract description 41
- 238000012545 processing Methods 0.000 claims abstract description 27
- 239000000314 lubricant Substances 0.000 claims abstract description 17
- 239000012760 heat stabilizer Substances 0.000 claims abstract description 13
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 18
- 150000007524 organic acids Chemical class 0.000 claims description 12
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 9
- 238000010907 mechanical stirring Methods 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000004381 surface treatment Methods 0.000 claims description 5
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 3
- 230000000640 hydroxylating effect Effects 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 2
- 150000001408 amides Chemical class 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 150000008301 phosphite esters Chemical class 0.000 claims description 2
- 239000000344 soap Substances 0.000 claims description 2
- 239000003381 stabilizer Substances 0.000 claims description 2
- 229910052769 Ytterbium Inorganic materials 0.000 claims 1
- 238000005660 chlorination reaction Methods 0.000 claims 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims 1
- 238000001125 extrusion Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 12
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 238000005453 pelletization Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 229940056319 ferrosoferric oxide Drugs 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- CKLHRQNQYIJFFX-UHFFFAOYSA-K ytterbium(III) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Yb+3] CKLHRQNQYIJFFX-UHFFFAOYSA-K 0.000 description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012913 prioritisation Methods 0.000 description 2
- 239000011975 tartaric acid Substances 0.000 description 2
- 235000002906 tartaric acid Nutrition 0.000 description 2
- 244000248349 Citrus limon Species 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 description 1
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 235000013922 glutamic acid Nutrition 0.000 description 1
- 239000004220 glutamic acid Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/01—Magnetic additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention provides a kind of reinforced polypropylene material and preparation method thereof with good microwave absorbing property includes 60~87 parts of polypropylene；10~30 parts of glass fibre of special surface processing；2~6 parts of polypropylene grafted maleic anhydride；1~3 part of nano ferriferrous oxide；0.1~0.5 part of heat stabilizer；0.1~0.5 part of lubricant；A kind of reinforced polypropylene material with good microwave absorbing property is prepared for using double screw extruder extrusion, the material shows better microwave absorbing property, and intensity is high, pollution-free and of the invention preparation method is simple, can be used for military and builds anti-electromagnetic pollution field.
Description
Technical field
The present invention relates to polypropylene technology fields, and in particular to a kind of reinforced polypropylene with good microwave absorbing property
Material and preparation method thereof.
Background technique
Extensive use with electromagnetic wave in telecommunications field, the brings electromagnetism such as mobile phone, wireless network, radar
The problem of radiation, interference, is increasingly taken seriously；Meanwhile electromagnetic wave technology is also widely used in present military field, such as
Radar Technology.Based on requirements above, the research and development of microwave absorbing material are particularly important.Glass fibre is that engineering plastics commonly enhance
Material prepares electroconductive glass fibre and has become the important method for solving the problems, such as electromagnetic shielding as the conductive filler of composite material,
It can achieve the effect that Material reinforcement and electromagnetic shielding simultaneously.Traditional chemical plating be prepare electroconductive glass fibre common technology it
One, but its complex process, and heavy metal is expensive and causes seriously to pollute to environment, while effectiveness and paying no attention to
Think.
Summary of the invention
The object of the present invention is to provide a kind of with the reinforced polypropylene material of good microwave absorbing property and its preparation side
Method.
A kind of reinforced polypropylene material with good microwave absorbing property, prepared in parts by weight by following components and
At:
60~87 parts of polypropylene；
10~30 parts of glass fibre of special surface processing；
2~6 parts of polypropylene grafted maleic anhydride；
1~3 part of nano ferriferrous oxide；
0.1~0.5 part of heat stabilizer；
0.1~0.5 part of lubricant；
The glass fibre is the chopped E glass of alkali-free, and 6~9 μm of glass fiber single filament diameter, length are 3~6mm, compared with
Thin glass fiber single filament diameter to be more advantageous to surface treatment, and be conducive to improve electromagnetic shielding performance；The special surface
The glass fibre of processing is fiber surface by the mixture of SrBiTiO and rare earth compound surface treatment glass fibers obtained
Dimension, SrBiTiO: rare earth compound mixture weight ratio is 5: 1~10: 1, and the rare earth compound is lanthanum chloride, in ytterbium chloride
One kind, SrBiTiO and rare earth compound are jointly processed by glass surface with synergistic effect；At least contain 10 in the polypropylene
~30 parts of physical aspect is the polypropylene of powdery, powdered granule help to improve nano ferriferrous oxide due to have it is magnetic and
Caused aggregation is conducive to it and disperses and add the ratio that concentration reaches formula design in reinforced polypropylene；The nanometer
The size of ferroso-ferric oxide powder is no more than 300 nanometers, and the addition of ferroso-ferric oxide further improves electromagnetic shielding performance.
Glass fibre special surface processing the preparation method is as follows:
(1) soaking and washing in acetone soln is put into after first calcining glass fibre 60~100 minutes at 200~300 DEG C
30~60 minutes；By the glass fibre after cleaning be put into the hydrochloric acid solution of 2mol/L~4mol/L carry out hydroxylating processing 30~
It 80 minutes, is then dried under the conditions of 40~70 DEG C after deionized water is washed.
(2) dimethylformamide, acetic acid and polyvinylpyrrolidone are passed through at room temperature according to the ratio of weight ratio 4: 1: 1
Mechanical stirring has configured mixed solution, and the mixture of SrBiTiO and rare earth compound is added to by 60~120rpm of mixing speed
The weight ratio of mixed solution, mixture and mixed solution is 1: 10, is configured to aaerosol solution through mechanical stirring, mixing speed 60~
120rpm。
(3) it glass fibre and will suspend through in (1) treated glass fibre the is added to aaerosol solution through (2) processing
The mass ratio of both solution is 4: 1, and 3~5 times of distilled water of glass fibre and aaerosol solution weight, mechanical stirring 10~15 is added
Minute, 80~100rpm of mixing speed；Glass is filtered out, is then dried at 50~60 DEG C, can be prepared by special surface processing
Glass fibre.
The polyacrylic melt flow rate (MFR) is in pressure 2.16kg, 230 DEG C of temperature of 0.1~100g/min of condition.
The heat stabilizer be one of phenolic thermostabilizers, amine heat stabilizer, phosphite ester type thermal stabilizing agent or
It is a variety of.
The lubricant is one of metal soap lubricant, the compound ester lubricant of stearic acid and amide series lubricant agent
Or it is a variety of.
The maleic anhydride content 1%~50% of the polypropylene grafted maleic anhydride.
A kind of preparation method of the reinforced polypropylene material with good microwave absorbing property, comprising the following steps:
(1), according to the ratio, by polypropylene, polypropylene grafted maleic anhydride, heat stabilizer, lubricant, nano ferriferrous oxide
It puts into height and stirs pot stirring 3~5 minutes, mixing speed 500rpm.
(2), the mixed material that will be stirred through (1) is fed by the main feeding of double screw extruder, special surface processing
Glass fibre added twin-screw extrude by lateral feeding, in double screw extruder carry out melt blending, squeeze out make
The obtained reinforced polypropylene material of grain；The draw ratio of the screw extruder is 40: 1~48: 1, and processing temperature is 170~250 DEG C,
Enhancing poly- third is prepared by water cooling bracing pelletizing in 400~600rpm of screw speed, negative-pressure vacuum 0.04~0.06MPa of degree
Alkene.
Although present invention employs powdered polypropylene, since nano ferriferrous oxide is easy in extrusion process
It is poly-, and since ferroso-ferric oxide itself has ferromagnetism, it is easily adsorbed in equipment in process, and be not easy to disperse, root
The reinforced polypropylene mechanical property of materials prepared according to above scheme is low, especially poor toughness, and the reinforced polypropylene material prepared
The content of middle ferroso-ferric oxide is lower than formula setting value, and invention further provides prioritization schemes, by weight by following components
Number is prepared:
60~87 parts of polypropylene；
10~30 parts of glass fibre of special surface processing；
2~6 parts of polypropylene grafted maleic anhydride；
1.5~4.5 parts of iron chloride mixture be dissolved in organic acid；
0.1~0.5 part of heat stabilizer；
0.1~0.5 part of lubricant；
Advanced optimize the preparation method of the reinforced polypropylene material of scheme, comprising the following steps:
(1), first by iron chloride FeCL3It is mixed in agitated kettle with organic acid according to 1.5: 1 ratios, organic acid is lemon
Acid, tartaric acid, citric acid, tartaric acid, one of glutamic acid, stearic acid, palmitic acid, mixing speed are 120~200rpm, stirring
Time 5~8 minutes, the iron chloride mixture being dissolved in organic acid is made.
(2), according to the ratio, by polypropylene, polypropylene grafted maleic anhydride, heat stabilizer, lubricant, through (1) processing it is molten
Iron chloride mixture of the solution in organic acid is put into stir in pot and be stirred 2~3 minutes, and 250~300rpm of mixing speed takes more
Low mixing speed is to lead to organic acid melting volatilization to prevent high-speed stirred from easily causing overheat, and material is caused to agglomerate.
(3) mixed material that will be stirred through (2) is fed by the main feeding of double screw extruder, special surface processing
Glass fibre is added twin-screw extrude by lateral feeding, carries out melt blending, reinforced polypropylene material is made in extruding pelletization
Material；The draw ratio of the screw extruder is 48: 1~60: 1,160~230 DEG C, 300~500rpm of screw speed of processing temperature, more
Low screw speed helps to elongate residence time of the material in twin-screw, negative-pressure vacuum degree 0.06~0.1MPa, higher
Vacuum degree facilitates the abundant devolatilization of organic acid low molecule in material, favorably improves the final mechanical property of materials, squeezes out and passes through water
Reinforced polypropylene is prepared in cold drawn bar pelletizing.
Prioritization scheme is FeCL3For presoma, organic acid is dispersing agent, is directly scattered in polypropylene, then by squeezing
Machine thermally decomposes FeCL in situ out3, nanoscale Fe 3 O 4 magnetic particle is formed under dispersing agent effect, while controlling and preparing
The technological parameters such as mixing time, mixing speed, extrusion temperature, screw speed, the vacuum degree of journey, so that the increasing finally prepared
Strong polypropylene mechanical performance is improved, and especially toughness is greatly improved.
Specific embodiment
The formula of comparative example 1~2 and Examples 1 to 4 is shown in Table 1
The formula of 1 comparative example 1~2 of table and Examples 1 to 4
Heat stabilizer selects 1010 and 168, and the two ratio is 1: 1 (weight ratio), and lubricant selects ethylene bis stearamide.
For the glass fiber single filament diameter that comparative example 1 uses for 13 μm, remaining formula filament diameter is 8 μm.Embodiment 3 is to glass fibers dimension table
Surface treatment is ytterbium chloride using rare earth compound, remaining uses lanthanum chloride.The screw rod for the double screw extruder that embodiment 4 uses is long
Diameter is than 52: 1, the screw slenderness ratio 44: 1 for the double screw extruder that remaining embodiment and comparative example use.4 screw rod of embodiment turns
Speed is 500rpm, 2 screw speed 300rpm of embodiment.
Fiberglass surfacing processing step in comparative example 1~2 and Examples 1 to 4 is as follows:
(1) soaking and washing 50 in acetone soln is put into after first calcining glass fibre 90 minutes at 200~300 DEG C to divide
Clock；Glass fibre after cleaning is put into the hydrochloric acid solution of 3mol/L and carries out hydroxylating processing 50 minutes, then through deionization
It is dried under the conditions of 50 DEG C after water washing；
(2) dimethylformamide, acetic acid and polyvinylpyrrolidone are passed through at room temperature according to the ratio of weight ratio 4: 1: 1
Mechanical stirring has configured mixed solution, and the mixture of SrBiTiO and rare earth compound are added to mixing by mixing speed 100rpm
The weight ratio of solution, mixture and mixed solution is 1: 10, is configured to aaerosol solution, mixing speed 100rpm through mechanical stirring；
(3) it glass fibre and will suspend through in (1) treated glass fibre the is added to aaerosol solution through (2) processing
The mass ratio of both solution is 4: 1, and 3 times of distilled water of glass fibre and aaerosol solution weight are added, mechanical stirring 12 minutes, stir
Mix speed 90rpm；Glass is filtered out, is then dried at 55 DEG C, can be prepared by the glass fibre of special surface processing.
The preparation method of the reinforced polypropylene material of comparative example 1~2 and implementation 1 and embodiment 3, comprising the following steps:
(1), according to the ratio, by polypropylene, polypropylene grafted maleic anhydride, heat stabilizer, lubricant, nano ferriferrous oxide
(the no added nano ferriferrous oxide of comparative example 2) puts into height and stirs pot stirring 4 minutes, mixing speed 500rpm.
(2), the mixed material that will be stirred through (1) is fed by the main feeding of double screw extruder, special surface processing
Glass fibre added twin-screw extrude by lateral feeding, in double screw extruder carry out melt blending, squeeze out make
The obtained reinforced polypropylene material of grain；The draw ratio of the screw extruder is 44: 1, and processing temperature is 170~250 DEG C, and screw rod turns
Reinforced polypropylene is prepared by water cooling bracing pelletizing in fast 500rpm, negative-pressure vacuum 0.04~0.06MPa of degree.
Implement 2 and embodiment 4 reinforced polypropylene material preparation method the following steps are included:
(1), first by iron chloride FeCL3It is mixed in agitated kettle with stearic acid according to 1.5: 1 ratios, mixing speed is
Mixing time 6 minutes, the iron chloride mixture being dissolved in organic acid was made in 180rpm.
(2), according to the ratio, by polypropylene, polypropylene grafted maleic anhydride, heat stabilizer, lubricant, through (1) processing it is molten
Iron chloride mixture of the solution in organic acid is put into stir in pot and be stirred 3 minutes, mixing speed 280rpm.
(3), the mixed material that will be stirred through (2) is fed by the main feeding of double screw extruder, special surface processing
Glass fibre added twin-screw extrude by lateral feeding, carry out melt blending, extruding pelletization be made reinforced polypropylene
Material；The draw ratio of the double screw extruder of embodiment 2 is 44: 1, and the draw ratio of the double screw extruder of embodiment 4 is 52: 1,
160~230 DEG C of processing temperature, 2 screw speed 300rpm of embodiment, 4 screw speed 500rpm of embodiment, negative-pressure vacuum degree 0.06
~0.1MPa is squeezed out and reinforced polypropylene is prepared by water cooling bracing pelletizing.
By polypropylene material prepared by above-described embodiment 1~4 and comparative example 1~2 according to using coaxial line transmission/reflection
The electromagnetic parameter of method measurement gained fibrous material, is made the ring-shaped sample of outer diameter 7.00mm, internal diameter 3.04mm, thickness about 2mm, in beauty
Their complex dielectric permittivities in 2~18GHz frequency range and multiple are measured on state's Agilent E5071C type vector network analyzer
Magnetic conductivity simulates the microwave absorbing property for calculating and analyzing corresponding single layer and double-layer structure microwave absorbing coating according to transmission line theory.
The mechanical performance of material is tested according to national standard.
The performance test results of comparative example 1~2 and Examples 1 to 4 are shown in Table 2
The performance of 2 comparative example 1~2 of table and Examples 1 to 4
Comparative example 1 and embodiment 1, which compare, shows that the electromagnetic wave absorption performance of thinner filament diameter is more preferable.Comparative example 2 and reality
It applies example 1 and compares the addition for showing nano ferriferrous oxide, can further improve the electromagnetic wave absorption performance of reinforced polypropylene.Implement
Example 3 and embodiment 1, which compare, shows that ytterbium chloride is more advantageous to the electromagnetic wave absorption performance for improving material than lanthanum chloride.4 He of embodiment
Embodiment 2, which compares, shows that lower screw speed, shorter screw slenderness ratio are more advantageous to the electromagnetic wave absorbability for improving material
Energy.
The mechanical performance testing result of Examples 1 to 2 is shown in Table 3
The mechanical performance of 3 Examples 1 to 2 of table
Embodiment 1 and embodiment 2 compare the iron chloride mixture substitution directly addition shown using being dissolved in organic acid
Nano ferriferrous oxide prepares reinforced polypropylene, and mechanical performance is greatly improved, and especially toughness is obviously improved, simultaneously
The electromagnetic wave absorption performance of material slightly improves.
It can be seen that from table 2 and table 3, the wave-sucking performance of polypropylene material produced by the present invention and to microwave absorption frequency range
Width makes modified polypropylene material show better microwave absorbing property, and intensity is high, pollution-free, can be used for it is military and
Anti- electromagnetic pollution field is built, and preparation method of the invention is simple.
This hair can be understood and applied the above description of the embodiments is intended to facilitate those skilled in the art
It is bright.Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein
General Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to implementations here
Example, those skilled in the art's announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be
Within protection scope of the present invention.
Claims (7)
1. a kind of reinforced polypropylene material with good microwave absorbing property, it is characterised in that: by weight by following components
Number is prepared:
60 ~ 87 parts of polypropylene；
10 ~ 30 parts of glass fibre of special surface processing；
2 ~ 6 parts of polypropylene grafted maleic anhydride；
1 ~ 3 part of nano ferriferrous oxide；
0.1 ~ 0.5 part of heat stabilizer；
0.1 ~ 0.5 part of lubricant；
The glass fibre is the chopped E glass of alkali-free, and 6 ~ 9 μm of glass fiber single filament diameter, length are 3 ~ 6mm；It is described special
The glass fibre of surface treatment is fiber surface by the mixture of SrBiTiO and rare earth compound surface treatment glass obtained
Fiber, SrBiTiO: rare earth compound mixture weight ratio is 5:1 ~ 10:1, and the rare earth compound is lanthanum chloride, chlorination
One of ytterbium；Contain 10 ~ 30 parts of physical aspect in the polypropylene at least for the polypropylene of powdery；The nanometer four aoxidizes
The size of three iron powder bodies is no more than 300 nanometers.
2. a kind of reinforced polypropylene material with good microwave absorbing property according to claim 1, the glass fibers
Tie up special surface processing the preparation method is as follows:
(1) soaking and washing 30 ~ 60 in acetone soln are put into after first calcining glass fibre 60 ~ 100 minutes at 200 ~ 300 DEG C
Minute；Glass fibre after cleaning is put into the hydrochloric acid solution of 2mol/L ~ 4mol/L and carries out 30 ~ 80 points of hydroxylating processing
Then clock is dried under the conditions of 40 ~ 70 DEG C after deionized water is washed；
(2) by dimethylformamide, acetic acid and polyvinylpyrrolidone according to the ratio of weight ratio 4:1:1 at room temperature through machinery
It is configured to be stirred mixed solution, the mixture of SrBiTiO and rare earth compound are added to mixing by 60 ~ 120rpm of mixing speed
The weight ratio of solution, mixture and mixed solution is 1:10, is configured to aaerosol solution through mechanical stirring, mixing speed 60 ~
120rpm；
(3) will be through in (1) treated glass fibre the is added to aaerosol solution through (2) processing, glass fibre and aaerosol solution
The mass ratio of the two be 4:1, be added glass fibre and aaerosol solution weight 3 ~ 5 times of distilled water, mechanical stirring 10 ~ 15 minutes,
80 ~ 100rpm of mixing speed；Glass is filtered out, is then dried at 50 ~ 60 DEG C, can be prepared by the glass fibers of special surface processing
Dimension.
3. a kind of reinforced polypropylene material with good microwave absorbing property, feature exist according to claim 1
In: the polyacrylic melt flow rate (MFR) is 0.1 ~ 100g/10min under conditions of pressure 2.16kg, 230 DEG C of temperature.
4. a kind of reinforced polypropylene material with good microwave absorbing property, feature exist according to claim 1
In: the heat stabilizer be one of phenolic thermostabilizers, amine heat stabilizer, phosphite ester type thermal stabilizing agent or a variety of.
5. a kind of reinforced polypropylene material with good microwave absorbing property, feature exist according to claim 1
In: the lubricant be one of metal soap lubricant, the compound ester lubricant of stearic acid and amide series lubricant agent or more
Kind.
6. a kind of reinforced polypropylene material with good microwave absorbing property, feature exist according to claim 1
In: the maleic anhydride content 1% ~ 50% of the polypropylene grafted maleic anhydride.
7. a kind of reinforced polypropylene material with good microwave absorbing property, feature exist according to claim 1
In: the nano ferriferrous oxide is replaced using the iron chloride mixture being dissolved in organic acid.
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| CN106479038A (en) * | 2015-08-27 | 2017-03-08 | 合肥杰事杰新材料股份有限公司 | A kind of RPP material of high electro-magnetic wave absorption performance and preparation method thereof |
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