CN113603983A - Wave-absorbing plastic master batch and preparation method thereof - Google Patents
Wave-absorbing plastic master batch and preparation method thereof Download PDFInfo
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- CN113603983A CN113603983A CN202110955393.1A CN202110955393A CN113603983A CN 113603983 A CN113603983 A CN 113603983A CN 202110955393 A CN202110955393 A CN 202110955393A CN 113603983 A CN113603983 A CN 113603983A
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- 239000004033 plastic Substances 0.000 title claims abstract description 34
- 229920003023 plastic Polymers 0.000 title claims abstract description 34
- 239000004594 Masterbatch (MB) Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000011246 composite particle Substances 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 23
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 13
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 9
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000004952 Polyamide Substances 0.000 claims abstract description 6
- 229920002647 polyamide Polymers 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 4
- 239000012856 weighed raw material Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 44
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 40
- 239000008367 deionised water Substances 0.000 claims description 39
- 229910021641 deionized water Inorganic materials 0.000 claims description 39
- 239000000463 material Substances 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 25
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 22
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 22
- 229910052757 nitrogen Inorganic materials 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 15
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 claims description 12
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 12
- 229960002089 ferrous chloride Drugs 0.000 claims description 12
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 12
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 15
- 239000002122 magnetic nanoparticle Substances 0.000 abstract description 11
- 239000011159 matrix material Substances 0.000 abstract description 6
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 6
- 239000005543 nano-size silicon particle Substances 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 4
- 239000000377 silicon dioxide Substances 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 239000011241 protective layer Substances 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 230000003301 hydrolyzing effect Effects 0.000 abstract description 2
- 239000002861 polymer material Substances 0.000 abstract description 2
- 239000011358 absorbing material Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000006467 substitution reaction 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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2427/00—Characterised by the use 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; Derivatives of such polymers
- C08J2427/02—Characterised by the use 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; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/04—Characterised by the use 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; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2427/06—Homopolymers or copolymers of vinyl chloride
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
-
- 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
- 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
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- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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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 invention relates to a wave-absorbing plastic master batch and a preparation method thereof, belonging to the technical field of high polymer materials and comprising the following raw materials in parts by weight: 25-35 parts of wave-absorbing particles, 50-60 parts of PVC, 10-15 parts of polyamide and 3-5 parts of antioxidant; uniformly mixing the weighed raw materials, adding the mixture into a double-screw extruder, blending and extruding, and then carrying out bracing and grain cutting to prepare wave-absorbing plastic master batches; the method comprises the steps of hydrolyzing tetraethoxysilane to generate nano-silicon dioxide, adding magnetic nano-particles in the reaction process, coating the magnetic nano-particles by the generated nano-silicon dioxide to prepare composite particles, preventing the magnetic nano-particles from being lost due to poor oxidation resistance and corrosion resistance, and modifying a silicon dioxide protective layer on the surfaces of the composite particles by a silane coupling agent to prevent the composite particles from agglomerating to cause that the prepared wave-absorbing particles cannot be uniformly dispersed in a plastic matrix.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a wave-absorbing plastic master batch and a preparation method thereof.
Background
The wave-absorbing material is also called as an electromagnetic wave absorbing material, a microwave absorbing material or a radar stealth material, and is a material capable of absorbing or greatly reducing electromagnetic wave energy received by the surface of the material so as to reduce electromagnetic wave interference. In engineering application, the wave-absorbing material is required to have high absorption rate to electromagnetic waves in a wider frequency band, and also required to have the properties of light weight, temperature resistance, moisture resistance, corrosion resistance and the like. The method is widely applied to the aspects of stealth of aerospace and military target radars, electromagnetic radiation shielding and the like.
When the microwave absorbing material is used in the field of plastic materials, due to the characteristics of plastics, the microwave absorbing performance is often endowed by adding a filler and a microwave absorbing material in a blending mode, and microwave absorbing particles are uniformly dispersed in a plastic matrix while the mechanical strength of the plastic materials is not influenced, so that the microwave absorbing material is an urgent problem to be solved.
Disclosure of Invention
In order to solve the technical problems, the invention provides a wave-absorbing plastic master batch and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
the wave-absorbing plastic master batch comprises the following raw materials in parts by weight: 25-35 parts of wave-absorbing particles, 50-60 parts of PVC, 10-15 parts of polyamide and 3-5 parts of antioxidant;
the wave-absorbing particles are prepared by the following steps:
step S1, mixing ferric chloride hexahydrate, ferrous chloride tetrahydrate and cobalt chloride hexahydrate, adding the mixture into treated deionized water, introducing nitrogen, stirring at a constant speed, heating to 75 ℃, slowly dropwise adding ammonia water, keeping the temperature at the temperature, reacting for 30min, separating a product by a magnet after the reaction is finished, washing the product to be neutral by the deionized water, dispersing the product into the deionized water, performing ultrasonic treatment for 15min, filtering and drying to obtain a primary material, and controlling the dosage ratio of the ferric chloride hexahydrate, the ferrous chloride tetrahydrate, the cobalt chloride hexahydrate and the deionized water to be 2.5-2.8 mmol: 1.05-1.08 mmol: 0.25 mmol: 100mL, and the volume ratio of the ammonia water to the deionized water to be 1: 20;
step S2, placing absolute ethyl alcohol in a water bath at 45 ℃ for heating, introducing nitrogen to remove oxygen for 30min, stirring at a constant speed, sequentially adding deionized water, ammonia water and tetraethoxysilane, stirring at a constant speed for 10min, adding the primary material, continuously stirring and reacting for 30min to obtain composite particles, wherein the dosage ratio of the absolute ethyl alcohol, the deionized water, the ammonia water, the tetraethoxysilane to the primary material is controlled to be 50 mL: 3 mL: 1.5 mL: 0.3-0.5 mL: 2 g;
and step S3, adding the composite particles into N-methyl pyrrolidone, performing ultrasonic dispersion for 30min, adding a silane coupling agent, introducing nitrogen, stirring at a constant speed for 2h to prepare a dispersion liquid, centrifuging, taking out and cleaning a product, and drying in a drying oven at 60 ℃ for 4h to prepare the wave-absorbing particles, wherein the weight ratio of the composite particles to the N-methyl pyrrolidone to the silane coupling agent is controlled to be 2: 1: 20.
Ferric chloride hexahydrate, ferrous chloride tetrahydrate, cobalt chloride hexahydrate and the like are used as raw materials, ammonia water is added as a precipitating agent to prepare a primary material, the primary material is magnetic nanoparticles, then ethyl orthosilicate is used for hydrolysis to generate nano-silica, the magnetic nanoparticles are added in the reaction process, the generated nano-silica forms a coating on the magnetic nanoparticles to prepare composite particles, the magnetic nanoparticles are prevented from being lost due to poor oxidation resistance and corrosion resistance, and then a silicon dioxide protective layer on the surface of the composite particles is modified by a silane coupling agent to prevent the composite particles from agglomerating, so that the prepared wave absorbing particles cannot be uniformly dispersed in a plastic matrix.
Further: the deionized water treated in step S1 is the deionized water after nitrogen has been deoxygenated.
Further: the antioxidant is any one of a phenol antioxidant or a phosphite antioxidant.
A preparation method of wave-absorbing plastic master batches comprises the following steps:
uniformly mixing the weighed raw materials, adding the mixture into a double-screw extruder, blending and extruding, controlling the blending temperature to be 200-250 ℃ and the screw rotating speed to be 200r/min, and then carrying out bracing and grain cutting to obtain the wave-absorbing plastic master batch.
The invention has the beneficial effects that:
the wave-absorbing plastic master batch of the invention takes PVC as a matrix, and provides good electromagnetic wave absorption performance for the matrix by adding wave-absorbing particles, in the preparation process of the wave-absorbing particles, ferric chloride hexahydrate, ferrous chloride tetrahydrate, cobalt chloride hexahydrate and the like are used as raw materials, ammonia water is added as a precipitator to prepare a primary material, the primary material is magnetic nanoparticles, then, the nano silicon dioxide is generated by hydrolyzing ethyl orthosilicate, the magnetic nanoparticles are added in the reaction process, the generated nano silicon dioxide coats the magnetic nanoparticles to prepare composite particles, the loss of the magnetic nanoparticles caused by poor oxidation resistance and corrosion resistance is prevented, and then, a silicon dioxide protective layer on the surface of the composite particles is modified by a silane coupling agent to prevent the composite particles from agglomerating to cause that the prepared wave-absorbing particles cannot be uniformly dispersed in a plastic matrix.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The wave-absorbing particles are prepared by the following steps:
step S1, mixing ferric chloride hexahydrate, ferrous chloride tetrahydrate and cobalt chloride hexahydrate, adding the mixture into deionized water obtained after nitrogen is deaerated, introducing nitrogen, stirring at a constant speed, heating to 75 ℃, then slowly dropwise adding ammonia water, keeping the temperature at the temperature, reacting for 30min, separating a product through a magnet after the reaction is finished, washing the product to be neutral by using the deionized water, dispersing the product into the deionized water, performing ultrasonic treatment for 15min, filtering and drying to obtain a primary material, and controlling the dosage ratio of the ferric chloride hexahydrate, the ferrous chloride tetrahydrate, the cobalt chloride hexahydrate and the deionized water to be 2.5 mmol: 1.05 mmol: 0.25 mmol: 100mL, and the volume ratio of the ammonia water to the deionized water to be 1: 20;
step S2, placing absolute ethyl alcohol in a water bath at 45 ℃ for heating, introducing nitrogen to remove oxygen for 30min, stirring at a constant speed, sequentially adding deionized water, ammonia water and tetraethoxysilane, stirring at a constant speed for 10min, adding the primary material, continuously stirring and reacting for 30min to obtain composite particles, wherein the dosage ratio of the absolute ethyl alcohol, the deionized water, the ammonia water, the tetraethoxysilane to the primary material is controlled to be 50 mL: 3 mL: 1.5 mL: 0.3 mL: 2 g;
and step S3, adding the composite particles into N-methyl pyrrolidone, performing ultrasonic dispersion for 30min, adding a silane coupling agent, introducing nitrogen, stirring at a constant speed for 2h to prepare a dispersion liquid, centrifuging, taking out and cleaning a product, and drying in a drying oven at 60 ℃ for 4h to prepare the wave-absorbing particles, wherein the weight ratio of the composite particles to the N-methyl pyrrolidone to the silane coupling agent is controlled to be 2: 1: 20.
Example 2
The wave-absorbing particles are prepared by the following steps:
step S1, mixing ferric chloride hexahydrate, ferrous chloride tetrahydrate and cobalt chloride hexahydrate, adding the mixture into deionized water obtained after nitrogen is deaerated, introducing nitrogen, stirring at a constant speed, heating to 75 ℃, then slowly dropwise adding ammonia water, keeping the temperature at the temperature, reacting for 30min, separating a product through a magnet after the reaction is finished, washing the product to be neutral by using the deionized water, dispersing the product into the deionized water, performing ultrasonic treatment for 15min, filtering and drying to obtain a primary material, and controlling the dosage ratio of the ferric chloride hexahydrate, the ferrous chloride tetrahydrate, the cobalt chloride hexahydrate and the deionized water to be 2.6 mmol: 1.06 mmol: 0.25 mmol: 100mL, and the volume ratio of the ammonia water to the deionized water to be 1: 20;
step S2, placing absolute ethyl alcohol in a water bath at 45 ℃ for heating, introducing nitrogen to remove oxygen for 30min, stirring at a constant speed, sequentially adding deionized water, ammonia water and tetraethoxysilane, stirring at a constant speed for 10min, adding the primary material, continuously stirring and reacting for 30min to obtain composite particles, wherein the dosage ratio of the absolute ethyl alcohol, the deionized water, the ammonia water, the tetraethoxysilane to the primary material is controlled to be 50 mL: 3 mL: 1.5 mL: 0.4 mL: 2 g;
and step S3, adding the composite particles into N-methyl pyrrolidone, performing ultrasonic dispersion for 30min, adding a silane coupling agent, introducing nitrogen, stirring at a constant speed for 2h to prepare a dispersion liquid, centrifuging, taking out and cleaning a product, and drying in a drying oven at 60 ℃ for 4h to prepare the wave-absorbing particles, wherein the weight ratio of the composite particles to the N-methyl pyrrolidone to the silane coupling agent is controlled to be 2: 1: 20.
Example 3
The wave-absorbing particles are prepared by the following steps:
step S1, mixing ferric chloride hexahydrate, ferrous chloride tetrahydrate and cobalt chloride hexahydrate, adding the mixture into deionized water obtained after nitrogen is deaerated, introducing nitrogen, stirring at a constant speed, heating to 75 ℃, then slowly dropwise adding ammonia water, keeping the temperature at the temperature, reacting for 30min, separating a product through a magnet after the reaction is finished, washing the product to be neutral by using the deionized water, dispersing the product into the deionized water, performing ultrasonic treatment for 15min, filtering and drying to obtain a primary material, and controlling the dosage ratio of the ferric chloride hexahydrate, the ferrous chloride tetrahydrate, the cobalt chloride hexahydrate and the deionized water to be 2.8 mmol: 1.08 mmol: 0.25 mmol: 100mL, and the volume ratio of the ammonia water to the deionized water to be 1: 20;
step S2, placing absolute ethyl alcohol in a water bath at 45 ℃ for heating, introducing nitrogen to remove oxygen for 30min, stirring at a constant speed, sequentially adding deionized water, ammonia water and tetraethoxysilane, stirring at a constant speed for 10min, adding the primary material, continuously stirring and reacting for 30min to obtain composite particles, wherein the dosage ratio of the absolute ethyl alcohol, the deionized water, the ammonia water, the tetraethoxysilane to the primary material is controlled to be 50 mL: 3 mL: 1.5 mL: 0.5 mL: 2 g;
and step S3, adding the composite particles into N-methyl pyrrolidone, performing ultrasonic dispersion for 30min, adding a silane coupling agent, introducing nitrogen, stirring at a constant speed for 2h to prepare a dispersion liquid, centrifuging, taking out and cleaning a product, and drying in a drying oven at 60 ℃ for 4h to prepare the wave-absorbing particles, wherein the weight ratio of the composite particles to the N-methyl pyrrolidone to the silane coupling agent is controlled to be 2: 1: 20.
Example 4
The wave-absorbing plastic master batch comprises the following raw materials in parts by weight: 25 parts of wave-absorbing particles, 50 parts of PVC, 10 parts of polyamide and 3 parts of antioxidant 168;
uniformly mixing the raw materials, adding the mixture into a double-screw extruder, blending and extruding, controlling the blending temperature to be 200 ℃ and the screw rotating speed to be 200r/min, and then carrying out bracing and grain cutting to obtain the wave-absorbing plastic master batch.
Example 5
The wave-absorbing plastic master batch comprises the following raw materials in parts by weight: 30 parts of wave-absorbing particles, 55 parts of PVC, 12 parts of polyamide and 4 parts of antioxidant 168;
uniformly mixing the raw materials, adding the mixture into a double-screw extruder, blending and extruding, controlling the blending temperature to be 200 ℃ and the screw rotating speed to be 200r/min, and then carrying out bracing and grain cutting to obtain the wave-absorbing plastic master batch.
Example 6
The wave-absorbing plastic master batch comprises the following raw materials in parts by weight: 35 parts of wave-absorbing particles, 60 parts of PVC, 15 parts of polyamide and 5 parts of antioxidant 168;
uniformly mixing the raw materials, adding the mixture into a double-screw extruder, blending and extruding, controlling the blending temperature to be 250 ℃ and the screw rotating speed to be 200r/min, and then carrying out bracing and grain cutting to obtain the wave-absorbing plastic master batch.
Comparative example 1
Compared with the embodiment 4, the comparative example uses the nano silicon dioxide to replace the wave-absorbing particles.
Comparative example 2
The comparative example is the wave-absorbing plastic master batch produced by a certain company on the market.
The shielding wave efficacy of the prepared plastic master batch was examined according to the regulation of SJ20524-1995, and the results are shown in the following table:
| example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example2 | |
| Frequency (MHz) | 1000 | 1000 | 1000 | 1000 | 1000 |
| Shielding effectiveness% | 97.6 | 97.3 | 97.5 | / | 90.0 |
| Frequency (MHz) | 10000 | 10000 | 10000 | 10000 | 10000 |
| Shielding effectiveness% | 97.3 | 97.1 | 97.2 | / | 85.6 |
From the above table, it can be seen that the wave-absorbing plastic master batch prepared by the invention has good electromagnetic shielding performance.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (7)
1. A wave-absorbing plastic master batch is characterized in that: the feed comprises the following raw materials in parts by weight: 25-35 parts of wave-absorbing particles, 50-60 parts of PVC, 10-15 parts of polyamide and 3-5 parts of antioxidant;
the wave-absorbing particles are prepared by the following steps:
step S1, mixing ferric chloride hexahydrate, ferrous chloride tetrahydrate and cobalt chloride hexahydrate, adding the mixture into treated deionized water, introducing nitrogen, stirring at a constant speed, heating to 75 ℃, then slowly dropwise adding ammonia water, keeping the temperature at the temperature, reacting for 30min, separating a product by a magnet after the reaction is finished, washing the product to be neutral by the deionized water, dispersing the product in the deionized water, performing ultrasonic treatment for 15min, and filtering and drying to obtain a primary material;
step S2, placing absolute ethyl alcohol in a water bath at 45 ℃ for heating, introducing nitrogen to remove oxygen for 30min, stirring at a constant speed, sequentially adding deionized water, ammonia water and tetraethoxysilane, stirring at a constant speed for 10min, adding the primary material, continuously stirring and reacting for 30min to obtain composite particles;
and step S3, adding the composite particles into N-methyl pyrrolidone, performing ultrasonic dispersion for 30min, adding a silane coupling agent, introducing nitrogen, stirring at a constant speed for 2h to prepare a dispersion liquid, centrifuging, taking out and cleaning a product, and drying in a drying oven at 60 ℃ for 4h to prepare the wave-absorbing particles.
2. The wave-absorbing plastic master batch according to claim 1, characterized in that: the deionized water treated in step S1 is the deionized water after nitrogen has been deoxygenated.
3. The wave-absorbing plastic master batch according to claim 1, characterized in that: in step S1, the dosage ratio of ferric chloride hexahydrate, ferrous chloride tetrahydrate, cobalt chloride hexahydrate and deionized water is controlled to be 2.5-2.8 mmol: 1.05-1.08 mmol: 0.25 mmol: 100mL, and the volume ratio of ammonia water to deionized water is 1: 20.
4. The wave-absorbing plastic master batch according to claim 1, characterized in that: in step S2, the dosage ratio of absolute ethyl alcohol, deionized water, ammonia water, ethyl orthosilicate and the primary material is controlled to be 50 mL: 3 mL: 1.5 mL: 0.3-0.5 mL: 2 g.
5. The wave-absorbing plastic master batch according to claim 1, characterized in that: in step S3, the weight ratio of the composite particles, N-methylpyrrolidone and silane coupling agent is controlled to be 2: 1: 20.
6. The wave-absorbing plastic master batch according to claim 1, characterized in that: the antioxidant is any one of a phenol antioxidant or a phosphite antioxidant.
7. The method for preparing the wave-absorbing plastic master batch according to claim 1, which is characterized by comprising the following steps: the method comprises the following steps:
uniformly mixing the weighed raw materials, adding the mixture into a double-screw extruder, blending and extruding, controlling the blending temperature to be 200-250 ℃ and the screw rotating speed to be 200r/min, and then carrying out bracing and grain cutting to obtain the wave-absorbing plastic master batch.
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