CN102585330A - Tungsten-polymer composite material and preparation method thereof - Google Patents

Tungsten-polymer composite material and preparation method thereof Download PDF

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Publication number
CN102585330A
CN102585330A CN2012100161038A CN201210016103A CN102585330A CN 102585330 A CN102585330 A CN 102585330A CN 2012100161038 A CN2012100161038 A CN 2012100161038A CN 201210016103 A CN201210016103 A CN 201210016103A CN 102585330 A CN102585330 A CN 102585330A
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tungsten
high molecular
molecular polymer
matrix material
tungsten powder
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赵国璋
宋久鹏
杨福民
赖亚洲
于洋
庄志刚
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HONGLU TUNGSTEN MOLYBDENUM INDUSTRY Co Ltd SHIAMEN
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HONGLU TUNGSTEN MOLYBDENUM INDUSTRY Co Ltd SHIAMEN
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Priority to CN2012100161038A priority Critical patent/CN102585330A/en
Priority to PCT/CN2012/073157 priority patent/WO2013107096A1/en
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/0887Tungsten
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/005Additives being defined by their particle size in general
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/54Silicon-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
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Abstract

The invention discloses a tungsten-polymer composite material and a preparation method thereof. The tungsten-polymer composite material comprises the following components in percentage by weight: 20-100% of polymers, 950-1000% of tungsten powder, 0-50% of tungsten fibers, 0.5-5% of coupling agent and 0.5-10% of other auxiliaries, wherein the tungsten powder is prepared through airflow pulverization and surface modification. The tungsten powder disclosed by the invention is good in compaction and flowability and high in loading capacity. The composite material disclosed by the invention is good in physical and mechanical properties, and excellent in weathering resistance, chemical resistance and organic solvent resistance, not only can be applied to the field of ray shielding, but also can be applied to the fields of vibration isolation, weight counterbalance, heat conduction, weapons and ammunitions and the like.

Description

A kind of tungsten-high molecular polymer matrix material and preparation method thereof
Technical field
The invention belongs to the material engineering field, be specifically related to a kind of tungsten-high molecular polymer matrix material and preparation method thereof.
Background technology
The reactor of nuclear power plant is a huge radioactive source; When fuel fission, can produce neutron and gamma-radiation; The activation products that fissium that fission reaction produces and priming reaction produce also can produce α, β and gamma-radiation when decaying, and therefore, the Nuclear power plants facility has very big potentially dangerous property; Must carry out radiation shielding to it, to avoid the generation of various possibility accidents.Simultaneously, the processing of nuke rubbish is also most important.Low-activity nuke rubbish and high radioactive nucleus waste were two types during usually said nuke rubbish comprised; The former refers to mainly that Nuclear power plants produces in power generation process has radioactive waste liquid, refuse; 99% of all nuke rubbish have been accounted for; The latter then is meant the nuclear fuel after the burning that from nuclear power plant reactor core, swaps out, because it has the height radioactivity, being commonly called as is that height radiates waste material.When above nuke rubbish is carried out harmless treatment, also need carry out necessary radiation shielding and handle.
Mostly radiation shielding material is metallic lead in the prior art; Its shield effectiveness is good, cost is low and be easy to processing; Yet, plumbous own toxic, atmosphere pollution, water source and farm crop such as plumbiferous waste gas, waste water, waste residue; Can jeopardize near resident, it is imperative therefore to replace lead to be applied to the nuclear radiation shield field with other material.
Research shows that a kind of radiation protection ability of material is relevant with its ordination number and density of material, and ordination number is high more, density of material is big more, and then shielding properties is good more.The ordination number of tungsten is 74, and density is 19.35g/cm 3, have good beta ray shield performance, be the choosing that is used for doing the best of shielding material, but tungsten is the HMP refractory metal, its shaping processing difficulties is easy to receive shape limits when using.Being matrix with the polymkeric substance in the prior art, is that filler prepares high density tungsten-polymer composites and solves the problems referred to above with the tungsten powder, and patent US5001354 is that the surgical glove of feedstock production has shielding property with nature rubber latex and tungsten powder.Patent US7304105B2 produces a kind of radioprotective matrix material with the tungsten powder filled elastomer of different-grain diameter; This material has good snappiness and processing characteristics; But the tungsten powder that needs three kinds of different-grain diameters is arranged in pairs or groups mutually and is improved the tonburden of tungsten, and ME is complicated.Employed tungsten powder normally makes through traditional grinding techniques such as ball millings in the prior art; The tungsten powder particles serious agglomeration that makes like this; Out-of-shape, flowability and density are relatively poor, and the tonburden in matrix material is lower; Be not easy to homodisperse in macromolecule matrix, cause the matrix material physical and mechanical properties relatively poor.
Summary of the invention
The objective of the invention is to overcome the prior art defective, the good tungsten of a kind of physical and mechanical properties-high molecular polymer matrix material and preparation method thereof is provided.
Technical scheme of the present invention is following:
A kind of tungsten-high molecular polymer matrix material comprises the component of following weight part:
Figure BDA0000132113600000021
The diameter of said tungsten fiber is 10~30 μ m, and length-to-diameter ratio is 50~150.
Said tungsten powder is the Fisher particle size 0.4 μ m~a kind of tungsten powder of 60 μ m or the mixing of several kinds of tungsten powders.
Said high molecular polymer is one or more in plastics, the thermoplastic elastic body.
Said plastics comprise one or more in Vilaterm, Vestolen PP 7052, PS, SE, polymeric amide, polyimide, urethane, polymethylmethacrylate, polyethylene terephthalate, the acrylonitrile-styrene-butadienecopolymer.
Said rubber comprises one or more in tree elastomer, viton, Zylox, paracril, ethylene-propylene rubber(EPR), X 050, polyisoprene rubber, styrene-butadiene rubber(SBR), the cis-1,4-polybutadiene rubber.
In said thermoplastic elastic body styrene analog thermoplastic elastomer, olefin hydrocarbons thermoplasticity elastic body, diene analog thermoplastic elastomer, polyvinyl chloride-base thermoplastic elastomer, polyurethanes elastomerics, polyester elastomer, polyamide-based thermoplastic elastomer, fluorinated thermoplastic elastomer, the silicone based thermoplastic elastomer one or more.
Said coupling agent is one or more in silane coupling agent, titanate coupling agent or the rare-earth coupling agent.
Said other auxiliary agents are one or more in softening agent, anti-aging agent, fire retardant, anti UV agent, additional crosslinker, vulcanizing agent, the vulcanization accelerator.
A kind of method for preparing said tungsten-high molecular polymer matrix material is characterized in that: comprise the steps:
(1) tungsten powder is carried out comminution by gas stream;
(2) will in the tungsten powder of comminution by gas stream or this tungsten powder and tungsten fiber are mixing pot, constantly stir, and spray carries out surface-treated with the coupling agent of alcohol dilution;
(3) with high molecular polymer, through the mixture of the tungsten powder of surface-treated or this tungsten powder and tungsten fiber and other auxiliary agent according to above-mentioned weight part mix, kneading evenly makes feeding;
(4) be shaped: feeding is passed through the forcing machine extrusion molding, or through the injector injection forming, or through the pressure forming machine die forming;
(5) aftertreatment: resulting product is cut out, chamfered.
The invention has the beneficial effects as follows:
1, matrix material of the present invention is made up of the component of following weight proportion: high molecular polymer 20~100, tungsten powder 950~1000, tungsten fiber 0~50, coupling agent 0.5~5 and other auxiliary agents 0.5~10; Compared with prior art; Except having good snappiness and the processing characteristics; Because the content of tungsten is very high thereby have good beta ray shield performance, make matrix material of the present invention have good physical strength and physicals owing to be added with tungsten fiber simultaneously in the matrix material of the present invention.
2, the used tungsten powder of matrix material of the present invention makes through comminution by gas stream and through surface-treated.Compared with prior art, gas flow crushing process is simple and efficient is high, greatly reduces the agglomeration of tungsten powder; Gained tungsten powder regular shape, good fluidity, further; Through surface-treated, make can better combine between tungsten powder and the macromolecule matrix, make it to be easy to homodisperse in macromolecule matrix; Tonburden is high, and the matrix material of the present invention that makes with this tungsten powder has good physical and mechanical properties.
3, be added with in softening agent, anti-aging agent, fire retardant, anti UV agent, additional crosslinker, vulcanizing agent, the vulcanization accelerator one or more in the matrix material of the present invention; Its weather resisteant, chemical resistant properties and organic solvent resistance are improved; Has very wide range of application; Not only can be applicable to the beta ray shield field, also can be applicable to fields such as vibration isolation, counterweight, thermal conduction, ordnance ammunition.
Embodiment
Followingly the present invention is further explained and describe according to specific embodiment.
Embodiment 1
High density tungsten-polymkeric substance beta ray shield composite-material formula is:
Figure BDA0000132113600000041
Figure BDA0000132113600000051
The preparation method of above-mentioned tungsten-high molecular polymer matrix material the steps include:
(1) take by weighing tungsten powder by above-mentioned weight part, tungsten powder is carried out comminution by gas stream, feed pressure 0.9MPa pulverizes pressure 1.1MPa.
(2) will in the doping pot, constantly stir through the tungsten powder of comminution by gas stream, and the titanate coupling agent that sprays with alcohol dilution carries out surface-treated;
(3) take by weighing other material according to above-mentioned weight part; Earlier styrene analog thermoplastic elastomer is added milling machine, drop into the above-mentioned tungsten powder of 500 weight parts then, will remain tungsten powder and anti-aging agent behind the kneading appropriate time and add; Kneading evenly makes feeding, and above-mentioned kneading temperature is 140 ℃.
(4) be shaped: extrude adding in the forcing machine 210 ℃ after the feeding granulation, cooling makes belt product.
(5) aftertreatment: resulting product is cut out, chamfered.
Embodiment 2
High density tungsten-polymkeric substance beta ray shield composite-material formula is:
Figure BDA0000132113600000052
Figure BDA0000132113600000061
The preparation method of above-mentioned tungsten-high molecular polymer matrix material the steps include:
(1) take by weighing tungsten powder by above-mentioned weight part, tungsten powder is carried out comminution by gas stream, feed pressure 0.8MPa pulverizes pressure 1.0MPa.
(2) will in the doping pot, constantly stir through the tungsten powder of comminution by gas stream, and the silane coupling agent that sprays with alcohol dilution carries out surface-treated;
(3) take by weighing other material according to above-mentioned weight part; Earlier terpolymer EP rubber is added milling machine; Drop into the above-mentioned tungsten powder of 500 weight parts then, behind 120 ℃ of kneading appropriate times, all leftover materials except that vulcanizing agent are added successively, mixing even back discharging; In mill, add vulcanizing agent at last, mixing even back slice makes feeding.
(4) be shaped: feeding 170 ℃ of sulfurations on rubber plate vulcanization machine are made sheet-like article.
(5) aftertreatment: resulting product is cut out, chamfered.
Embodiment 3
High density tungsten-polymkeric substance beta ray shield composite-material formula is:
Figure BDA0000132113600000062
Figure BDA0000132113600000071
The preparation method of above-mentioned tungsten-high molecular polymer matrix material the steps include:
(1) take by weighing tungsten powder by above-mentioned weight part, tungsten powder is carried out comminution by gas stream, feed pressure 0.9MPa pulverizes pressure 1.0MPa.
(2) will in the doping pot, constantly stir through the tungsten powder and the tungsten fiber of comminution by gas stream, and the rare-earth coupling agent that sprays with alcohol dilution carries out surface-treated;
(3) take by weighing other material according to above-mentioned weight part; Earlier tree elastomer is added milling machine; Add the above-mentioned tungsten powder of styrene-butadiene rubber(SBR) and 500 weight parts and the mixture of tungsten fiber then; Behind 80 ℃ of kneading appropriate times, all leftover materials except that vulcanizing agent are added successively, mixing even back discharging, dump temperature is lower than 130 ℃.In mill, add vulcanizing agent at last, mixing even back slice makes feeding.
(4) be shaped: feeding 150 ℃ of sulfurations on rubber plate vulcanization machine are made sheet-like article.
(5) aftertreatment: resulting product is cut out, chamfered.
Embodiment 4
High density tungsten-polymkeric substance beta ray shield composite-material formula is:
Figure BDA0000132113600000072
Figure BDA0000132113600000081
The preparation method of above-mentioned tungsten-high molecular polymer matrix material the steps include:
(1) take by weighing tungsten powder by above-mentioned weight part, tungsten powder is carried out comminution by gas stream, feed pressure 1.0MPa pulverizes pressure 1.1MPa.
(2) will in the doping pot, constantly stir through the tungsten powder of comminution by gas stream, and the titanate coupling agent that sprays with alcohol dilution carries out surface-treated;
(3) take by weighing other material according to above-mentioned weight part, earlier nylon 6 is added milling machine, drop into the above-mentioned tungsten powder of 500 weight parts then, will remain tungsten powder and anti-aging agent behind the kneading appropriate time and add, kneading evenly makes feeding, and above-mentioned kneading temperature is 230 ℃.
(4) be shaped: with after the feeding granulation on injector 240 ℃ of injection formings make abnormal member.
(5) aftertreatment: resulting product is cut out, chamfered.
Embodiment 5
High density tungsten-polymkeric substance beta ray shield composite-material formula is:
The preparation method of above-mentioned tungsten-high molecular polymer matrix material the steps include:
(1) take by weighing tungsten powder by above-mentioned weight part, tungsten powder is carried out comminution by gas stream, feed pressure 0.9MPa pulverizes pressure 0.9MPa.
(2) will in the doping pot, constantly stir through the tungsten powder of comminution by gas stream, and the titanate coupling agent that sprays with alcohol dilution carries out surface-treated;
(3) take by weighing other material according to above-mentioned weight part; Earlier Zylox is added milling machine, add the above-mentioned tungsten powder of 500 weight parts then, behind 40 ℃ of kneading appropriate times, all leftover materials except that vulcanizing agent are added successively; Mixing even back discharging, dump temperature is lower than 50 ℃; Mixing materials is naturally cooled to room temperature, places baking oven then in 140 ℃ of following insulation 2h, take out and naturally cooling after, back mixing and to add vulcanizing agent mixing evenly in mill, age overnight then, back mixing again, slice make feeding.
(4) be shaped: feeding 200 ℃ of sulfurations on rubber plate vulcanization machine are made sheet-like article.
(5) aftertreatment: resulting product is cut out, chamfered.
Embodiment 6
High density tungsten-polymkeric substance beta ray shield composite-material formula is:
Figure BDA0000132113600000091
The preparation method of above-mentioned tungsten-high molecular polymer matrix material the steps include:
(1) take by weighing tungsten powder by above-mentioned weight part, tungsten powder is carried out comminution by gas stream, feed pressure 0.9MPa pulverizes pressure 1.1MPa.
(2) will in the doping pot, constantly stir through the tungsten powder of comminution by gas stream, and the titanate coupling agent that sprays with alcohol dilution carries out surface-treated;
(3) take by weighing other material according to above-mentioned weight part; Earlier olefin hydrocarbons thermoplasticity elastic body is added milling machine, drop into the above-mentioned tungsten powder of 500 weight parts then, will remain tungsten powder and anti-aging agent behind the kneading appropriate time and add; Kneading evenly makes feeding, and above-mentioned kneading temperature is 140 ℃.
(4) be shaped: extrude adding in the forcing machine 200 ℃ after the feeding granulation, cooling makes rod-shaped products.
(5) aftertreatment: resulting product is cut out.
Embodiment 7
High density tungsten-polymkeric substance beta ray shield composite-material formula is:
Figure BDA0000132113600000101
The preparation method of above-mentioned tungsten-high molecular polymer matrix material the steps include:
(1) take by weighing tungsten powder by above-mentioned weight part, tungsten powder is carried out comminution by gas stream, feed pressure 1.0MPa pulverizes pressure 1.0MPa.
(2) will in the doping pot, constantly stir through the tungsten powder and the tungsten fiber of comminution by gas stream, and the titanate coupling agent that sprays with alcohol dilution carries out surface-treated;
(3) take by weighing other material according to above-mentioned weight part; Earlier styrene analog thermoplastic elastomer is added milling machine; Drop into the above-mentioned tungsten powder of 500 weight parts and the mixture of tungsten fiber then; The mixture and the anti-aging agent that will remain tungsten powder and tungsten fiber behind the kneading appropriate time add, and kneading evenly makes feeding, and above-mentioned kneading temperature is 140 ℃.
(4) be shaped: extrude adding in the forcing machine 210 ℃ after the feeding granulation, cooling makes tubular body.
(5) aftertreatment: resulting product is cut out.
Embodiment 8
High density tungsten-polymkeric substance beta ray shield composite-material formula is:
Figure BDA0000132113600000111
The preparation method of above-mentioned tungsten-high molecular polymer matrix material the steps include:
(1) take by weighing tungsten powder by above-mentioned weight part, tungsten powder is carried out comminution by gas stream, feed pressure 1.0MPa pulverizes pressure 1.0MPa.
(2) will in the doping pot, constantly stir through the tungsten powder of comminution by gas stream, and the silane coupling agent and the titanate coupling agent that spray with alcohol dilution carry out surface-treated;
(3) take by weighing other material according to above-mentioned weight part; Earlier styrene analog thermoplastic elastomer and Vestolen PP 7052 are added milling machine, drop into the above-mentioned tungsten powder of 500 weight parts then, will remain tungsten powder and anti-aging agent behind the kneading appropriate time and add; Kneading evenly makes feeding, and above-mentioned kneading temperature is 180 ℃.
(4) be shaped: extrude adding in the forcing machine 210 ℃ after the feeding granulation, cooling makes belt product.
(5) aftertreatment: resulting product is cut out, chamfered.
The above is merely preferred embodiment of the present invention, so can not limit the scope that the present invention implements according to this, the equivalence of promptly doing according to claim of the present invention and description changes and modifies, and all should still belong in the scope that the present invention contains.

Claims (10)

1. tungsten-high molecular polymer matrix material is characterized in that: the component that comprises following weight part:
2. a kind of tungsten as claimed in claim 1-high molecular polymer matrix material is characterized in that: the diameter of said tungsten fiber is 10~30 μ m, and length-to-diameter ratio is 50~150.
3. a kind of tungsten as claimed in claim 2-high molecular polymer matrix material is characterized in that: said tungsten powder is the Fisher particle size 0.4 μ m~a kind of tungsten powder of 60 μ m or the mixture of several kinds of tungsten powders.
4. like the described a kind of tungsten of arbitrary claim in the claim 1 to 3-high molecular polymer matrix material, it is characterized in that: said high molecular polymer is one or more in plastics, the thermoplastic elastic body.
5. a kind of tungsten as claimed in claim 4-high molecular polymer matrix material, it is characterized in that: said plastics comprise one or more in Vilaterm, Vestolen PP 7052, PS, SE, polymeric amide, polyimide, urethane, polymethylmethacrylate, polyethylene terephthalate, the acrylonitrile-styrene-butadienecopolymer.
6. a kind of tungsten as claimed in claim 4-high molecular polymer matrix material, it is characterized in that: said rubber comprises one or more in tree elastomer, viton, Zylox, paracril, ethylene-propylene rubber(EPR), X 050, polyisoprene rubber, styrene-butadiene rubber(SBR), the cis-1,4-polybutadiene rubber.
7. a kind of tungsten as claimed in claim 4-high molecular polymer matrix material is characterized in that: said thermoplastic elastomer comprises one or more in styrene analog thermoplastic elastomer, olefin hydrocarbons thermoplasticity elastic body, diene analog thermoplastic elastomer, polyvinyl chloride-base thermoplastic elastomer, polyurethanes elastomerics, polyester elastomer, polyamide-based thermoplastic elastomer, fluorinated thermoplastic elastomer, the silicone based thermoplastic elastomer.
8. like the described a kind of tungsten of arbitrary claim in the claim 1 to 3-high molecular polymer matrix material, it is characterized in that: said coupling agent is one or more in silane coupling agent, titanate coupling agent or the rare-earth coupling agent.
9. like the described a kind of tungsten of arbitrary claim in the claim 1 to 3-high molecular polymer matrix material, it is characterized in that: said other auxiliary agents are one or more in softening agent, anti-aging agent, fire retardant, anti UV agent, additional crosslinker, vulcanizing agent, the vulcanization accelerator.
10. a method for preparing the described a kind of tungsten of arbitrary claim-high molecular polymer matrix material in the claim 1 to 3 is characterized in that: comprise the steps:
(1) tungsten powder is carried out comminution by gas stream;
(2) will in the tungsten powder of comminution by gas stream or this tungsten powder and tungsten fiber are mixing pot, constantly stir, and spray carries out surface-treated with the coupling agent of alcohol dilution;
(3) with high molecular polymer, through the mixture of the tungsten powder of surface-treated or this tungsten powder and tungsten fiber and other auxiliary agent according to above-mentioned weight part mix, kneading evenly makes feeding;
(4) be shaped: feeding is passed through the forcing machine extrusion molding, or through the injector injection forming, or through the compression molding press die forming;
(5) aftertreatment: resulting product is cut out, chamfered.
CN2012100161038A 2012-01-18 2012-01-18 Tungsten-polymer composite material and preparation method thereof Pending CN102585330A (en)

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