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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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
tungsten powder
rubber
thermoplastic elastomer
polymer
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于洋
宋久鹏
庄志刚
杨福民
赖亚洲
赵国璋
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厦门虹鹭钨钼工业有限公司
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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
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/06Elements

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

一种铭一高分子聚合物复合材料及其制备方法 Ming composite material and method for preparing a polymer

技术领域 FIELD

[0001] 本发明属于材料工程领域,具体涉及一种钨-高分子聚合物复合材料及其制备方法。 [0001] The present invention belongs to the field of materials engineering, in particular to tungsten - composite material and method for preparing polymers.

背景技术 Background technique

[0002] 核电厂的反应堆是一个巨大的放射源,在核燃料裂变时会产生中子和Y辐射,裂变反应产生的裂变产物和活化反应产生的活化产物衰变时也会产生a、0和Y辐射,因此,核电站设施具有很大的潜在危险性,必须对其进行辐射屏蔽,以避免各种可能事故的发生。 Reactor [0002] The nuclear power plant is a huge radiation source, when the nuclear fuel and fission neutron radiation Y, activation products and fission products of the activation reaction fission reaction also yields a, 0, and Y radiation decay Therefore, nuclear power plant facility has great potential danger, it must be a radiation shield to avoid all possible accidents. 同时,核废料的处理也至关重要。 Meanwhile, the disposal of nuclear waste is also crucial. 通常所说的核废料包括中低放射性核废料和高放射性核废料两类,前者主要指核电站在发电过程中产生的具有放射性的废液、废物,占到了所有核废料的99%,后者则是指从核电站反应堆芯中换出来的燃烧后的核燃料,因为其具有高度放射性,俗称为高放射废料。 Commonly referred to as nuclear waste comprises radioactive nuclear waste of low and high level radioactive nuclear waste categories, the former mainly refers to nuclear power generation during power generation of radioactive waste, waste, accounting for 99% of all nuclear waste, the latter refers to a change from the nuclear reactor core of the nuclear fuel after combustion, because of its highly radioactive, commonly known as a high radiation waste. 在对以上核废料进行无害化处理时,也需要进行必要的辐射屏蔽处理。 When the above sound processing nuclear waste, but also requires the necessary radiation shielding process.

[0003] 现有技术中射线屏蔽材料多为金属铅,其屏蔽效果好、成本低且易于加工,然而, 铅本身有毒性,含铅的废气、废水、废渣等污染大气、水源和农作物,可危及附近居民,因此以其它材料代替铅应用于核辐射屏蔽领域势在必行。 [0003] In the prior art multi-ray-shielding material is a metal of lead, the shielding effect is good, low cost and ease of processing, however, lead itself toxic, lead-containing waste gas, waste water, waste air pollution, water and crops, can endanger nearby residents, so instead of lead material applied to other fields of nuclear radiation shielding imperative.

[0004] 研究表明,一种物质的防辐射能力与其原子序数及材料密度有关,原子序数越高、 材料密度越大,则屏蔽性能越好。 [0004] Studies have shown that the ability of a substance to its radiation and the atomic number density of the material, the higher the atomic number, the greater the density of the material, the better the shielding properties. 钨的原子序数为74,密度为19. 35g/cm3,具有良好的射线屏蔽性能,是用来做屏蔽材料的最佳之选,但钨为高熔点难熔金属,其成形加工困难,在应用时易于受到形状限制。 Tungsten atomic number of 74, a density of 19. 35g / cm3, having a good radiation shielding performance, is used to make the best choice of shielding material, but the high-melting refractory metal is tungsten, forming processing difficulties which, in the application when susceptible shape restricted. 现有技术中以聚合物为基体,以钨粉为填料制备高密度钨-聚合物复合材料来解决上述问题,专利US5001354以天然橡胶乳液及钨粉为原料制备的外科手套具有防辐射性能。 In the prior art polymer matrix to tungsten powder to prepare a high-density tungsten filler - polymer composites to solve the above problems, Patent US5001354 natural rubber latex surgical glove, and tungsten powder is prepared starting materials having radiation properties. 专利US7304105B2以不同粒径的钨粉填充弹性体而生产出一种防辐射复合材料,该材料具有良好的柔韧性及加工性能,但需要三种不同粒径的钨粉互相搭配来提高钨的装载量,制造工艺复杂。 Patent US7304105B2 tungsten powder filled elastomers of different diameters of the radiation to produce a composite material, the material has good workability and flexibility, but requires three different particle size tungsten powder with each other to increase the loading of tungsten the amount of manufacturing process is complicated. 现有技术中所使用的钨粉通常是通过球磨等传统研磨技术制得的,这样制得的钨粉颗粒团聚严重,形状不规则,流动性和密实性较差,在复合材料中的装载量较低,不易于在高分子基体中均匀分散,导致复合材料物理机械性能较差。 The tungsten powder used in the prior art usually by conventional ball milling techniques and the like made of tungsten powder thus obtained severe particle agglomeration, irregular shape, flowability and compactibility is poor, loading the composite material low, is not easy to uniformly in the polymer matrix dispersion, resulting in poor mechanical properties of the composite material.

发明内容 SUMMARY

[0005] 本发明的目的在于克服现有技术缺陷,提供一种物理机械性能好的钨-高分子聚合物复合材料及其制备方法。 [0005] The object of the present invention is to overcome defects in the prior art, to provide a good physical and mechanical properties of tungsten - polymer composite material and its preparation method.

[0006] 本发明的技术方案如下: [0006] aspect of the present invention is as follows:

[0007] —种钨-高分子聚合物复合材料,包括以下重量份的组分: [0007] - Species tungsten - polymer composites, parts by weight of component comprising:

[0008]高分子聚合物 20〜100 [0008] The polymers 20-100

钨粉 950〜1000 Tungsten powder 950~1000

钨纤维 0〜50 Tungsten fibers 0~50

偶联剂 0.5〜5 Coupling 0.5~5

其他助剂 0.5〜IO。 Other additives 0.5~IO.

[0009] 所述钨纤维的直径为10〜30 ii m,长径比为50〜150。 [0009] The diameter of the tungsten fibers have 10~30 ii m, an aspect ratio of 50~150.

[0010] 所述钨粉为费氏粒度0. 4 m〜60 m的一种钨粉或几种钨粉的混合。 [0010] A mixture of the tungsten powder particle size is Fisher 0. 4 m~60 m or more of tungsten powder, tungsten powder.

[0011] 所述高分子聚合物为塑料、橡胶或热塑性弹性体中的一种或几种。 [0011] The one or more polymers as plastic, rubber or thermoplastic elastomer.

[0012] 所述塑料包括聚乙烯、聚丙烯、聚苯乙烯、聚氯乙烯、聚酰胺、聚酰亚胺、聚氨酯、聚甲基丙烯酸甲酯、聚对苯二甲酸乙二醇酯、丙烯腈-苯乙烯-丁二烯共聚物中的一种或几种。 [0012] The plastics include polyethylene, polypropylene, polystyrene, polyvinyl chloride, polyamide, polyimide, polyurethane, polymethyl methacrylate, polyethylene terephthalate, acrylonitrile - styrene - butadiene copolymer of one or more.

[0013] 所述橡胶包括天然橡胶、氟橡胶、硅橡胶、丁腈橡胶、乙丙橡胶、氯丁橡胶、异戊橡胶、丁苯橡胶、顺丁橡胶中的一种或几种。 [0013] The rubber include natural rubber, fluorine rubber, silicone rubber, nitrile rubber, ethylene propylene rubber, chloroprene rubber, isoprene rubber, styrene-butadiene rubber, butadiene rubber of one or more.

[0014] 所述热塑性弹性体苯乙烯类热塑性弹性体、烯烃类热塑性弹性体、双烯类热塑性弹性体、氯乙烯类热塑性弹性体、聚氨酯类弹性体、聚酯类弹性体、聚酰胺类热塑性弹性体、 含氟类热塑性弹性体、有机硅类热塑性弹性体中的一种或几种。 [0014] The thermoplastic elastomer of the styrene-based thermoplastic elastomer, olefin-based thermoplastic elastomer, diene-based thermoplastic elastomer, a vinyl chloride-based thermoplastic elastomer, polyurethane elastomer, polyester elastomer, polyamide-based thermoplastic one or more elastomers, fluorine-based thermoplastic elastomer, a silicone-based thermoplastic elastomer.

[0015] 所述偶联剂为硅烷偶联剂、钛酸酯偶联剂或稀土偶联剂中的一种或几种。 [0015] The coupling agent is a silane coupling agent, a titanate coupling agent or a rare earth is one or more coupling agent.

[0016] 所述其他助剂为增塑剂、防老剂、阻燃剂、抗紫外线剂、助交联剂、硫化剂、硫化促进剂中的一种或几种。 The [0016] Other auxiliaries are plasticizers, one or more antioxidant, flame retardant, anti-UV agents, crosslinking agents, vulcanizing agents, vulcanization accelerators.

[0017] 一种制备所述钨-高分子聚合物复合材料的方法,其特征在于:包括如下步骤: [0017] A process for preparing the tungsten - high molecular polymer composite material, characterized by: comprising the steps of:

[0018] (I)将钨粉进行气流粉碎; [0018] (I) pulverized tungsten powder stream;

[0019] (2)将经气流粉碎的钨粉或该钨粉及钨纤维在掺杂锅中不断搅拌,并喷淋以乙醇稀释的偶联剂进行表面改性; [0019] (2) the gas stream through the pulverized tungsten powder or tungsten powder and tungsten-doped fiber continuously stirred pot, and diluted with ethanol to spray the surface modification of a coupling agent;

[0020] (3)将高分子聚合物、经表面改性的钨粉或该钨粉与钨纤维的混合物及其它助剂按照上述重量份混合、捏炼均匀制得喂料; [0020] (3) the polymers, surface-modified or a mixture of tungsten powder and tungsten powder and other additives which tungsten fibers mixed in the above parts by weight, uniform kneading prepared feed;

[0021] (4)成形:将喂料通过挤出机挤出成形,或通过注射机注射成形,或通过压力成型机模压成形; [0021] (4) Molding: The feed extrusion molding through an extruder, injection molding machine or by injection, or press molding by a press molding machine;

[0022] (5)后处理:将所得制品进行剪裁、去角。 [0022] (5) Post-treatment: The resulting article cropping, chamfered.

[0023] 本发明的有益效果是: [0023] Advantageous effects of the present invention are:

[0024] I、本发明的复合材料由以下重量配比的组分构成:高分子聚合物20〜100、钨粉950〜1000、钨纤维0〜50、偶联剂0. 5〜5及其他助剂0. 5〜10,与现有技术相比,除了具有良好的柔韧性和加工性能以外,本发明的复合材料中由于钨的含量很高因而具有很好的射线屏蔽性能,同时由于添加有钨纤维使得本发明的复合材料具有很好的机械强度和物理性能。 [0024] I, the composite material of the present invention the weight ratio of the components by the following composition: 20-100 polymers, 950~1000 tungsten powder, tungsten fibers 0~50, coupling agents and other 0. 5~5 0. 5 to 10 auxiliaries, compared to the prior art, in addition to having good flexibility and processing properties, the composite material of the present invention due to the high content of tungsten which has good radiation shielding properties, while the addition of tungsten fiber composite material such that the present invention has good mechanical strength and physical properties.

[0025] 2、本发明的复合材料所用钨粉通过气流粉碎并经表面改性制得。 [0025] 2, the composite material used in the present invention is tungsten powder and pulverized to obtain surface-modified by air. 与现有技术相比,气流粉碎工艺简单且效率高,大大降低了钨粉的团聚现象,所得钨粉形状规则,流动性好,进一步的,通过表面改性,使得钨粉与高分子基体之间能够更好的结合,使之易于在高分子基体中均匀分散,装载量高,用该钨粉制得的本发明的复合材料具有良好的物理机械性能。 Compared with the prior art, jet milling process is simple and efficient, significantly reducing the agglomeration of the tungsten powder, tungsten powder resulting regular shape, good fluidity, and further, the surface modification, so that the tungsten powder with the polymer matrix among the better binding, allowing easy in the polymer matrix uniformly dispersed, high loading, has good physical and mechanical properties of the composite material of the present invention, the tungsten powder was prepared.

[0026] 3、本发明的复合材料中添加有增塑剂、防老剂、阻燃剂、抗紫外线剂、助交联剂、 硫化剂、硫化促进剂中的一种或几种,使其耐侯性、耐化学性及耐有机溶剂性提高,具有很广的应用范围,不仅可应用于射线屏蔽领域,亦可应用于隔振、配重、热传导、军械弹药等领域。 [0026] 3, the composite material of the present invention, there is added a plasticizer, an antioxidant, a flame retardant, anti-UV agents, crosslinking agents, vulcanizing agent, vulcanization accelerator is one or more, it weather resistance, chemical resistance and improved resistance to organic solvents, having a wide range of applications, can be applied not only to the field of radiation shielding, isolation can also be applied, weight, thermal conductivity, ordnance ammunition art.

具体实施方式 Detailed ways

[0027] 以下根据具体实施例对本发明进行进一步的说明和描述。 [0027] Here will be further described and description of the invention According to a particular embodiment.

[0028] 实施例I [0028] Example I

[0029] 高密度钨-聚合物射线屏蔽复合材料配方为: [0029] The high density tungsten - polymer ray shielding composite formulation is:

[0030] [0030]

Figure CN102585330AD00061

[0031] [0031]

[0032] 上述钨-高分子聚合物复合材料的制备方法,其步骤为: [0032] The tungsten - preparation of the polymer composite material, comprising the steps of:

[0033] (I)按上述重量份称取钨粉,将钨粉进行气流粉碎,进料压力O. 9MPa,粉碎压力I. IMPa。 [0033] (I) by the above-described parts by weight of tungsten powder weighed, was jet milled tungsten powder, feed pressure O. 9MPa, pulverization pressure I. IMPa.

[0034] (2)将经气流粉碎的钨粉在掺杂锅中不断搅拌,并喷淋以乙醇稀释的钛酸酯偶联剂进行表面改性; [0034] (2) the gas stream through the pulverized-doped tungsten powder in a pot continuously stirred, and diluted with ethanol spray titanate coupling agents for surface modification;

[0035] (3)按照上述重量份称取其它物料,先将苯乙烯类热塑性弹性体加入捏炼机,然后投入500重量份的上述钨粉,捏炼适当时间后将剩余钨粉及防老剂加入,捏炼均匀制得喂料,上述捏炼温度为140°C。 [0035] (3) According to the above parts by weight of other materials weighed, the first styrene-based thermoplastic elastomer to a kneader, and then put into 500 parts by weight of the tungsten powder, kneading tungsten powder remaining after the appropriate time and antioxidant was added, to obtain a uniform feeding kneading the kneading temperature of 140 ° C.

[0036] (4)成形:将喂料造粒后加入挤出机中210 C挤出,冷却制得带状制品。 [0036] (4) Molding: The feed to the extruder after the extrusion granulation 210 C, cooled to obtain strip article.

[0037] (5)后处理:将所得制品进行剪裁、去角。 [0037] (5) Post-treatment: The resulting article cropping, chamfered.

[0038] 实施例2 [0038] Example 2

[0039] 高密度钨-聚合物射线屏蔽复合材料配方为: [0039] High density W - polymer ray shielding composite formulation is:

[0040] [0040]

Figure CN102585330AD00071

[0041] [0041]

[0042] 上述钨-高分子聚合物复合材料的制备方法,其步骤为: [0042] The tungsten - preparation of the polymer composite material, comprising the steps of:

[0043] (I)按上述重量份称取钨粉,将钨粉进行气流粉碎,进料压力0. 8MPa,粉碎压力I. OMPa。 [0043] (I) by the above-described parts by weight of tungsten powder weighed, was jet milled tungsten powder, a feed pressure of 0. 8MPa, pulverization pressure I. OMPa.

[0044] (2)将经气流粉碎的钨粉在掺杂锅中不断搅拌,并喷淋以乙醇稀释的硅烷偶联剂进行表面改性; [0044] (2) the gas stream through the pulverized-doped tungsten powder in a pot continuously stirred, and diluted with ethanol to spray the surface-modified silane coupling agent;

[0045] (3)按照上述重量份称取其它物料,先将三元乙丙橡胶加入捏炼机,然后投入500 重量份的上述钨粉,于120°C捏炼适当时间后将除硫化剂外的所有剩余物料依次加入,混炼均勾后出料,最后在开炼机上加入硫化剂,混炼均勾后出片制得喂料。 [0045] (3) According to the above referred to other materials taken parts by weight of EPDM rubber was added first a kneader, and then put into 500 parts by weight of the tungsten powder at 120 ° C after appropriate curing agent in addition to the kneading time All remaining outside the material added sequentially, after kneading the material are hook, and finally vulcanizing agent is added in the open roll, the kneaded sheet was prepared by feeding the hook.

[0046] (4)成形:将喂料在橡胶平板硫化机上170°C硫化制得片状制品。 [0046] (4) Molding: The feed in the flat vulcanized rubber vulcanization 170 ° C to obtain a sheet article.

[0047] (5)后处理:将所得制品进行剪裁、去角。 [0047] (5) Post-treatment: The resulting article cropping, chamfered.

[0048] 实施例3 [0048] Example 3

[0049] 高密度钨-聚合物射线屏蔽复合材料配方为: [0049] The high density tungsten - polymer ray shielding composite formulation is:

[0050] [0050]

Figure CN102585330AD00072
Figure CN102585330AD00081

[0052] 上述钨-高分子聚合物复合材料的制备方法,其步骤为: [0052] The tungsten - preparation of the polymer composite material, comprising the steps of:

[0053] (I)按上述重量份称取钨粉,将钨粉进行气流粉碎,进料压力0. 9MPa,粉碎压力I. OMPa。 [0053] (I) by the above-described parts by weight of tungsten powder weighed, was jet milled tungsten powder, a feed pressure of 0. 9MPa, pulverization pressure I. OMPa.

[0054] (2)将经气流粉碎的钨粉与钨纤维在掺杂锅中不断搅拌,并喷淋以乙醇稀释的稀土偶联剂进行表面改性; [0054] (2) by jet milling the tungsten powder and tungsten-doped fiber continuously stirred pot, and diluted with ethanol to spray the surface-modified rare earth coupling agent;

[0055] (3)按照上述重量份称取其它物料,先将天然橡胶加入捏炼机,然后加入丁苯橡胶及500重量份的上述钨粉与钨纤维的混合物,于80°C捏炼适当时间后将除硫化剂外的所有剩余物料依次加入,混炼均匀后出料,排胶温度低于130°C。 [0055] (3) According to the above parts by weight of other materials weighed, natural rubber was added first a kneader, and a mixture of styrene and 500 parts by weight of tungsten powder and the tungsten fibers, at 80 ° C suitable kneading after the remaining time of all materials except the vulcanizing agent were added, and kneaded uniformly discharge, discharge temperature below 130 ° C. 最后在开炼机上加入硫化剂,混炼均勾后出片制得喂料。 Finally, curatives were added on the open roll, the kneaded sheet was prepared by feeding the hook.

[0056] (4)成形:将喂料在橡胶平板硫化机上150°C硫化制得片状制品。 [0056] (4) Molding: The feed in the flat vulcanized rubber vulcanization 150 ° C to obtain a sheet article.

[0057] (5)后处理:将所得制品进行剪裁、去角。 [0057] (5) Post-treatment: The resulting article cropping, chamfered.

[0058] 实施例4 [0058] Example 4

[0059] 高密度钨-聚合物射线屏蔽复合材料配方为: [0059] The high density tungsten - polymer ray shielding composite formulation is:

[0060] [0060]

Figure CN102585330AD00082

[0061] [0061]

[0062] 上述钨-高分子聚合物复合材料的制备方法,其步骤为: [0062] The tungsten - preparation of the polymer composite material, comprising the steps of:

[0063] (I)按上述重量份称取钨粉,将钨粉进行气流粉碎,进料压力I. OMPa,粉碎压力I. IMPa。 [0063] (I) by the above-described parts by weight of tungsten powder weighed, was jet milled tungsten powder, feed pressure I. OMPa, pulverization pressure I. IMPa. [0064] (2)将经气流粉碎的钨粉在掺杂锅中不断搅拌,并喷淋以乙醇稀释的钛酸酯偶联剂进行表面改性; [0064] (2) the gas stream through the pulverized-doped tungsten powder in a pot continuously stirred, and diluted with ethanol spray titanate coupling agents for surface modification;

[0065] (3)按照上述重量份称取其它物料,先将尼龙6加入捏炼机,然后投入500重量份的上述钨粉,捏炼适当时间后将剩余钨粉及防老剂加入,捏炼均匀制得喂料,上述捏炼温度为230 0C o [0065] (3) According to the above parts by weight of other materials weighed, nylon 6 was added first a kneader, and then put into 500 parts by weight of the tungsten powder, kneading tungsten powder remaining after the appropriate time and the antioxidant is added, kneading obtain a uniform feeding the kneading temperature is 230 0C o

[0066] (4)成形:将喂料造粒后在注射机上240°C注射成形制得异型件。 [0066] (4) Molding: After feeding the granulated on an injection machine to obtain shaped member 240 ° C injection molding.

[0067] (5)后处理:将所得制品进行剪裁、去角。 [0067] (5) Post-treatment: The resulting article cropping, chamfered.

[0068] 实施例5 [0068] Example 5

[0069] 高密度钨-聚合物射线屏蔽复合材料配方为: [0069] The high density tungsten - polymer ray shielding composite formulation is:

[0070] [0070]

Figure CN102585330AD00091

[0071] 上述钨-高分子聚合物复合材料的制备方法,其步骤为: [0071] The tungsten - preparation of the polymer composite material, comprising the steps of:

[0072] (I)按上述重量份称取钨粉,将钨粉进行气流粉碎,进料压力0. 9MPa,粉碎压力0. 9MPa。 [0072] (I) by the above-described parts by weight of tungsten powder weighed, was jet milled tungsten powder, a feed pressure of 0. 9MPa, pulverization pressure 0. 9MPa.

[0073] (2)将经气流粉碎的钨粉在掺杂锅中不断搅拌,并喷淋以乙醇稀释的钛酸酯偶联剂进行表面改性; [0073] (2) the gas stream through the pulverized-doped tungsten powder in a pot continuously stirred, and diluted with ethanol spray titanate coupling agents for surface modification;

[0074] (3)按照上述重量份称取其它物料,先将硅橡胶加入捏炼机,然后加入500重量份上述钨粉,于40°C捏炼适当时间后将除硫化剂外的所有剩余物料依次加入,混炼均匀后出料,排胶温度低于50°C ;将混炼料自然冷却至室温,然后置于烘箱中于140°C下保温2h,取出并自然冷却后,在开炼机上返炼并加入硫化剂混炼均匀,然后停放过夜,再返炼、出片制得喂料。 [0074] (3) According to the above referred to other materials taken parts by weight, the silicone rubber was added first a kneader, followed by addition of 500 parts by weight of the tungsten powder, at 40 ° C after kneading appropriate time all remaining except the vulcanizing agent materials were added, and kneaded uniformly discharge, discharge temperature below 50 ° C; kneading the material allowed to cool to room temperature and then placed in an oven for 2h at 140 ° C, remove and cool naturally, in the open remill on the mill and adding a vulcanizing agent is mixed uniformly and then parked overnight, and then back to refining, to prepare a sheet feeder.

[0075] (4)成形:将喂料在橡胶平板硫化机上200°C硫化制得片状制品。 [0075] (4) Molding: The feed in the flat vulcanized rubber vulcanization 200 ° C to obtain a sheet article.

[0076] (5)后处理:将所得制品进行剪裁、去角。 [0076] (5) Post-treatment: The resulting article cropping, chamfered.

[0077] 实施例6 [0077] Example 6

[0078] 高密度钨-聚合物射线屏蔽复合材料配方为: [0078] The high density tungsten - polymer ray shielding composite formulation is:

[0079] [0079]

Figure CN102585330AD00101

[0080] 上述钨-高分子聚合物复合材料的制备方法,其步骤为: [0080] The tungsten - preparation of the polymer composite material, comprising the steps of:

[0081] (I)按上述重量份称取钨粉,将钨粉进行气流粉碎,进料压力0.9MPa,粉碎压力I. IMPa。 [0081] (I) by the above-described parts by weight of tungsten powder weighed, was jet milled tungsten powder, feed pressure 0.9MPa, pulverization pressure I. IMPa.

[0082] (2)将经气流粉碎的钨粉在掺杂锅中不断搅拌,并喷淋以乙醇稀释的钛酸酯偶联剂进行表面改性; [0082] (2) the gas stream through the pulverized-doped tungsten powder in a pot continuously stirred, and diluted with ethanol spray titanate coupling agents for surface modification;

[0083] (3)按照上述重量份称取其它物料,先将烯烃类热塑性弹性体加入捏炼机,然后投A 500重量份的上述钨粉,捏炼适当时间后将剩余钨粉及防老剂加入,捏炼均匀制得喂料, 上述捏炼温度为140°c。 [0083] (3) According to the above parts by weight of other materials weighed, the first olefin-based thermoplastic elastomer to a kneader, and 500 parts by weight A cast tungsten powder described above, after a suitable kneading time remaining tungsten powder and antioxidant was added, to obtain a uniform feeding kneading, the kneading temperature is above 140 ° c.

[0084] (4)成形:将喂料造粒后加入挤出机中200 C挤出,冷却制得棒状制品。 [0084] (4) forming: After the feed to the extruder pelletizing extruder 200 C, cooled to obtain a rod-shaped article.

[0085] (5)后处理:将所得制品进行剪裁。 [0085] (5) Post-treatment: The resulting article is clipped.

[0086] 实施例I [0086] Example I

[0087] 高密度钨-聚合物射线屏蔽复合材料配方为: [0087] High density W - polymer ray shielding composite formulation is:

[0088] [0088]

Figure CN102585330AD00102

[0089] 上述钨-高分子聚合物复合材料的制备方法,其步骤为: [0089] The tungsten - preparation of the polymer composite material, comprising the steps of:

[0090] (I)按上述重量份称取钨粉,将钨粉进行气流粉碎,进料压力I. OMPa,粉碎压力I. OMPa0 [0090] (I) by the above-described parts by weight of tungsten powder weighed, was jet milled tungsten powder, feed pressure I. OMPa, pulverization pressure I. OMPa0

[0091] (2)将经气流粉碎的钨粉与钨纤维在掺杂锅中不断搅拌,并喷淋以乙醇稀释的钛酸酯偶联剂进行表面改性; [0091] (2) by jet milling the tungsten powder and tungsten-doped fiber continuously stirred pot, and diluted with ethanol spray titanate coupling agents for surface modification;

[0092] (3)按照上述重量份称取其它物料,先将苯乙烯类热塑性弹性体加入捏炼机,然后投入500重量份的上述钨粉与钨纤维的混合物,捏炼适当时间后将剩余钨粉与钨纤维的混合物及防老剂加入,捏炼均匀制得喂料,上述捏炼温度为140°C。 [0092] (3) According to the above parts by weight of other materials weighed, first a styrene based thermoplastic elastomer is added a kneader, 500 parts by weight of the mixture was then put in the tungsten powder and tungsten fibers, after a suitable kneading time remaining antioxidant mixture of tungsten powder and tungsten fibers added, to obtain a uniform feeding kneading the kneading temperature of 140 ° C.

[0093] (4)成形:将喂料造粒后加入挤出机中210 C挤出,冷却制得管状制品。 [0093] (4) Molding: The feed to the extruder after the extrusion granulation 210 C, cooled to obtain a tubular article.

[0094] (5)后处理:将所得制品进行剪裁。 [0094] (5) Post-treatment: The resulting article is clipped.

[0095] 实施例8 [0095] Example 8

[0096] 高密度钨-聚合物射线屏蔽复合材料配方为: [0096] High density W - polymer ray shielding composite formulation is:

[0097] [0097]

Figure CN102585330AD00111

[0098] 上述钨-高分子聚合物复合材料的制备方法,其步骤为: [0098] The tungsten - preparation of the polymer composite material, comprising the steps of:

[0099] (I)按上述重量份称取钨粉,将钨粉进行气流粉碎,进料压力I. OMPa,粉碎压力I. OMPa0 [0099] (I) by the above-described parts by weight of tungsten powder weighed, was jet milled tungsten powder, feed pressure I. OMPa, pulverization pressure I. OMPa0

[0100] (2)将经气流粉碎的钨粉在掺杂锅中不断搅拌,并喷淋以乙醇稀释的硅烷偶联剂及钛酸酯偶联剂进行表面改性; [0100] (2) the gas stream through the pulverized-doped tungsten powder in a pot continuously stirred, and diluted with ethanol to spray the silane coupling agent and a titanate coupling agent for surface modification;

[0101] (3)按照上述重量份称取其它物料,先将苯乙烯类热塑性弹性体及聚丙烯加入捏炼机,然后投入500重量份的上述钨粉,捏炼适当时间后将剩余钨粉及防老剂加入,捏炼均匀制得喂料,上述捏炼温度为180°C。 [0101] (3) According to the above referred to the other parts by weight of the material taken, first a styrene based thermoplastic elastomer and the polypropylene was added a kneader, and then put into 500 parts by weight of the tungsten powder, kneading the tungsten powder remaining after an appropriate time and the antioxidant was added, to obtain a uniform feeding kneading the kneading temperature of 180 ° C.

[0102] (4)成形:将喂料造粒后加入挤出机中210 C挤出,冷却制得带状制品。 [0102] (4) Molding: The feed to the extruder after the extrusion granulation 210 C, cooled to obtain strip article.

[0103] (5)后处理:将所得制品进行剪裁、去角。 [0103] (5) Post-treatment: The resulting article cropping, chamfered.

[0104] 以上所述,仅为本发明的较佳实施例而已,故不能依此限定本发明实施的范围,即依本发明专利范围及说明书内容所作的等效变化与修饰,皆应仍属本发明涵盖的范围内。 [0104] The above are only preferred embodiments of the present invention only, modifications and equivalent so it can not limit the scope of embodiments of the present invention, i.e., under this patent specification the content and scope of the invention is made, are still to be It encompassed within the scope of the present invention.

Claims (10)

1. 一种钨-高分子聚合物复合材料,其特征在于:包括以下重量份的组分:高分子聚合物 20〜100钨粉 950〜1000钨纤维 0〜50偶联剂 0.5〜5其他助剂 0.5〜IO。 A tungsten - polymer composites, characterized by: comprising the following parts by weight of component: 20-100 tungsten powder polymer fiber 950~1000 tungsten coupling 0.5~5 0~50 other co agent 0.5~IO.
2.如权利要求I所述的一种钨-高分子聚合物复合材料,其特征在于:所述钨纤维的直径为10〜30 μ m,长径比为50〜150。 2. tungsten claim I - polymer composites, characterized in that: the tungsten fibers have a diameter of 10~30 μ m, an aspect ratio of 50~150.
3.如权利要求2所述的一种钨-高分子聚合物复合材料,其特征在于:所述钨粉为费氏粒度O. 4 μ m〜60 μ m的一种钨粉或几种钨粉的混合物。 3. tungsten according to claim 2 - polymer composites, characterized in that: the tungsten powder as a particle size tungsten powder Fisher O. 4 μ m~60 μ m or more of tungsten powder mixture.
4.如权利要求I至3中任一权利要求所述的一种钨-高分子聚合物复合材料,其特征在于:所述高分子聚合物为塑料、橡胶或热塑性弹性体中的一种或几种。 The polymer is a plastic, rubber or a thermoplastic elastomer or: polymer composites, characterized in that - 4 I according to any one of claims 3 and tungsten claim several.
5.如权利要求4所述的一种钨-高分子聚合物复合材料,其特征在于:所述塑料包括聚乙烯、聚丙烯、聚苯乙烯、聚氯乙烯、聚酰胺、聚酰亚胺、聚氨酯、聚甲基丙烯酸甲酯、聚对苯二甲酸乙二醇酯、丙烯腈-苯乙烯-丁二烯共聚物中的一种或几种。 5. tungsten claimed in claim 4, wherein - polymer composites, characterized in that: said plastic include polyethylene, polypropylene, polystyrene, polyvinyl chloride, polyamide, polyimide, polyurethane, polymethyl methacrylate, polyethylene terephthalate, acrylonitrile - styrene - butadiene copolymer in one or more of.
6.如权利要求4所述的一种钨-高分子聚合物复合材料,其特征在于:所述橡胶包括天然橡胶、氟橡胶、硅橡胶、丁腈橡胶、乙丙橡胶、氯丁橡胶、异戊橡胶、丁苯橡胶、顺丁橡胶中的一种或几种。 6. tungsten claimed in claim 4, wherein - polymer composites, characterized in that: said rubber comprises natural rubber, fluorine rubber, silicone rubber, nitrile rubber, ethylene propylene rubber, chloroprene rubber, iso isoprene rubber, styrene-butadiene rubber, butadiene rubber of one or more.
7.如权利要求4所述的一种钨-高分子聚合物复合材料,其特征在于:所述热塑性弹性体包括苯乙烯类热塑性弹性体、烯烃类热塑性弹性体、双烯类热塑性弹性体、氯乙烯类热塑性弹性体、聚氨酯类弹性体、聚酯类弹性体、聚酰胺类热塑性弹性体、含氟类热塑性弹性体、有机硅类热塑性弹性体中的一种或几种。 7. tungsten claimed in claim 4, wherein - polymer composites, wherein: said thermoplastic elastomer comprises a styrene-based thermoplastic elastomer, olefin-based thermoplastic elastomer, diene-based thermoplastic elastomer, vinyl chloride-based thermoplastic elastomer, polyurethane elastomer, polyester elastomer, polyamide-based thermoplastic elastomer, fluorine-based thermoplastic elastomer, silicone-based thermoplastic elastomer is one or more.
8.如权利要求I至3中任一权利要求所述的一种钨-高分子聚合物复合材料,其特征在于:所述偶联剂为硅烷偶联剂、钛酸酯偶联剂或稀土偶联剂中的一种或几种。 The coupling agent is a silane coupling agent, a titanate coupling agent or RE: polymer composites, characterized in that - 8 I according to any one of claims 3 and tungsten claim one or more coupling agents.
9.如权利要求I至3中任一权利要求所述的一种钨-高分子聚合物复合材料,其特征在于:所述其他助剂为增塑剂、防老剂、阻燃剂、抗紫外线剂、助交联剂、硫化剂、硫化促进剂中的一种或几种。 I as claimed in claim 9 tungsten to 3 of any one of claims - polymer composites, characterized in that: the other auxiliaries are plasticizers, anti-aging agents, flame retardants, UV one or more agents, crosslinking agents, vulcanizing agents, vulcanization accelerators.
10. 一种制备权利要求I至3中任一权利要求所述的一种钨-高分子聚合物复合材料的方法,其特征在于:包括如下步骤:(1)将钨粉进行气流粉碎;(2)将经气流粉碎的钨粉或该钨粉及钨纤维在掺杂锅中不断搅拌,并喷淋以乙醇稀释的偶联剂进行表面改性;(3)将高分子聚合物、经表面改性的钨粉或该钨粉与钨纤维的混合物及其它助剂按照上述重量份混合、捏炼均匀制得喂料;(4)成形:将喂料通过挤出机挤出成形,或通过注射机注射成形,或通过压力成形机模压成形;(5)后处理:将所得制品进行剪裁、去角。 (; (1) was jet milled tungsten powder: comprising the steps of: high molecular polymer composite material, characterized in that - A tungsten-I according to claim any of claim 3 for preparing 2) the gas stream through the pulverized tungsten powder or tungsten powder and tungsten-doped fiber continuously stirred pot, and diluted with ethanol to spray the surface-modified coupling agent; (3) the polymer, the surface modified tungsten powder or the mixture of tungsten powder and tungsten fibers and other additives in accordance with the above-described parts by weight are mixed to obtain a uniform kneaded feeding; (4) molding: the feed extrusion molding through an extruder, or by injection molding machine injection, by means of a pressure molding machine or molding press; (5) post-treatment: the resulting article cropping, chamfered.
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