CN105837896A - Preparation method of ultra-high molecular weight polyethylene (UHMWPE) composite material - Google Patents

Preparation method of ultra-high molecular weight polyethylene (UHMWPE) composite material Download PDF

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CN105837896A
CN105837896A CN 201610247210 CN201610247210A CN105837896A CN 105837896 A CN105837896 A CN 105837896A CN 201610247210 CN201610247210 CN 201610247210 CN 201610247210 A CN201610247210 A CN 201610247210A CN 105837896 A CN105837896 A CN 105837896A
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composite material
molecular weight
uhmwpe
weight polyethylene
powder
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倪自丰
李广飞
陈国美
段为朋
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江南大学
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/24Crosslinking, e.g. vulcanising, of macromolecules
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/28Treatment by wave energy or particle radiation
    • 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
    • C08K3/04Carbon
    • 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
    • C08K5/04Oxygen-containing compounds
    • C08K5/15Heterocyclic compounds having oxygen in the ring
    • C08K5/151Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
    • C08K5/1545Six-membered rings
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G
    • C08J2323/00Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/04Homopolymers or copolymers of ethene
    • C08J2323/06Polyethene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00Properties characterising the ingredient of the composition
    • C08L2207/06Properties of polyethylene
    • C08L2207/068Ultra high molecular weight polyethylene

Abstract

The invention relates to a preparation method of an ultra-high molecular weight polyethylene (UHMWPE) composite material, belonging to the technical field of high-polymer materials. The preparation method comprises the following steps: by using medical UHMWPE powder as a base material, compositely adding natural vitamin-E (VE) and single-layer graphene oxide (GO) to prepare mixed powder, adding the mixed powder into a mold, carrying out hot pressing to prepare a UHMWPE/GO-VE composite material; and carrying out gamma-ray irradiation crosslinking treatment to finally obtain the oxidation-resistant ultra-low-abrasion UHMWPE composite material. The gamma-ray irradiation crosslinking UHMWPE/GO-VE composite material has excellent wear resistance. The two-dimensional-structure GO with excellent mechanical properties and biocompatibility can lower the abrasion, thereby reducing the abrasive dust quantity and lowering the cell untoward effect degree caused by abrasive dust. The composite material has excellent oxidation resistance and aging resistance.

Description

一种超高分子量聚乙烯复合材料的制备方法 A process for producing a composite material of ultrahigh molecular weight polyethylene

技术领域 FIELD

[0001]本发明涉及一种超高分子量聚乙烯复合材料的制备方法,属于高分子材料技术领域。 [0001] The present invention relates to a method for preparing a composite ultrahigh molecular weight polyethylene, it belongs to the technical field of polymer materials.

背景技术 Background technique

[0002]医用超高分子量聚乙烯(英文名称缩写:UHMWPE)是目前广泛采用的髋关节臼材料。 [0002] The medical ultrahigh molecular weight polyethylene (abbreviated English name: UHMWPE) is a hip acetabular materials are currently widely used. 目前,应用于临床的超高分子量聚乙烯复合材料主要是辐照交联VE/UHMWPE复合材料,然而,VE的加入降低了复合材料的交联度,从而降低了复合材料的耐磨粒磨损的性能。 Currently, clinical application of ultra high molecular weight polyethylene composite mainly irradiation crosslinked VE / UHMWPE composite, however, VE is added to reduce the degree of crosslinking of the composite material, thereby reducing the composites Abrasive wear performance. 此外复合材料的力学性能相较于纯UHMffPE有待进一步提高,因此进一步提高其在力学与耐磨方面的性能,对医疗应用有重大的意义。 Also mechanical properties of composites compared to the pure UHMffPE be further improved, thus further improving its performance in terms of mechanics and wear, has great significance for medical applications.

发明内容 SUMMARY

[0003]本发明的目的在于克服上述不足之处,提供一种具有优良的力学性能、抗氧化超低磨损超高分子量聚乙稀复合材料。 [0003] The object of the present invention is to overcome the above disadvantages, to provide a good mechanical properties, oxidation ultra low wear composite ultrahigh molecular weight polyethylene.

[0004]按照本发明提供的技术方案,一种超高分子量聚乙烯复合材料的制备方法,按重量份计步骤为: [0004] according to the aspect of the present invention provides a method for preparing ultra high molecular weight polyethylene composite material, parts by weight by the steps of:

(1)混合粉末的制备:将单层氧化石墨烯GO和维生素-E加入到溶剂中充分搅拌分散后经超声处理,再加入超高分子量聚乙烯UHMffPE粉末磁力搅拌分散,再次超声处理,经超声剥离得到粉末,然后进行球磨混合,形成均匀的三体混合粉末; Preparation of mixed powder (1): GO monolayer graphene oxide and Vitamin -E added to the solvent and stirred fully by ultrasonic dispersion treatment, adding high molecular weight polyethylene powder magnetic stirring UHMffPE dispersed again sonicated by ultrasound peeled to obtain a powder, and then a ball mill mixing, to form a uniform three mixed powder;

(2)成型:将步骤(I)所得混合粉末添加到模具中,采用平板硫化机在预压,然后在保温箱中保温,再采用平板硫化机在压模处理得到板材,冷却至室温; (2) Molding: The addition step (I) the resulting mixed powder in a mold using vulcanizing machine in the pre-press, and then incubated in an incubator, and then employed in the vulcanizing machine to obtain a stamper plate, cooled to room temperature;

(3)辐照:将步骤(3)所得的复合材料0.5-0.9MPa真空密封,然后在室温下,采用γ-射线进行辐照交联处理,辐照量为10kGy,辐照的剂量率为5kGyh—1,γ -射线原材用60Co,最终得到超高分子量聚乙稀复合材料。 (3) Irradiation: The step (3) the resulting composite material 0.5-0.9MPa vacuum sealed, and then at room temperature using γ- rays irradiation crosslinking, in an amount of 10 kGy irradiation, radiation dose rate 5kGyh-1, γ - ray raw materials with 60Co, the finally obtained ultra high molecular weight polyethylene composite.

[0005] 所述维生素E的纯度为VE > 98%,粒径小于ΙΟΟμπι。 Purity of [0005] Vitamin E for VE> 98%, particle size less than ΙΟΟμπι.

[0006] 所述超高分子量聚乙烯UHMWPE粉末的粒径范围为4.3-200μπι。 The [0006] UHMWPE UHMWPE powder size range 4.3-200μπι.

[0007]所述超高分子量聚乙烯复合材料的制备方法,具体步骤如下: [0007] The method for preparing ultra high molecular weight polyethylene composite material, the following steps:

(1)混合粉末的制备:将0.3-0.7份的单层氧化石墨烯GO和0.1-0.3份的维生素-E粉末加入到500份溶剂中充分搅拌分散,然后再以200-4001超声处理0.5-211;将99-99.6份的超高分子量聚乙烯粉末UHMWPE加入到上述溶液中,将混合物经磁力搅拌30-90min后再次200-400W超声剥离0.5-2h;将所得混合物置于球磨机中研磨混合2-4h; Preparation of mixed powder (1): 0.3 to 0.7 parts of a single layer of graphene oxide GO and 0.1 to 0.3 parts of Vitamin -E powder is added to 500 parts of a solvent dispersion sufficiently stirred and then sonicated to 200-4001 0.5 211; 99-99.6 parts of the ultrahigh molecular weight polyethylene UHMWPE powder is added to the solution, and the mixture was stirred again 200-400W ultrasonic peeling was magnetically 0.5-2h after 30-90 min; the resulting mixture was placed in a ball mill and mixed for 2 -4h;

将研磨后的混合物置于60-80 0C水浴中干燥,在60-80 °C下保温至其完全干燥;再次置于球磨机中研磨粉碎,以300_600r/min的转速粉碎2_4h; The milled mixture was placed in a water bath at 60-80 0C and dried, incubated at 60-80 ° C until completely dry; again placed in a ball mill grind at a rotation speed 300_600r / min pulverized 2_4h;

(2)成型:将10g的步骤(I)所得混合粉末添加到模具中,采用平板硫化机在10-15MPa压力下预压10_15min,然后在保温箱中180-200°C保温2-3h,再采用平板硫化机在15-20MPa压强下压模处理15_20min得到复合材料板材,冷却至室温; (3)辐照:将步骤(3)所得的复合材料真空密封;然后在室温下,采用γ-射线进行辐照交联处理,辐照时间为9-12天,最终得到产品超高分子量聚乙烯复合材料。 (2) Molding: The resulting mixed powder addition step (I) 10g of a mold using vulcanizing press at a pressure of 10-15MPa preloading 10_15min, and 180-200 ° C in an incubator incubated 2-3h, then using vulcanizing press at a pressure of 15-20MPa stamper process 15_20min composite laminate obtained was cooled to room temperature; (3) exposure: the step (3) vacuum sealing the resulting composite material; and then at room temperature using γ- rays irradiation crosslinking, the irradiation time is 9-12 days, to give the final product UHMWPE composite.

[0008] 步骤(I)所述溶剂为无水乙醇或丙酮。 [0008] Step (I) the solvent is ethanol or acetone.

[0009] 采用γ -射线进行辐照交联处理时,辐照量为10kGy,辐照的剂量率为5kGyh—1,γ -射线原材用60Co。 [0009] The γ - ray irradiation during the crosslinking treatment, the irradiation amount is 10 kGy, the dose rate irradiation 5kGyh-1, γ - ray original timber 60Co.

[0010]本发明的有益效果:本发明选用医用超高分子量聚乙烯UHMWPE粉末为基础材料,并对其复合添加维生素Ve和氧化石墨烯,充分利用了维生素-E和氧化石墨烯的优良品质,既增加了UHMWPE的抗氧化性和生物相容性,又增加了UHMWPE的耐磨性等力学性能,最终得到具有优良力学性能、抗氧化超低磨损超高分子量聚乙烯复合材料;维生素-E分子结构中的氧杂蔡满端可以吸取和稳定自由基,形成苯氧基自由基;苯氧基自由基会遭受位阻,使本身稳定并保留在聚合物内,阻止氧化过程。 [0010] Advantageous Effects of Invention: The present invention selects a medical ultrahigh molecular weight polyethylene UHMWPE powder based materials, and vitamin Ve graphene oxide and their composite, full use of the excellent quality and Vitamin -E graphene oxide, UHMWPE both increased oxidation resistance and biocompatibility, and mechanical properties of UHMWPE increases the wear resistance, the finally obtained has excellent mechanical properties, abrasion antioxidant Super UHMWPE composite; vitamin -E molecule Cai oxa structure can absorb the full end and stable free radical, a phenoxy radical formation; phenoxy radical suffer from steric hindrance, so that in itself is stable and retained within the polymer, to prevent oxidation.

具体实施方式 detailed description

[0011 ]以下对本发明作进一步详细说明。 [0011] The following further detailed description of the present invention.

[0012]医用超高分子量聚乙烯粉末UHMWPE,其为常规的市购产品,粒度范围为4.3-200μmD [0012] Medical the UHMWPE UHMWPE powder, which is a conventional commercially available product, particle size range 4.3-200μmD

[0013]维生素为常规的市购产品,纯度大于98%,对其进行研磨处理,粒度小于ΙΟΟμπι。 [0013] Vitamins are conventional commercially available products, purity of greater than 98%, subjected to rubbing treatment, a particle size of less than ΙΟΟμπι.

[0014]单层氧化石墨烯(GO),是通过氧化还原反应制备出石墨烯的一种衍生物,它是在单层石墨烯二维结构上连接大量含氧官能团,如竣基、揣基、轻基等,具有较高的弹性模量、抗拉强度等力学性能;可市购或自行制备。 [0014] monolayer graphene oxide (the GO), is a derivative of graphene prepared by the redox reaction, which is connected to a large number of oxygen-containing functional groups on the two-dimensional graphene structure, such as group Jun, hides group light group and the like, having high mechanical properties of elastic modulus, tensile strength and the like; self-prepared or commercially available.

[0015]本发明下述实施例所涉及的单层氧化石墨烯GO的制备方法如下: [0015] Preparation of a monolayer of graphene oxide GO following examples of the present invention is as follows:

(1)在40°C温度下,向46g质量浓度为98%的浓硫酸中加入5g细鳞片石墨和0.75g高锰酸钾,连续搅拌90min后,反应产物用去离子水洗至中性,真空干燥后,在900°C下保温50秒,得到膨胀石墨其中浓硫酸的密度按1.84g/mL计算,对应25mL浓硫酸; (1) at 40 ° C for temperature, concentration of 46g to 98% concentrated sulfuric acid was added 0.75g 5g fine flake graphite and potassium permanganate, continuous stirring 90min, the reaction product was washed with deionized water to neutral, vacuum after drying, incubated for 50 seconds at 900 ° C, wherein the density of the expanded graphite obtained by concentrated sulfuric acid 1.84g / mL is calculated, corresponding to 25mL of concentrated sulfuric acid;

(2)在冰浴环境下,向盛有42.3g质量浓度为98%的浓硫酸中加入0.5g硝酸钠、0.5g膨胀石墨及1.5g高锰酸钾,在35 °C下搅拌30min,然后加热升温98°C,加入46g去离子水,搅拌15min,观察到混合物由黑色变为金黄色,用30mL溶度为30%的过氧化氢溶液中和剩余氧化剂,直至无气泡生成其中浓硫酸的密度按1.84g/mL计算,对应23mL浓硫酸; (2) in an ice bath environment, 42.3g filled with the mass concentration of 98% concentrated sulfuric acid was added 0.5g of sodium nitrate, potassium permanganate 1.5g 0.5g expanded graphite and the mixture was stirred at 35 ° C 30min, then heating temperature 98 ° C, was added 46g of deionized water, stirred for 15min, the mixture was observed from black to gold, solubility with 30mL of 30% hydrogen peroxide solution and the oxidizing agent remaining until no bubble generation in which concentrated sulfuric acid press density 1.84g / mL is calculated, corresponding to 23mL of concentrated sulfuric acid;

(3)用质量浓度为5%的稀盐酸溶液和去离子水分别洗涤多次,去除上层溶液得到稳定的分散液,真空干燥后得到所述单层氧化石墨烯。 (3) with a concentration of 5% dilute hydrochloric acid solution and deionized water were washed several times to remove supernatant solution to obtain a stable dispersion, and dried in vacuo to give the single graphene oxide.

[0016] 实施例1 [0016] Example 1

(I)混合粉末的制备工艺: (I) Preparation of mixed powder of:

a、将0.5份的单层氧化石墨烯和0.1份的维生素-E粉末加入到500份溶剂中充分搅拌分散,然后再以200W超声处理Ih; a, 0.5 parts of a single graphene oxide and 0.1 parts of Vitamin -E powder is added to 500 parts of a solvent dispersion sufficiently stirred and then sonicated to Ih is 200W;

b、将99.4份的UHMWPE加入到步骤a得到的溶液中,将混合物经磁力搅拌30min后再次200W超声剥离Ih; B, 99.4 parts of the UHMWPE obtained in step a was added to the solution, the mixture was again stirred for 30min 200W ultrasound was magnetically Ih is peeled;

c、将步骤b得到的混合物置于转速为400r/min球磨机中研磨混合2h; c, the mixture obtained in step b was placed speed of 400r / min ball mill for mixing 2H;

d、将步骤c得到的混合物置于60°C水浴中干燥,在60°C下保温至其完全干燥; d, the mixture obtained in step c was placed in a water bath at 60 ° C and dried until completely dry incubation at 60 ° C;

e、将步骤d处理后的干燥物置于球磨机中研磨粉碎,以400r/min的转速粉碎2h; (2)成型工艺:将10g的上述混合粉末添加到模具中,采用平板硫化机在15MPa压力下预压lOmin,然后在保温箱中200°C保温2h,再采用平板硫化机在20MPa压强下压模处理15min得到板材,冷却至室温; E, after step d treating the dried product was placed in a ball mill pulverization at a rotational speed 400r / min pulverized 2h; (2) Molding Process: adding the mixed powder 10g into a mold using vulcanizing press at 15MPa pressure preload lOmin, then at 200 ° C incubator for incubation 2h, then vulcanizing machine using at 20MPa pressure to obtain a stamper plate processing 15min, cooled to room temperature;

(3)辐照工艺:将复合材料0.9MPa真空密封然后在室温下,采用γ -射线进行辐照交联处理,辐照量为10kGy,辐照的剂量率为5kGyh—1,γ -射线原材用60Co,辐照9天,最终得到具有优良力学性能、抗氧化超低磨损超高分子量聚乙烯复合材料。 (3) irradiation process: the composite material is then vacuum sealed 0.9MPa at room temperature, using γ - ray irradiation cross-linking treatment, in an amount of 10 kGy irradiation, the irradiation dose rate 5kGyh-1, γ - ray original 60Co timber, irradiated 9 days, the finally obtained polyethylene composite material having excellent mechanical properties, high molecular weight antioxidant ultra-low wear.

[0017]所述溶剂为无水乙醇。 The [0017] solvent is ethanol.

[0018] 实施例2 [0018] Example 2

(1)混合粉末的制备工艺: (1) Preparation of mixed powder process:

a、将0.6份的单层氧化石墨烯和0.2份的维生素-E粉末加入到500份溶剂中充分搅拌分散,然后再以400W超声处理1.5h; a, 0.6 parts of a single graphene oxide and 0.2 parts of Vitamin -E powder is added to 500 parts of solvent sufficiently stirred and dispersed, and then sonicated for 1.5 h to 400W;

b、将99.2份的UHMffPE加入到经过步骤a得到的溶液中,将混合物经磁力搅拌60min后再次300W超声剥离1.5h; Again B, 99.2 parts of the following steps a UHMffPE added to the resulting solution, and the mixture was magnetically stirred for 1.5 h 60min 300W ultrasonic peeling;

c、将步骤b得到的混合物置于转速为400r/min球磨机中研磨混合2h; c, the mixture obtained in step b was placed speed of 400r / min ball mill for mixing 2H;

d、将步骤c得到的混合物置于70°C水浴中干燥,在70°C下保温至其完全干燥; d, the mixture obtained in step c was placed in a water bath at 70 ° C and dried until completely dry incubation at 70 ° C;

e、将步骤d处理后的干燥物置于球磨机中研磨粉碎,以400r/min的转速粉碎3小时; E, after the drying process of step d grind was placed in a ball mill, pulverizing speed 400r / min for 3 hours;

(2)成型工艺:将10g的上述混合粉末添加到模具中,采用平板硫化机在1MPa压力下预压15min,然后在保温箱中180°C保温3h,再采用平板硫化机在15MPa压强下压模处理20min得到板材,冷却至室温; (2) Molding Process: adding the mixed powder 10g into a mold using vulcanizing press at 1MPa pressure preloading 15min, then 180 ° C for 3h in an incubator, and then using the vulcanizing machine pressed at 15MPa pressure sheet molding process to obtain 20min, cooled to room temperature;

(3)辐照工艺:将复合材料0.9MPa真空密封然后在室温下,采用γ -射线进行辐照交联处理,辐照量为10kGy,辐照的剂量率为5kGyh—1,γ -射线原材用60Co,辐照9天,最终得到具有优良力学性能、抗氧化超低磨损超高分子量聚乙烯复合材料。 (3) irradiation process: the composite material is then vacuum sealed 0.9MPa at room temperature, using γ - ray irradiation cross-linking treatment, in an amount of 10 kGy irradiation, the irradiation dose rate 5kGyh-1, γ - ray original 60Co timber, irradiated 9 days, the finally obtained polyethylene composite material having excellent mechanical properties, high molecular weight antioxidant ultra-low wear.

[0019]所述溶剂为丙酮。 [0019] The solvent is acetone.

[0020] 实施例3 [0020] Example 3

(1)混合粉末的制备工艺: (1) Preparation of mixed powder process:

a、将0.7份的单层氧化石墨烯和0.3份的维生素-E粉末加入到500份溶剂中充分搅拌分散,然后再以400W超声处理Ih; a, 0.7 parts of a single graphene oxide and 0.3 parts of Vitamin -E powder is added to 500 parts of a solvent dispersion sufficiently stirred and then sonicated to Ih is 400W;

b、将99份的UHMWPE加入到经过步骤a得到的溶液中,将混合物经磁力搅拌90分钟后再次400W超声剥离2h; B again, the UHMWPE is added to 99 parts of the resulting solution through a step, and the mixture was magnetically stirred for 90 minutes 400W ultrasound release 2H;

c、将步骤b得到的混合物置于转速为400r/min球磨机中研磨混合4h; c, the mixture obtained in step b was placed speed of 400r / min ball mill for mixing 4H;

d、将步骤c得到的混合物置于80°C水浴中干燥,在80°C下保温至其完全干燥; d, the mixture obtained in step c was placed in a water bath at 80 ° C and dried until completely dry incubation at 80 ° C;

e、将步骤d处理后的干燥物置于球磨机中研磨粉碎,以600r/min的转速粉碎3小时; E, after the drying process of step d grind was placed in a ball mill, pulverizing speed 600r / min for 3 hours;

(2)成型工艺:将10g的上述混合粉末添加到模具中,采用平板硫化机在13MPa压力下预压12min,然后在保温箱中190°C保温2.5h,再采用平板硫化机在ISMPa压强下压模处理18min得到板材,冷却至室温; (2) Molding Process: add 10g of the mixed powder into a mold using vulcanizing press at a pressure of 13MPa preloading 12min, then at 190 ° C incubator for incubation 2.5h, then using the vulcanizing press at a pressure ISMPa processing 18min stamper plate obtained, cooled to room temperature;

(3)辐照工艺:将复合材料0.9MPa真空密封然后在室温下,采用γ -射线进行辐照交联处理,辐照量为10kGy,辐照的剂量率为5kGyh—1,γ -射线原材用60Co,辐照9天,最终得到具有优良力学性能、抗氧化超低磨损超高分子量聚乙烯复合材料。 (3) irradiation process: the composite material is then vacuum sealed 0.9MPa at room temperature, using γ - ray irradiation cross-linking treatment, in an amount of 10 kGy irradiation, the irradiation dose rate 5kGyh-1, γ - ray original 60Co timber, irradiated 9 days, the finally obtained polyethylene composite material having excellent mechanical properties, high molecular weight antioxidant ultra-low wear.

[0021]所述溶剂为无水乙醇。 The [0021] solvent is ethanol.

Claims (6)

  1. 1.一种超高分子量聚乙烯复合材料的制备方法,其特征是按重量份计步骤为: (1)混合粉末的制备:将单层氧化石墨烯GO和维生素-E加入到溶剂中充分搅拌分散后经超声处理,再加入超高分子量聚乙烯UHMffPE粉末磁力搅拌分散,再次超声处理,经超声剥离得到粉末,然后进行球磨混合,形成均匀的三体混合粉末; (2)成型:将步骤(I)所得混合粉末添加到模具中,采用平板硫化机在预压,然后在保温箱中保温,再采用平板硫化机在压模处理得到板材,冷却至室温; (3)辐照:将步骤(3)所得的复合材料0.5-0.9MPa真空密封,然后在室温下,采用γ-射线进行辐照交联处理,辐照量为10kGy,辐照的剂量率为5kGyh—1,γ -射线原材用60Co,最终得到超高分子量聚乙稀复合材料。 Preparation 1. A composite ultrahigh molecular weight polyethylene, characterized in that the parts by weight by the steps of: preparing a mixed powder (1): monolayer graphene oxide GO Vitamin -E added to the solvent and thoroughly stirred after the dispersion was sonicated, then add UHMffPE UHMWPE powder dispersed magnetic stirring again sonicated by ultrasound to obtain a powder peeling, followed by a ball mill mixed to form a uniform mixed powder trisomy; (2) molding: the step ( I) the resultant mixed powder is added to a mold, employed in the pre-press vulcanizing press, and then incubated in an incubator, and then employed in the vulcanizing machine to obtain a stamper plate, cooled to room temperature; (3) exposure: the step ( 3) the resultant composite material 0.5-0.9MPa vacuum sealed, and then at room temperature using γ- rays irradiation crosslinking, in an amount of 10 kGy irradiation, radiation dose rate 5kGyh-1, γ - ray raw material with 60Co, the finally obtained ultra high molecular weight polyethylene composite.
  2. 2.如权利要求1所述超高分子量聚乙烯复合材料的制备方法,其特征是:所述维生素E的纯度为VE > 98%,粒径小于ΙΟΟμπι。 2. The preparation of claim 1 ultra high molecular weight polyethylene composite material, characterized in that: the purity of vitamin E for VE> 98%, particle size less than ΙΟΟμπι.
  3. 3.如权利要求1所述超高分子量聚乙烯复合材料的制备方法,其特征是:所述超高分子量聚乙烯UHMffPE粉末的粒径范围为4.3-200μπι。 The ultra-high molecular weight as claimed in claim 3. A method for preparing a polyethylene composite material, characterized in that: said ultrahigh molecular weight polyethylene powder size range UHMffPE 4.3-200μπι.
  4. 4.如权利要求1所述超高分子量聚乙烯复合材料的制备方法,其特征是具体步骤如下: (1)混合粉末的制备:将0.3-0.7份的单层氧化石墨烯GO和0.1-0.3份的维生素-E粉末加入到500份溶剂中充分搅拌分散,然后再以200-4001超声处理0.5-211;将99-99.6份的超高分子量聚乙烯粉末UHMWPE加入到上述溶液中,将混合物经磁力搅拌30-90min后再次200-400W超声剥离0.5-2h;将所得混合物置于球磨机中研磨混合2-4h; 将研磨后的混合物置于60-80°C水浴中干燥,在60-80°C下保温至其完全干燥;再次置于球磨机中研磨粉碎,以300_600r/min的转速粉碎2_4h; (2)成型:将10g的步骤(I)所得混合粉末添加到模具中,采用平板硫化机在10-15MPa压力下预压10_15min,然后在保温箱中180-200°C保温2-3h,再采用平板硫化机在15-20MPa压强下压模处理15_20min得到复合材料板材,冷却至室温; (3)辐照:将步骤(3)所得的复合材料真空密封 Preparation of mixed powder (1):: The as claimed in claim 1 preparation of ultra high molecular weight polyethylene composite material, characterized in that the following steps will be 0.3 to 0.7 parts of a single layer of graphene oxide and 0.1-0.3 GO vitamin -E parts powder to 500 parts of a solvent dispersion sufficiently stirred and then sonicated to 200-4001 0.5-211; 99-99.6 parts of the ultrahigh molecular weight polyethylene UHMWPE powder is added to the solution, the mixture was after magnetic stirring again 30-90min 200-400W ultrasonic peeling 0.5-2h; the resulting mixture was placed in a ball mill mixing 2-4h; the milled mixture was placed in a water bath at 60-80 ° C and dried at 60-80 ° drying the insulation to its full C; again placed in a ball mill pulverization at a rotational speed 300_600r / min pulverized 2_4h; (2) molding: the resulting mixed powder was added to the mold in step (I) 10g, using the vulcanizing machine 10-15MPa under preload pressure 10_15min, and then in an incubator incubated 2-3h 180-200 ° C, and then using the vulcanizing press at a pressure of 15-20MPa stamper process 15_20min composite laminate obtained was cooled to room temperature; (3 ) irradiation: obtained in step (3) vacuum sealing the composite material ;然后在室温下,采用γ-射线进行辐照交联处理,辐照时间为9-12天,最终得到产品超高分子量聚乙烯复合材料。 ; Then at room temperature using γ- rays irradiation crosslinking, the irradiation time is 9-12 days, to give the final product UHMWPE composite.
  5. 5.如权利要求2所述超高分子量聚乙烯复合材料的制备方法,其特征是:步骤(I)所述溶剂为无水乙醇或丙酮。 5. The preparation of claim 2 ultra high molecular weight polyethylene composite material, characterized in that: step (I) the solvent is ethanol or acetone.
  6. 6.如权利要求2所述超高分子量聚乙烯复合材料的制备方法,其特征是:采用γ -射线进行辐照交联处理时,辐照量为10kGy,辐照的剂量率为5kGyh—1,γ -射线原材用60Co。 6. The preparation of claim 2 ultra high molecular weight polyethylene composite material, characterized in that: the use of γ - ray irradiation cross-linking treatment, the amount is 10 kGy irradiation, the irradiation dose rate 5kGyh-1 , γ - ray original timber 60Co.
CN 201610247210 2016-04-20 2016-04-20 Preparation method of ultra-high molecular weight polyethylene (UHMWPE) composite material CN105837896A (en)

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US6277390B1 (en) * 1998-10-21 2001-08-21 Sulzer Orthopaedie Ag UHMW polyethylene for implants
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US6277390B1 (en) * 1998-10-21 2001-08-21 Sulzer Orthopaedie Ag UHMW polyethylene for implants
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