CN103980593A - Modified high density polyethylene 3D printing moulding material and preparation method - Google Patents
Modified high density polyethylene 3D printing moulding material and preparation method Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
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Abstract
The invention discloses a modified high density polyethylene 3D printing moulding material with toughness. The modified high density polyethylene 3D printing moulding material comprises the following components, by weight, 60 parts of high density polyethylene, 10-50 parts of powdered steatile, 20-25 parts of calcium carbonate, 10-50 parts of wollastonite, 10-15 parts of carbon nanotube, 0.1-0.5 part of an antioxidant and 0.1-0.5 part of a silane coupling agent. The modified high density polyethylene material has high tensile strength and good impact toughness. Application value of high density polyethylane can be raised and its application field can be widened. The high density polyethylene material is more in line with characteristics of a 3D printing material. The material provided by the invention is environmentally friendly, has low cost and has important industrial application value.
Description
Technical field
The present invention relates to 3D printing shaping Material Field, be specifically related to a kind of modification high-density polyethylene 3D printing shaping material that is rich in toughness and preparation method thereof.
Background technology
3D printing technique (Three Dimensions Printing, three-dimensional printing technology, 3DP), be lamination manufacture (Additive Manufacturing, AM) a kind of form of technology, its principle is to produce material object by adding material to article layering.3D printing technique has been realized the leap from orthographic plan to entity, and a series of digital applications technology taking it as representative are even known as the Industrial Revolution for the third time.The technology that 3D prints mainly comprises the techniques such as SLA, FDM, SLS, LOM.Wherein fusion sediment forming technique (FDM) and selective laser sintering (SLS) technology are all used thermoplastics as basic 3D printed material.But 3D printing technique faces at present the most serious problem and challenge are that 3D printing shaping material is very rare.Current 3D printing shaping material is mainly the thermoplastic materials such as nylon, polyethylene terephthalate, polybutylene terephthalate and ABS (acrylonitrile-butadiene-styrene (ABS)).These materials not only hardness are higher, and the parts that print are more crisp frangible, and high to printing conditional request, and usually cannot be by small structure high-resolution ground printing shaping.
High density polyethylene(HDPE) (HDPE) is a kind of large kind general-purpose plastics, and in the world, its output is only second to polyvinyl chloride and Low Density Polyethylene, occupies the 3rd.HDPE is nontoxic, cheap, light weight, has higher rigidity, good processibility, excellent wet fastness and chemical stability, is widely used.But himself have the shortcoming in some application, use temperature is not high yet, and ageing resistance is poor, under the effect of atmosphere, sunlight, oxygen, become fragile gradually, mechanical strength and electrical property decline, under mold temperature, can cause viscosity degradation because of oxygenizement, occur variable color, produce striped etc.More, because its homopolymer shock strength is low, be difficult to meet the demand of some engineering fields to performance.Conventional 3D printed material need to possess certain toughness and shock resistance, and conventional H DPE does not possess these features.This patent has been studied HDPE has been strengthened to toughening modifying can be applied to 3D printing field.
CN1433443A relates to a kind of method that embeds the complex body of nanofiber in polymeric matrix that is formed on, the method is included in sneaks into nanofiber to form coacervate in plastic substrate, and by diplomatic corps's aggressiveness under hydrodynamic force stress and the nanofiber that distributes equably; Described hydrodynamic force stress splits off described coacervate, flows and can be used to realize minor diameter and arrangement in conjunction with carrying out extra extension.Gained complex body can deposit with consolidation (FDM) moulding, and the polymkeric substance wherein a volume nanofiber being strengthened is as the wire raw material of FDM technique.In this process, nanofiber complex line (diameter is about 2 millimeters) is extruded through the die head of mm size, produces complex line in a row and makes sheet material and 3D parts.In this patent, raw material used is the polymkeric substance wire rod that nanofiber strengthens.Its shortcoming is: the FDM of nanofiber complex line is very complicated, is difficult for processing.
CN1812878A relates to a kind of powder of the 3D of being suitable for printing, and this powder comprises the blend of thermoplastic granulates thing and adhesive particle thing, and wherein said thermoplastic granulates thing is optional from polyolefine.The powder of this patent, in the time printing for 3D, need to use solvent.Therefore, the 3D printing system of CN1812878A is liquid composition, and its shortcoming is to need to use in many cases to the mankind and harmful solvent or the dispersion agent of environment, and complicated operation, is difficult for dispersed or dissolves.
CN102093646B relates to a kind of material of printing rapid shaping for 3D and preparation method thereof, rapid prototyping material comprises modified powder materials A and binding agent B, wherein: the preparation of modified powder materials A: powdered material and the first solvent are joined to ball mill or grinding machine for grinding, obtain powdered material pre-treatment material; By tensio-active agent, lubricant, organic resin successively joins in the second solvent, and dispersed with stirring 2-3h, obtains modification liquid; Powdered material pre-treatment material is mixed with modification liquid, put into shredder, normal temperature mixed grinding, dry, grind, obtain modified powder materials A; When use, 1 part of modified powder materials A and 0.01-0.07 part binding agent B adapted.This patent 3D formed body used is solution system, and its shortcoming is to prepare in materials process needs material to grind and modification, and uses supercritical drying, complicated operation.
US2004/0232583A1 relates to a kind of method of manufacturing three-dimensional body, and it comprises: a powdered substrate layer a) is provided; B) on one or more regions of described base material, selectivity applies at least one microwave absorbing first sensitive materials; C) with layer described in microwave radiation processing at least one times.Wherein loosely mention and can use the polymkeric substance that is selected from polyester, polyvinyl chloride, polyacetal, polypropylene, polyethylene, polystyrene, polycarbonate, PMMI, PMMA, ionomer, polymeric amide, copolyesters, copolyamide, terpolymer, ABS or its mixture.US2004/0232583A1 does not mention polyethylene is carried out to modification, so that it is suitable for 3D printing.
The object of the invention is for low in HDPE toughness at present, the feature such as shock strength is low, proposes a kind of method of toughness of the HDPE of improvement material.By adding appropriate compound inorganic powder filled HDPE, toughness and resistance to impact shock are greatly improved.
Summary of the invention
The object of the invention is to overcome the defect of above-mentioned prior art, a kind of modification high-density polyethylene 3D printing shaping material that is rich in toughness is provided, described material modified have higher tensile strength and good impelling strength, it is characterized in that comprising following component by weight, preferably by the following component of meter by weight:
Described high density polyethylene(HDPE) can be any commercially available high density polyethylene(HDPE).Its density is for example 0.94-0.96g/cm
3, molecular weight is for example 40000-300000.
Described talcum is the talcum powder with 1000-1500 order granularity.In preferred embodiments, before use, talcum powder is carried out to modification with sodium stearate and silane coupling agent.Modified talc powder disperses more even in resin matrix, and the interface binding power between resin and talcum powder is stronger, thereby makes the physical and chemical performance of described composition more superior.The consumption of talcum is 10-50 part, for example, be 15,20,25,30,35,40,45 parts.
Described calcium carbonate is 2000-2500 object calcium carbonate, is preferably water-ground limestone.In preferred embodiments, before use, calcium carbonate is carried out to modification to improve consistency and the dispersiveness of calcium carbonate and polymkeric substance with stearic acid, strengthen its avidity.The consumption of calcium carbonate is 20-25 part, for example, be 21,22,23,24 parts.
The granularity of described wollastonite is 1000-1500 order.In preferred embodiments, before use, with silane coupling agent, wollastonite is carried out to modification and fill reinforced effects to improve the consistency of itself and superpolymer base-material, to improve.The consumption of wollastonite is 10-50 part, for example, be 5,20,25,30,35,40,45 parts.
Described carbon nanotube can be various carbon nanotubes, for example Single Walled Carbon Nanotube or multi-walled carbon nano-tubes.In preferred embodiments, with concentrated nitric acid (65%), described carbon nanotube is activated.The inventor finds surprisingly, and the carbon nanotube after nitric acid activation can make its specific surface area greatly increase, and can improve avtive spot, improves dispersiveness in matrix etc.The concrete technology of nitric acid activation can be 2h-2.5h that carbon nanotube is refluxed in concentrated nitric acid, disperses (preferred ultrasonic dispersion) simultaneously, is washed till neutrality subsequently with distilled water.The consumption of carbon nanotube can be 10-15 part, for example, be 11,12,13,14 parts.
Described oxidation inhibitor is antioxidant CA.The consumption of oxidation inhibitor is 0-0.5 part, for example, be 0.1,0.2,0.3,0.4 part.
Described silane coupling agent can be selected from KH550 and DB550.The consumption of silane coupling agent is 0-0.5 part, for example, be 0.1,0.2,0.3,0.4 part.
The present invention also provides a kind of method of preparing the modification high-density polyethylene 3D printing shaping material that is rich in toughness, it is characterized in that: each raw material is mixed to then extruding pelletization.
Described mixing can be carried out in high-speed mixer.Extruding pelletization can carry out in single screw extrusion machine or twin screw extruder.Extrusion temperature is 170-180 DEG C, and screw speed is 240-300r/min.
In order to carry out mechanical test, the pellet injection molding that extruding pelletization can be obtained is Mechanics Performance Testing national standard test bars.
The outstanding feature of the present invention is:
1. compared with traditional HDPE, modification HDPE material of the present invention has higher tensile strength and impelling strength preferably, and this is suitable for as 3D printing shaping material it.
2. production cost of the present invention is low, and production process is simple, is easy to suitability for industrialized production.
In another embodiment of the present invention, the present invention relates to the purposes of a kind of modification high-density polyethylene of the present invention in 3D prints.
In another embodiment of the present invention, the present invention relates to a kind of 3D Method of printing, it is characterized in that using modification high-density polyethylene of the present invention.
Embodiment
Below by embodiment, the present invention is described in further detail, but this should be interpreted as to scope of the present invention only limits to following embodiment.In the situation that not departing from aforesaid method thought of the present invention, various replacements or the change made according to ordinary skill knowledge and customary means, all should be within the scope of the present invention.
In the context of the present invention, except as otherwise noted, otherwise all umbers and percentage ratio are weight part and weight percentage.
In embodiment below, tensile strength is carried out according to GB/T1040-92, and shock strength is carried out according to GB/T1843-2008, and flexural strength is carried out according to GB/T9341-2008.
Embodiment 1
By the HDPE of 60 weight parts, the CaCO of 20 parts
3, 20 parts of wollastonites, the talcum of 0,10,20,30,40 or 50 part, the carbon nanotube of 10 parts, the antioxidant CA of 0.1 part, the silane coupling agent of 0.1 part, through high-speed mixer mixing 5min, then at twin screw extruder extruding pelletization, pellet is injection moulding after cooling drying, makes batten.Wherein said carbon nanotube activates through nitric acid, and the concrete technology of nitric acid activation is 2h that carbon nanotube is refluxed in 65% concentrated nitric acid, and ultrasonic dispersion simultaneously, is washed till neutrality with distilled water subsequently.
Processing condition: 1. expressing technique: 175 DEG C of extrusion temperatures, screw speed 240r/min.2. injection technique: 180 DEG C of injecting forming temperatures, injection pressure 80MPa; Injection speed 40g/s; Inject time 6s; Dwell time 10s; 50 DEG C of mould temperature.
HDPE salient features after modification is tested, and test result is as follows:
| Test item | 0 part, talcum | 10 parts, talcum | 20 parts, talcum | 30 parts, talcum | 40 parts, talcum | 50 parts, talcum |
| Tensile strength/MPa | 17.5 | 18.8 | 20.3 | 22.1 | 23.0 | 23.9 |
| Shock strength/KJ/m2 | 32.8 | 31.5 | 30.1 | 28.7 | 27.2 | 25.3 |
| Flexural strength/MPa | 17.8 | 18.3 | 19.0 | 19.4 | 19.9 | 20.8 |
As seen from the above table: 1) add the increase of massfraction along with talcum powder, the tensile strength of compound system is linear ascendant trend altogether, in the time that talcum powder interpolation is greater than 20 parts, system tensile strength reaches 20.3MPa, has exceeded the tensile strength (20.03MPa) of matrix resin.In the time that talcum powder is added to 50 parts, the tensile strength of compound system reaches 23.9MPa altogether, has improved nearly 20% than the tensile strength of matrix resin.This has embodied talcous enhancement.2) along with the increase of talcum powder interpolation massfraction, the shock strength of compound system declines gradually altogether.In the time that talcum powder is added to 50 parts, the impact strength decreased of compound system is 25.3kJ/m altogether
2, but still a little more than the shock strength (24.92kJ/m of matrix resin
2).This is due to CaCO
3particle connects by having produced good interface between coupling agent and HDPE, has made up to a great extent the impact of weak interface, makes HDPE/ talcum/CaCO
3compound system still keeps higher shock strength altogether.3) along with talcum powder adds the increase of massfraction, the flexural strength of compound system increases to some extent altogether, and within the scope of all interpolations flexural strengths higher than matrix resin (13.34MPa) all.When talcous, while being added to 50 parts, the flexural strength of compound system is 20.8MPa altogether, has improved 55% than the flexural strength of matrix resin.
Embodiment 2
By the HDPE of 60 weight parts, the CaCO of 20 parts
3, the talcum of 10 parts, the carbon nanotube of 10 parts, the antioxidant CA of 0.5 part, 0.5 part of silane coupling agent, and the wollastonite of 0,10,20,30,40 or 50 part is through high-speed mixer mixing 5min, then at twin screw extruder extruding pelletization, pellet is injection moulding after cooling drying, makes batten.Wherein said carbon nanotube activates through nitric acid, and the concrete technology of nitric acid activation is 2h that carbon nanotube is refluxed in 65% concentrated nitric acid, and ultrasonic dispersion simultaneously, is washed till neutrality with distilled water subsequently.
Processing condition: 1. expressing technique: 175 DEG C of extrusion temperatures, screw speed 240r/min.2. injection technique: 180 DEG C of injecting forming temperatures, injection pressure 80MPa; Injection speed 40g/s; Inject time 6s; Dwell time 10s; 50 DEG C of mould temperature.
HDPE salient features after modification detects, and test result is as follows:
As seen from the above table: 1) along with the increase of wollastonite proportioning altogether the tensile strength of compound system increase to some extent, in the time that the proportioning of wollastonite is 50 parts, the tensile strength of compound system is 19.4MPa altogether, a little less than matrix resin (20.03MPa).The enhancement that wollastonite is described can partly make up the destruction of spherical calcium carbonate to system intensity.2) along with the increase of wollastonite proportioning altogether the shock strength of compound system decline to some extent.In the time that the proportioning of wollastonite is 50 parts, the shock strength of compound system is 30.3KJ/m altogether
2, far away higher than the shock strength (24.9KJ/m of matrix resin
2).Illustrate that these two kinds of powders of wollastonite and calcium carbonate can form good interface bonding with matrix resin under the existence of coupling agent, under the acting in conjunction of two kinds of powders, compound system toughness is greatly improved altogether.3) along with the increase of wollastonite proportioning altogether the flexural strength of compound system increase to some extent, and within the scope of all interpolations flexural strengths higher than matrix resin (13.34MPa) all.In the time that the proportioning of wollastonite is 50 parts, the flexural strength of compound system is 22.1MPa altogether, has improved nearly 60% than matrix resin.
Embodiment 3
By the HDPE of 60 weight parts, the CaCO of 20 parts
3, the talcum of 20 parts, the antioxidant CA of 0.1 part, the silane coupling agent of 0.1 part, 30 parts of wollastonites, 0,10 (through nitric acid activation), 10 (without nitric acid activation), 12 (through nitric acid activation), 13 (through nitric acid activation) and 15 (through nitric acid activation) part carbon nanotube are through high-speed mixer mixing 5min, then at twin screw extruder extruding pelletization, pellet is injection moulding after cooling drying, makes batten.Wherein the activation of carbon nanotube is identical with embodiment 1 and 2.
Processing condition: 1. expressing technique: 175 DEG C of extrusion temperatures, screw speed 240r/min.2. injection technique: 180 DEG C of injecting forming temperatures, injection pressure 80MPa; Injection speed 40g/s; Inject time 6s; Dwell time 10s; 50 DEG C of mould temperature.
HDPE salient features after modification is tested, and test result is as follows:
Find out from upper table, do not add in the situation of carbon nanotube, the performance of gained HDPE all has decline in various degree.In the time adding 10 parts of not activated carbon nanotubes, the performance of gained HDPE improves.In the time adding activated carbon nanotube, the performance of gained HDPE further improves.
This embodiment can find out that carbon nanotube plays keying action to the lifting of HDPE performance in this patent.
The common HDPE toughness of this patent is low, the features such as shock strength is low are to its modification, modification high-density polyethylene material has high tensile strength and good impelling strength, can improve the using value of high density polyethylene(HDPE), expand its Application Areas, make high-density polyethylene material more meet the feature of 3D printed material.The not only environmental protection of this material, and cost is low, has important industrial application value.
Claims (8)
1. a modification high-density polyethylene, it comprises following component by weight:
2. according to the modification high-density polyethylene of claim 1, wherein said talcum is the talcum powder with 1000-1500 order granularity.
3. according to the modification high-density polyethylene of claim 1 or 2, wherein said calcium carbonate is 2000-2500 object water-ground limestone.
4. according to the modification high-density polyethylene of any one in claim 1-3, the granularity of wherein said wollastonite is 1000-1500 order.
5. according to the modification high-density polyethylene of any one in claim 1-4, wherein carbon nanotube activates with nitric acid.
6. prepare according to a method for the modification high-density polyethylene of any one in claim 1-5, it comprises each raw material is mixed, then extruding pelletization.
7. the purposes in 3D prints according to the modification high-density polyethylene of any one in claim 1-5.
8. a 3D Method of printing, is characterized in that using according to the modification high-density polyethylene of any one in claim 1-5.
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Cited By (14)
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| CN105623054A (en) * | 2016-04-08 | 2016-06-01 | 张哲夫 | HDPE (high-density polyethylene) nano plastic and preparation method thereof |
| CN106479054A (en) * | 2016-11-03 | 2017-03-08 | 宁波尚高新材料有限公司 | A kind of polymer composite and preparation method thereof |
| WO2017079282A1 (en) | 2015-11-04 | 2017-05-11 | Imerys Filtration Minerals, Inc. | Compositions and methods for additive manufacturing |
| CN106893173A (en) * | 2015-12-21 | 2017-06-27 | 上海邦中新材料有限公司 | A kind of 3D printing material |
| CN108002814A (en) * | 2017-12-15 | 2018-05-08 | 李进宅 | A kind of ceramic material for 3D printing and its preparation method and application |
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| CN109467744A (en) * | 2018-09-13 | 2019-03-15 | 苏州巴夏科技发展有限公司 | A kind of high-speed molten deposition modeling composite material and the application in 3D printing |
| CN111187456A (en) * | 2018-10-26 | 2020-05-22 | 中国石油化工股份有限公司 | High-density polyethylene composition, preparation method thereof, 3D printing material and application thereof |
| CN111440371A (en) * | 2020-03-24 | 2020-07-24 | 杭州联通管业有限公司 | Anti-freezing polyethylene power tube and preparation method thereof |
| CN113527786A (en) * | 2020-04-14 | 2021-10-22 | 中国石油化工股份有限公司 | Ultrahigh molecular weight polyethylene composition and preparation method thereof, ultrahigh molecular weight polyethylene pipe and preparation method and application thereof, and composite pipe |
| CN114213810A (en) * | 2021-12-28 | 2022-03-22 | 宁波美佳速创智能科技有限公司 | High-strength 3D printing photosensitive resin material |
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