CN111073208A - A low warpage, low odor 3D printing ABS material and its preparation method and application - Google Patents
A low warpage, low odor 3D printing ABS material and its preparation method and application Download PDFInfo
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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Abstract
本发明提供了一种低翘曲、低气味3D打印ABS材料及其制备方法，所述ABS材料的原料组成按重量计包括：ABS树脂：42‑99.4％；抗氧剂：0.1‑3％；相容剂：0.1‑5％；抗冲击改性剂：0.1‑10％；无机填料：0.1‑20％；除味剂：0.1‑10％；增塑剂：0.1‑10％。本发明的ABS材料可应用于3D打印，产品打印精度高，打印流畅，不易出现拉丝、断裂、翘曲等问题影响打印产品质量。The invention provides a low-warping, low-odor 3D printing ABS material and a preparation method thereof. The raw material composition of the ABS material comprises by weight: ABS resin: 42-99.4%; antioxidant: 0.1-3%; Compatibilizer: 0.1‑5%; Impact Modifier: 0.1‑10%; Inorganic Filler: 0.1‑20%; Deodorant: 0.1‑10%; Plasticizer: 0.1‑10%. The ABS material of the invention can be applied to 3D printing, and the product has high printing accuracy, smooth printing, and is less prone to problems such as wire drawing, breakage, warpage, etc., which affect the quality of the printed product.
Description
Technical Field
The invention relates to an ABS material, in particular to a low-warpage and low-odor 3D printing ABS material and a preparation method and application thereof.
Background
Fused deposition printing (FDM) is one of the first 3D printing technologies, and is suitable for many kinds of materials, and relatively low in equipment cost, and is the most widely used 3D printing technology at present.
The material suitable for the FDM technology is mainly a high polymer filament material, and the material is conveyed into a printing nozzle through a gear to be printed and molded at a certain processing temperature. The ABS material is a terpolymer material polymerized by three monomers of acrylonitrile (A), butadiene (B) and styrene (S), and is a material with better comprehensive performance which is used as an FDM technology at first. However, the common ABS material applied to 3D printing technology still has the following two main defects: 1. the problems of warpage and deformation caused by insufficient material processing fluidity and high shrinkage rate cause low printing yield and poor finished product quality; 2. residual auxiliary agents and monomers in the ABS polymerization process and peculiar smell sources such as micromolecules generated by secondary thermal processing volatilize to generate serious peculiar smell.
CN107603181A discloses an ABS composite material for 3D printing and a preparation method thereof, wherein the ABS composite material for 3D printing is formed by mixing ABS, PC, a compatibilizer and white carbon black. In the technology, the addition of PC resin improves the performances of the alloy material such as impact strength and the like, but the printing temperature of the material is relatively increased, the adhesion force among material layers is reduced, and the cracking problem is generated along with the increase of the printing temperature of the material.
CN109206832A discloses an ABS material with extremely low warpage and no cracking for 3D printing and a preparation method thereof, wherein amorphous copolyester with low shrinkage and spherical inorganic powder are used to reduce the shrinkage of the material and improve the warpage resistance of the material, but the problem of peculiar smell of the material is still generated.
CN103059409A discloses a low-odor and low-emission modified polypropylene material and a preparation method thereof, wherein a nano zinc oxide prepared by a microemulsion method is used for preparing a nano zinc oxide modified activated carbon material, the nano zinc oxide modified activated carbon material is loaded on the surface of porous activated carbon, and the porous activated carbon is used for absorbing residual monomers, decomposition products and organic acid in base material polypropylene, so as to achieve an obvious odor removal effect. However, activated carbon is limited to use in black materials due to its own black color.
Disclosure of Invention
It is an object of the present invention to provide a novel low warpage, low odor ABS material suitable for 3D printing applications.
Another object of the present invention is to provide a method for preparing a low warpage, low odor ABS material suitable for 3D printing use.
The invention also aims to provide application of the low-warpage and low-odor ABS material.
According to one aspect of the invention, the invention provides an ABS material, which comprises the following raw materials by weight:
ABS resin: 42 to 99.4 percent;
antioxidant: 0.1-3%;
a compatilizer: 0.1-5%;
impact modifier: 0.1-10%;
inorganic filler: 0.1-20%;
odor removing agent: 0.1-10%;
plasticizer: 0.1 to 10 percent.
According to the specific embodiment of the invention, in the raw material composition of the ABS material, the ABS resin is an acrylonitrile-butadiene-styrene terpolymer produced by polymerization by a bulk method, an emulsion method or a suspension method. Preferably, the ABS resin with the total residual amount of styrene, acrylonitrile and ethylbenzene monomer less than 800ppm is selected in the invention.
According to a specific embodiment of the invention, the raw material composition of the ABS material of the invention comprises at least one of pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris (2, 4-di-tert-butylphenyl) phosphite, triethylene glycol bis [ β - (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ], octadecyl β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate and distearyl alcohol pentaerythritol diphosphite.
According to a specific embodiment of the present invention, the ABS material of the present invention comprises a raw material composition, wherein the compatibilizer comprises at least one of a blend of maleic anhydride grafted ABS and styrene, and a cyclic anhydride grafted ABS.
According to a specific embodiment of the present invention, in the raw material composition of the ABS material of the present invention, the impact modifier comprises at least one of natural rubber, styrene, acrylonitrile-butadiene rubber, styrene-based thermoplastic elastomer, and thermoplastic polyurethane elastomer.
According to a specific embodiment of the invention, in the raw material composition of the ABS material of the invention, the inorganic filler comprises at least one of barium sulfate, glass microsphere, titanium dioxide, attapulgite, boron nitride, calcium carbonate, talc powder and pottery clay. Preferably, the mesh number of the inorganic filler particles selected in the present invention is not less than 500, more preferably 1200-3000 mesh.
According to a specific embodiment of the present invention, in the raw material composition of the ABS material of the present invention, the odor removing agent comprises at least one of porous aluminum silicon, organic chelating agent, nano odor removing agent, and inorganic silicate material with a single pore structure. Preferably, the mesh number of the deodorant selected in the invention is not less than 500, and more preferably 1200-2000 mesh number.
According to the specific embodiment of the invention, in the raw material composition of the ABS material, the plasticizer comprises tasteless environment-friendly medium and high molecular weight polyester, the molecular weight is 1500-.
In the invention, if no special specification exists, no special requirement exists on the performance parameters of all the raw materials which are not mentioned in the invention, and the raw materials meet the relevant industry standards or requirements.
The ABS material disclosed by the invention can be used as a consumable product for 3D printing, and has the performance characteristics of high fluidity, high performance, low warpage, low VOC and low odor.
According to another aspect of the present invention, the present invention further provides a preparation method of the ABS material, which comprises the following steps:
s1, preparing other raw materials except the plasticizer in the raw materials according to the weight part ratio, putting the raw materials into a premixer to be uniformly mixed, heating the mixture to 60-80 ℃, and then preserving the heat for 30-120 minutes to obtain a premix;
s2, adding the premix obtained in the step S1 into a double-screw extruder, injecting a plasticizer through a gear pump, and injecting H into the middle section of the extruder2O/CO2/N2H is pumped out by a vacuum pumping section2O/CO2/N2Pumping out, wherein the vacuum pressure of a vacuum pumping section is-0.05 MPa to-0.1 MPa, and cutting into granules to obtain ABS particles, wherein the rotating speed of a screw of the double-screw extruder is 50-400rpm, and the temperature of a charging barrel is 170-280 ℃;
s3, drying ABS particles, adding the particle products into an extruder by using a polymer spinning process after drying, extruding by using a screw rod, using a tractor to draw, adjusting material threads by adjusting the extrusion speed and the drawing speed, shaping the materials by using a water/air cooling mode, winding and winding by using a servo motor/torque motor, wherein the material threads are controllable at 1.1-3.5mm, the extrusion rotating speed of the extruder is 10-200rpm, the temperature of a charging barrel is 170 plus materials and 260 ℃, the drawing and winding speed is 10-120m/min, and the cooling water temperature is 40-95 ℃.
According to the technology, when the high molecular weight polyester and the inorganic filler are used, the material molding shrinkage rate is reduced, the material processing flow property is improved, the warping and cracking problems caused by 3D printing of the ABS material are effectively reduced, the extraction technology is adopted to use water or inert gas, the cost is low, the extraction technology is combined with a deodorant for use, the product is pure, the operation is simple, and the application prospect is wide.
According to another aspect of the invention, the invention also provides the application of the ABS material in 3D printing, in other words, the invention provides a method for 3D printing by using the ABS material, wherein the printing speed is controlled to be 10-150mm/s, the printing temperature is 190-260 ℃, the printing layer height is 0.05-0.2mm, the printing bottom plate temperature is 40-110 ℃, and the printing chamber temperature is 40-100 ℃. The ABS material disclosed by the invention has the characteristics of high printing precision of products, smooth printing, difficulty in causing problems of wire drawing, fracture, warping and the like to influence the quality of printed products, low warping, high strength and high fluidity, and no toxic and harmful substances are volatilized in the printing process.
In conclusion, the invention provides the ABS material, the environment-friendly medium and high molecular weight polyester and the inorganic filler are used for improving the processing flow property of the material and improving the warpage problem of the material, the ABS material produced by combining the extraction technology and the deodorant has the characteristics of low odor, low warpage, high strength and high fluidity, no toxic substances are volatilized in the printing process, the ABS material is not limited to be used as a consumable product in the 3D printing industry, and the ABS material has wide application prospects in the fields of automobiles, household appliances and the like. The method has the advantages of simple technical process and obvious implementation effect, and can be applied to production capacity areas of different scales.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
Operations not described in detail in the examples are performed according to the instructions of the conventional operations or instruments in the field. The raw materials used in the examples meet the performance requirements set forth in the invention above for the raw materials.
Example 1
Weighing 77.96% of ABS resin produced by bulk polymerization, 0.26% of antioxidant β - (3, 5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate and 0.4% of tris [ 2.4-di-tert-butylphenyl ] propionate]0.78% of phosphite ester, 3% of ABS-g-MAH compatilizer, 10% of 1200-mesh heavy calcium carbonate, 3% of SEBS and 2% of organic chelating deodorant are uniformly mixed in a high-speed premixer, heated to 80 ℃ and then kept warm for 30 minutes. The premix was fed into a twin-screw extruder and 3% of the polyester oligomer was injected by a gear pump. Injecting H into the middle section of the extruder2O, flow rate of 2.5m3H, the vacuum pressure of a vacuum pumping section is-0.098 MPa, and the ABS material is obtained by cutting into granules, wherein a screw of the double-screw extruder rotatesThe speed was 300rpm and the barrel temperature was 190 ℃ and 260 ℃.
And (3) introducing the dried ABS granular material into a single-screw extruder, and processing the extruded ABS granular material into a 1.75 +/-0.03 mm wire rod meeting the requirement of a 3D printer in a traction water cooling mode through a tractor, wherein the screw rotating speed of the single-screw extruder is 50rpm, the temperature of a charging barrel is 190 plus one year, and the traction winding speed is 70 m/min.
Example 2
65.96% of ABS resin produced by bulk polymerization with the same mark as that of example 1, 0.26% of antioxidant β - (3, 5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate and 0.4% of tris [ 2.4-di-tert-butylphenyl ] propionate were weighed]0.78% of phosphite ester, 3% of ABS-g-MAH compatilizer, 20% of 1200 mesh barium sulfate, 5% of HR-181 styrene, 5% of acrylonitrile-butadiene rubber and 2% of organic chelating deodorant are uniformly mixed in a high-speed premixer, heated to 80 ℃ and then kept warm for 30 minutes. The premix was fed into a twin-screw extruder and 3% of the polyester oligomer was injected by a gear pump. Injecting CO into the middle section of the extruder2At a flow rate of 2.5m3And h, cutting into granules to obtain the ABS material, wherein the vacuum pressure of a vacuum pumping section is-0.098 MPa, the rotating speed of a screw of the double-screw extruder is 300rpm, and the temperature of a charging barrel is 190-.
And (3) introducing the dried ABS granular material into a single-screw extruder, and processing the extruded ABS granular material into a 1.75 +/-0.03 mm wire rod meeting the requirement of a 3D printer in a traction water cooling mode through a tractor, wherein the screw rotating speed of the single-screw extruder is 50rpm, the temperature of a charging barrel is 190 plus one year, and the traction winding speed is 70 m/min.
Comparative example 1
Weighing 75.96% of ABS resin produced by emulsion polymerization, 0.26% of antioxidant β - (3, 5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate and 0.4% of tris [ 2.4-di-tert-butylphenyl ] propionate]0.78% of phosphite ester, 3% of ABS-g-MAH compatilizer, 10% of 1200-mesh heavy calcium carbonate, 5% of SEBS and 2% of organic chelating deodorant are uniformly mixed in a high-speed premixer, heated to 80 ℃ and then kept for 30 minutes. The premix was fed into a twin-screw extruder and 3% of the polyester oligomer was injected by a gear pump. Injecting CO into the middle section of the extruder2At a flow rate of 2.5m3H, the vacuum pressure of a vacuum pumping section is-0.098 MPa, and the ABS is obtained by cutting into granulesThe material, wherein the screw rotating speed of the double-screw extruder is 300rpm, and the cylinder temperature is 190-260 ℃.
And (3) introducing the dried ABS granular material into a single-screw extruder, and processing the extruded ABS granular material into a 1.75 +/-0.03 mm wire rod meeting the requirement of a 3D printer in a traction water cooling mode through a tractor, wherein the screw rotating speed of the single-screw extruder is 50rpm, the temperature of a charging barrel is 190 plus one year, and the traction winding speed is 70 m/min.
Comparative example 2
79.96% of ABS resin produced by bulk polymerization of the same brand as in example 1, 0.26% of antioxidant β - (3, 5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate and 0.4% of tris [ 2.4-di-tert-butylphenyl ] propionate were weighed]0.78% of phosphite ester, 3% of ABS-g-MAH compatilizer, 10% of 1200-mesh heavy calcium carbonate and 3% of SEBS are uniformly mixed in a high-speed premixer, heated to 80 ℃ and then kept warm for 30 minutes. The premix was fed into a twin-screw extruder and 3% of the polyester oligomer was injected by a gear pump. Injecting H into the middle section of the extruder2O, flow rate of 2.5m3And h, cutting into granules to obtain the ABS material, wherein the vacuum pressure of a vacuum pumping section is-0.098 MPa, the rotating speed of a screw of the double-screw extruder is 300rpm, and the temperature of a charging barrel is 190-.
And (3) introducing the dried ABS granular material into a single-screw extruder, and processing the extruded ABS granular material into a 1.75 +/-0.03 mm wire rod meeting the requirement of a 3D printer in a traction water cooling mode through a tractor, wherein the screw rotating speed of the single-screw extruder is 50rpm, the temperature of a charging barrel is 190 plus one year, and the traction winding speed is 70 m/min.
The ABS materials prepared in the embodiments 1 and 2 and the comparative examples 1 and 2 are subjected to odor grade detection, styrene, ethylbenzene and acrylonitrile residue sheet analysis is performed through gas chromatography, FDM3D printing technology equipment is used for printing, the 3D printing speed is controlled to be 50mm/s, the printing temperature is controlled to be 240 ℃, the printing bottom plate temperature is 110 ℃, the printing layer height is 0.14mm, the filling rate is 100%, a sample meeting the ASTM test standard is prepared, and the test is performed through a melt index instrument, a universal stretcher, a cantilever beam impact analyzer and a thermal deformation temperature tester.
The properties of the obtained product were characterized as follows:
the obtained odor grade was characterized as follows:
| temperature of | Unit of | Example 1 | Example 2 | Comparative example 1 | Comparative example 2 | Detection method |
| 23℃ | Stage | 1 | 1 | 1 | 1 | VDA270 |
| 40℃ | Stage | 1 | 1 | 2 | 1 | VDA270 |
| 80℃ | Stage | 1 | 2 | 2 | 2 | VDA270 |
Comparative examples 1, 2 and comparative examples 1, 2 show that: the use of the extraction technology can effectively reduce the total amount of ABS resin residual sheets and realize the low VOC target of the material. The use of extraction techniques in combination with odor removal agents can be effective in reducing odor levels. The mass ABS resin is superior to emulsion ABS resin in terms of total amount of residual monomers and odor grade by using a deodorant and an extraction technology.
The ABS materials prepared in examples 1 and 2 and comparative examples 1 and 2 and the ABS resin material used as the raw material were printed using FDM3D printing equipment, the 3D printing speed was controlled at 50mm/s, the printing temperature was 240 ℃, the printing substrate temperature was 110 ℃, the printing layer height was 0.14mm, the filling ratio was 20% to prepare a geometric body of 50 × 100mm, 100 × 100mm, 200 × 100mm, the substrate of the printer was a flat surface, and the average of the heights of the four corners of the bottom surface of the geometric body raised from the substrate flat surface was measured.
The foregoing is merely a preferred embodiment of this invention, which is intended to be illustrative, not limiting; it will be understood by those skilled in the art that various changes, modifications and equivalents may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. An ABS material comprises the following raw materials in percentage by weight:
ABS resin: 42 to 99.4 percent;
antioxidant: 0.1-3%;
a compatilizer: 0.1-5%;
impact modifier: 0.1-10%;
inorganic filler: 0.1-20%;
odor removing agent: 0.1-10%;
plasticizer: 0.1 to 10 percent.
2. The ABS material of claim 1 wherein the ABS resin is an acrylonitrile-butadiene-styrene terpolymer produced by bulk, emulsion, or suspension polymerization.
3. The ABS material of claim 1 wherein the antioxidant comprises at least one of tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] pentaerythritol ester, tris (2, 4-di-tert-butylphenyl) phosphite, triethylene glycol bis [ β - (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ], β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate octadecyl ester, and dioctadecyl alcohol pentaerythritol diphosphite.
4. The ABS material of claim 1 wherein the compatibilizer comprises at least one of a blend of maleic anhydride grafted ABS and styrene and a cyclic anhydride grafted ABS.
5. The ABS material of claim 1 wherein the impact modifier comprises at least one of natural rubber, styrene, acrylonitrile-butadiene rubber, styrenic thermoplastic elastomers, thermoplastic polyurethane elastomers.
6. The ABS material of claim 1 wherein the inorganic filler comprises at least one of barium sulfate, glass microspheres, titanium dioxide, attapulgite, boron nitride, calcium carbonate, talc, and china clay.
7. The ABS material of claim 1, wherein the odor eliminator comprises at least one of porous aluminum silicon, an organic chelating agent, a nano odor eliminator, and a single pore structured inorganic silicate material.
8. The ABS material of claim 1 wherein the plasticizer comprises a odorless environment-friendly medium and high molecular weight polyester having a molecular weight of 1500-5000 and a viscosity of 1500-8000 cps.
9. A method of preparing an ABS material according to any one of claims 1 to 8, comprising the steps of:
s1, preparing other raw materials except the plasticizer in the raw materials according to the weight part ratio, putting the raw materials into a premixer to be uniformly mixed, heating the mixture to 60-80 ℃, and then preserving the heat for 30-120 minutes to obtain a premix;
s2, adding the premix obtained in the step S1 into a double-screw extruder, injecting a plasticizer through a gear pump, and injecting H into the middle section of the extruder2O/CO2/N2At least one of (1), a vacuum pumping section (H)2O/CO2/N2Pumping out, wherein the vacuum pressure of a vacuum pumping section is-0.05 MPa to-0.1 MPa, and cutting into granules to obtain ABS particles, wherein the rotating speed of a screw of the double-screw extruder is 50-400rpm, and the temperature of a charging barrel is 170-280 ℃;
s3, drying ABS particles, adding the particle products into an extruder by using a polymer spinning process after drying, extruding by using a screw rod, using a tractor to draw, adjusting material threads by adjusting the extrusion speed and the drawing speed, shaping the materials by using a water/air cooling mode, winding and winding by using a servo motor/torque motor, wherein the material threads are controllable at 1.1-3.5mm, the extrusion rotating speed of the extruder is 10-200rpm, the temperature of a charging barrel is 170 plus materials and 260 ℃, the drawing and winding speed is 10-120m/min, and the cooling water temperature is 40-95 ℃.
10. Use of the ABS material according to one of claims 1 to 8 in 3D printing, wherein the printing speed is controlled to be 10 to 150mm/s, the printing temperature is 190 ℃ and 260 ℃, the printing layer height is 0.05 to 0.2mm, the printing substrate temperature is 40 to 110 ℃, and the printing chamber temperature is 40 to 100 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911326958.9A CN111073208A (en) | 2019-12-20 | 2019-12-20 | A low warpage, low odor 3D printing ABS material and its preparation method and application |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911326958.9A CN111073208A (en) | 2019-12-20 | 2019-12-20 | A low warpage, low odor 3D printing ABS material and its preparation method and application |
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| CN201911326958.9A Pending CN111073208A (en) | 2019-12-20 | 2019-12-20 | A low warpage, low odor 3D printing ABS material and its preparation method and application |
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| CN (1) | CN111073208A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112662085A (en) * | 2020-12-16 | 2021-04-16 | 上海长伟锦磁工程塑料有限公司 | Ultrahigh heat-resistant ABS material with excellent bonding strength with polyurethane and preparation method thereof |
| CN113773519A (en) * | 2021-09-01 | 2021-12-10 | 福建师范大学 | ABS wire with low VOCs emission characteristics for FDM printers |
| CN115651351A (en) * | 2022-12-29 | 2023-01-31 | 广州市威柏乐器制造有限公司 | ABS composite material for 3D printing of guitar and preparation method thereof |
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| CN109608815A (en) * | 2018-11-21 | 2019-04-12 | 北方华锦化学工业股份有限公司 | A kind of 3D printing low smell ABS material and preparation method thereof |
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| CN109608815A (en) * | 2018-11-21 | 2019-04-12 | 北方华锦化学工业股份有限公司 | A kind of 3D printing low smell ABS material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112662085A (en) * | 2020-12-16 | 2021-04-16 | 上海长伟锦磁工程塑料有限公司 | Ultrahigh heat-resistant ABS material with excellent bonding strength with polyurethane and preparation method thereof |
| CN113773519A (en) * | 2021-09-01 | 2021-12-10 | 福建师范大学 | ABS wire with low VOCs emission characteristics for FDM printers |
| CN115651351A (en) * | 2022-12-29 | 2023-01-31 | 广州市威柏乐器制造有限公司 | ABS composite material for 3D printing of guitar and preparation method thereof |
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Application publication date: 20200428 |