CN115785571B - Large-scale industrial model and 3D printing polypropylene particles for outdoor building and preparation method thereof - Google Patents
Large-scale industrial model and 3D printing polypropylene particles for outdoor building and preparation method thereof Download PDFInfo
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- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 2
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- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 2
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 2
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Abstract
The invention provides a 3D printing polypropylene particle applied to a large-scale industrial model and outdoor building and a preparation method thereof, which solve the technical problems of large shrinkage, easy warping and poor interlayer binding force of the existing 3D printing polypropylene. According to the 3D printing polypropylene particles, polypropylene, a toughening agent, an adhesive, a compatilizer, an organic nucleating agent, an antioxidant and a plasticizer which are prepared by certain mass components are mixed in proportion, glass fibers and mineral powder are fed on a double-screw extruder laterally, and the modified polypropylene particles are obtained through extrusion. The invention is particularly suitable for 3D printing of large industrial models and outdoor buildings, has high rigidity, good dimensional stability and interlayer binding force, and has wide application prospect in the 3D printing technology of granules.
Description
Technical Field
The invention belongs to the field of high polymer materials, and relates to 3D printing polypropylene particles for large industrial models and outdoor buildings, and a preparation method and application thereof.
Background
The additive manufacturing technology can directly carry out die-free manufacturing through Computer Aided Design (CAD), and has the advantages of die-free production, design freedom and short manufacturing time, so that the process is very suitable for small-batch production of parts with high design varieties. Different additive manufacturing techniques are very different and have different industrial interests. Only a few manufacturing processes are particularly suitable for producing large polymer parts (greater than 0.5x0.5x0.5 m). Particle-based additive manufacturing techniques are most suitable for producing large parts because of their scalable build volume and economic value of production due to high build rates.
Fused particle fabrication (FGF) is a particle-based additive manufacturing technology that has increased industry interest in this technology because of its economic advantages (shorter production time and reduced material costs) and availability of a variety of materials. Essentially standard pellets (injection molded or extruded materials) can be used with an extruder. However, different processing conditions typically require changing standard materials. In particular, polypropylene (PP) is a promising material for industrial applications because of its high impact strength, chemical resistance and low cost.
However, 3D printing processing of PP is also challenging, especially due to poor adhesion of PP material to the print bed and warpage. In many cases PP sheets or tapes are used as printing surfaces, the warpage of the printed polypropylene parts is significantly reduced due to the high adhesion. A great challenge with PP sheet is the risk of welding parts at the printed surface, with a narrow process window between achieving good adhesion to the printed surface and welding the parts to the printed surface. However, the adhesion of the heated print bed can in principle be regulated by the temperature of the print bed, however, studies have shown that large-area components can still be separated from the print surface, since these components are particularly prone to tilting. In addition to low adhesion, the strong shrinkage of PP due to its crystallinity is also a major factor affecting warpage of the article.
Meanwhile, the 3D printing forming mode brings great convenience and has some own defects, one is that the interface bonding property between layers is obviously different from that of the traditional material body, the mechanical properties in certain directions are seriously reduced, often less than 50% of raw materials, the performance and the application of the device are seriously influenced, and the printing device is only displayed when a model is displayed in many times.
In order to increase the application of polypropylene materials in FGF industrial-grade large-scale printing, a 3D printing polypropylene particle with high rigidity, good dimensional stability and interlayer binding force needs to be developed to solve the technical defects of the existing materials.
Disclosure of Invention
The invention aims to provide a 3D printing polypropylene particle for a large-scale industrial model and outdoor building and a preparation method thereof, which overcome the problems of poor interlayer binding force, serious warping caused by crystallization and the like of the existing polypropylene material for 3D printing. According to the invention, the shrinkage rate of polypropylene is reduced by adding the inorganic filler and the toughening agent, so that the dimensional stability is greatly improved; meanwhile, the added adhesive contains more ester groups, has strong cohesive strength and adhesive force, can effectively bond materials between layers in the printing process, and can enable the printed materials to be in a molten state for a long time in the printing process due to the lower melting point of the adhesive, so that the printed materials of the next layer can be better adhered.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
The 3D printing polypropylene particle for the large-scale industrial model and outdoor building comprises polypropylene resin, a toughening agent, an adhesive, glass fiber, mineral powder, a compatilizer, an organic nucleating agent, an antioxidant and a plasticizer;
Wherein the polypropylene resin comprises a homo-polypropylene resin and an impact co-polypropylene resin;
Based on the total weight of the final 3D printing polypropylene particles, the content of the homopolymerized polypropylene resin is 5-20wt%, the content of the impact copolymerization polypropylene resin is 20-50wt%, the content of the toughening agent is 5-15wt%, the content of the adhesive is 5-15wt%, the content of the glass fiber is 10-50wt%, the content of the mineral powder is 10-30wt%, the content of the compatilizer is 0.5-5wt%, and the content of the organic nucleating agent, the antioxidant and the plasticizer is 0.1-1wt%.
Preferably, the melt flow index of the homo-polypropylene resin is 10-200g/10min at 230 ℃ under a load of 2.16 kg.
Preferably, the impact copolymer polypropylene resin is a polymer obtained by copolymerizing propylene and ethylene, the ethylene content is 3-30wt%, and the melt flow index under the action of 2.16kg load at 230 ℃ is 1-40g/10min.
Preferably, the toughening agent is one or more of ethylene-butene copolymer and ethylene-octene copolymer, and has a melt flow index of 0.5-30 g/10min at 230 ℃ and 2.16 kg weight.
Preferably, the adhesive is low-melting-point polyester polyol, and the melting point measured under the condition of heating rate of 10 ℃/min is 50-80 ℃; the melt flow index is 3-10g/10min at 160℃and 2.16 kg weight.
Preferably, the glass fiber has a length of 2-10mm.
Preferably, the mineral powder is one or more of calcium carbonate, talcum powder, mica, silicon carbide and montmorillonite, and the particle size is 1000-7000 meshes.
Preferably, the compatilizer is obtained by grafting modified polypropylene with maleic anhydride, and the content of maleic anhydride functional groups is 0.5-2wt%.
Preferably, the organic nucleating agent is one or more of sorbitol, phosphate and rosin nucleating agents.
Preferably, the antioxidant is one or more of hindered phenol macromolecular antioxidants, phosphorous acid antioxidants and alkyl ester antioxidants.
Preferably, the plasticizer is one or more of phthalic acid esters, fatty acid esters, phosphoric acid esters and epoxy esters.
The invention also provides a preparation method of the 3D printing polypropylene particles for the large-scale industrial model and the outdoor building, which comprises the following steps:
(1) Uniformly mixing polypropylene resin, a toughening agent, an adhesive, a compatilizer, an organic nucleating agent, an antioxidant and a plasticizer in a high-speed mixer to obtain a mixture;
(2) Feeding the mixture through a main feeding port of a double-screw extruder, adding glass fiber and mineral powder from a side feeding port, extruding, cooling, and granulating by a granulator to obtain a granular modified polypropylene material;
preferably, the conditions for extrusion granulation in the step (2) include: the extrusion temperature is 180-250 ℃.
The invention also provides application of the 3D printing polypropylene particles as a 3D printing material for large industrial models and outdoor buildings.
Compared with the prior art, the invention has the following technical advantages:
1) The mixture of the copolymerized polypropylene and the homopolypropylene reduces the crystallinity; by adding a large amount of inorganic filler and toughening agent, the shrinkage rate of the modified polypropylene is obviously reduced, the dimensional stability is greatly improved, the warping phenomenon is basically eliminated, and the polypropylene particles have good 3D printing effect and precision.
2) The added adhesive contains more ester groups, has strong cohesive strength and adhesive force, can effectively bond materials between layers in the printing process, and can lead the printed materials to be in a molten state for a long time in the printing process due to the lower melting point, so as to better adhere the printed materials of the next layer.
3) The 3D printing modified polypropylene obtained by the invention is particularly suitable for printing large industrial models and outdoor building particles, and has the advantages of simple preparation method, high production efficiency, high rigidity, difficult warping and good interlayer binding force, and has wide market prospect and benefit.
Detailed Description
The invention will now be further illustrated by means of specific examples which are given solely by way of illustration of the invention and do not limit the scope thereof.
The preparation method of the polypropylene particles for 3D printing comprises the following steps:
(1) Mixing the reagent with the raw materials: firstly, putting homo-polypropylene resin, co-polypropylene resin and a toughening agent into a stirrer, then adding an adhesive, uniformly stirring, then adding an antioxidant, an organic nucleating agent, a compatilizer and a plasticizer for subsequent mixing, continuously mixing for 2 minutes, and finally obtaining a mixed raw material.
(2) And (3) extruding and granulating: adding the mixed raw materials in the step (1) into a main feeding bin of a double-screw extruder, adding glass fibers and mineral powder into a side feeding bin of the extruder, adding the glass fibers and the mineral powder into the extruder according to the component proportion, and uniformly melting and mixing, wherein the feeding speed is kept uniform and smooth, the temperature of a melting section in the double-screw extrusion process is 180-200 ℃, the temperature of a mixing section is 210-250 ℃, and the temperature of an extrusion section is 180-200 ℃. And (5) granulating the mixture by a granulator after cooling to obtain the polypropylene granular material.
Polypropylene melting point and crystallinity test method: polypropylene melting point and crystallinity tests were performed using a type PEAKINELMER differential scanning calorimeter.
Polypropylene shrinkage test method: the prepared polypropylene particles are injection molded into a flat plate with the thickness of 150 multiplied by 300 multiplied by 2mm by adopting a kraussmaffei-750 CX injection molding machine, the injection molding temperature is 230 ℃, and other parameters are molded by adopting default parameters of a system. And (3) standing the injection molded sample plate at room temperature for 24 hours, and then measuring the side length of the plate, wherein the shrinkage rate is obtained by dividing the absolute value of the difference between the injection molded sample plate and the design value by the design value.
The method for testing the bonding force between polypropylene printing layers comprises the following steps: and (3) adopting an innovative three-emperor G5 particle printer, vertically printing a 3D printing template with the thickness of 200mm multiplied by 100mm on the prepared polypropylene particles vertical to the bottom plate, cutting out an A dumbbell type stretching spline required in ISO527 through a sample cutting machine, and testing the stretching performance in the Z-axis direction.
In each of the examples and comparative examples, the main raw material sources are as shown in table 1:
TABLE 1 Main raw material brands and sources
13-4.5-T438H of glass fiber with the length of 4.5mm purchased from Taishan glass fiber Co., ltd; calcium carbonate, KL5, 1000 mesh, purchased from Colon powder Co., ltd; talc powder, E05L, with a mesh number of 5000 mesh, purchased from Liaoning Ai Hai Talc Co., ltd; mica, HC-400, mesh number 2500, purchased from Lingshou county Hua Jing mica Co.
Other materials and reagents were obtained commercially, unless otherwise specified.
Polypropylene particles were prepared according to the above preparation method, according to the composition of the components of comparative examples 1-4 and examples 1-2 in table 2:
Table 2 formulations (weight percent) of examples 1-4 and comparative examples 1-2
The polypropylene particles thus obtained were subjected to performance test, and the results are shown in Table 3:
TABLE 3 Properties of examples 1-4 and comparative examples 1-2
From the sample differential scanning calorimeter test data of table 3, it can be seen that there is no significant change in the melting point of each sample, and the addition of the copolymer polypropylene slightly reduces the melting point to less than 1 ℃; the crystallinity is not changed significantly, but from comparative example 2, it can be seen that the crystallinity is slightly reduced after adding the polypropylene copolymer, so that the example adopts the combination of the polypropylene homopolymer and the polypropylene copolymer, and then adds the thermoplastic elastomer and the inorganic filler, and adds a large amount of glass fiber, so that the shrinkage of the modified polypropylene is reduced sharply, and the result of the printing test is consistent with the result of the shrinkage test.
From the printing test result, the fracture in the comparative example shows brittle fracture, and after the adhesive is added, the fracture is converted into ductile fracture, so that the interlayer bonding force in the Z-axis direction is obviously increased; in particular, comparative examples 1,2 and 3, 4, when the adhesive agent was lowered, although the tensile modulus was raised (as a result of the raised glass fiber content), the elongation at break was lowered, indicating that the adhesive agent plays an effective adhesive role in the printing process, and the interlayer bonding force of printing can be effectively improved.
From the comprehensive test results, the polypropylene particles prepared in the examples 1-4 have the advantages of processability and molding accuracy, small molding shrinkage deformation and warping, and are suitable for being used as 3D printing materials, particularly high rigidity and good interlayer binding force, and are extremely suitable for 3D printing of large-scale industrial models and outdoor buildings.
While particular embodiments of the present invention have been illustrated and described, it would be obvious to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. Such modifications and variations are intended to be included within the scope of the present invention.
Claims (8)
1. The 3D printing polypropylene particle for the large-scale industrial model and outdoor building is characterized by comprising polypropylene resin, a toughening agent, an adhesive, glass fiber and mineral powder;
Wherein the polypropylene resin comprises a homo-polypropylene resin and an impact co-polypropylene resin;
the adhesive is Capa 2200;
based on 3D printing polypropylene particles, the content of the homopolymerized polypropylene resin is 5-20 wt%, the content of the impact copolymerization polypropylene resin is 20-50 wt%, the content of the toughening agent is 5-15 wt%, the content of the adhesive is 5-15 wt%, the content of the glass fiber is 10-50 wt%, and the content of the mineral powder is 10-30 wt%.
2. The 3D printing polypropylene particle for the large-scale industrial model and the outdoor building is characterized by comprising polypropylene resin, a toughening agent, an adhesive, glass fiber, mineral powder, a compatilizer, an organic nucleating agent, an antioxidant and a plasticizer;
Wherein the polypropylene resin comprises a homo-polypropylene resin and an impact co-polypropylene resin;
the adhesive is Capa 2200;
based on 3D printing polypropylene particles, the content of the homopolymerized polypropylene resin is 5-20 wt%, the content of the impact copolymerization polypropylene resin is 20-50 wt%, the content of the toughening agent is 5-15 wt%, the content of the adhesive is 5-15 wt%, the content of the glass fiber is 10-50 wt%, the content of the mineral powder is 10-30 wt%, the content of the compatilizer is 0.5-5 wt%, and the content of the organic nucleating agent, the antioxidant and the plasticizer are all 0.1-1 wt%.
3. 3D printed polypropylene particles according to claim 1 or 2, wherein the melt flow index of the homo-polypropylene resin is 10-200 g/10min at 230 ℃ under a load of 2.16 kg; and/or
The anti-impact copolymerized polypropylene resin is a polymer obtained by copolymerization of propylene and ethylene, and the melt flow index of the anti-impact copolymerized polypropylene resin is 1-40 g/10min under the action of 2.16kg load at 230 ℃.
4. The 3D printed polypropylene particles according to claim 1 or 2, wherein the toughening agent is one or both of an ethylene-butene copolymer and an ethylene-octene copolymer having a melt flow index of 0.5 to 30g/10min at 230 ℃, 2.16 kg weight.
5. The 3D printed polypropylene particles according to claim 1 or 2, wherein the glass fiber length is 2-10 mm; and/or
The mineral powder is one or more of calcium carbonate, talcum powder, mica, silicon carbide and montmorillonite.
6. The 3D printed polypropylene particles according to claim 5, wherein the mineral powder has a particle size of 1000-7000 mesh.
7. The 3D printed polypropylene particles according to claim 2, wherein the compatibilizer is a maleic anhydride grafted modified polypropylene having a maleic anhydride functional group content of 0.5-2 wt%; and/or
The organic nucleating agent is one or more of sorbitol, phosphate and rosin nucleating agents; and/or
The antioxidant is one or more of hindered phenol macromolecular antioxidants, phosphorous acid antioxidants and alkyl ester antioxidants; and/or
The plasticizer is one or more of phthalic acid esters, fatty acid esters, phosphoric acid esters and epoxy esters.
8. Use of the 3D printed polypropylene particles of any one of claims 1-7 as 3D printed material for large industrial models and outdoor buildings.
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| KR101864159B1 (en) * | 2016-11-29 | 2018-06-05 | 주식회사 삼양사 | Environment-friendly polycarbonate resin composition with good adhesive properties |
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