CN117922009A - Preparation method of polylactic acid fiber composite 3D printing material - Google Patents
Preparation method of polylactic acid fiber composite 3D printing material Download PDFInfo
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- CN117922009A CN117922009A CN202410102030.7A CN202410102030A CN117922009A CN 117922009 A CN117922009 A CN 117922009A CN 202410102030 A CN202410102030 A CN 202410102030A CN 117922009 A CN117922009 A CN 117922009A
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- polylactic acid
- printing material
- antioxidant
- fiber composite
- fibers
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- 239000000835 fiber Substances 0.000 title claims abstract description 69
- 229920000747 poly(lactic acid) Polymers 0.000 title claims abstract description 59
- 239000004626 polylactic acid Substances 0.000 title claims abstract description 59
- 239000000463 material Substances 0.000 title claims abstract description 38
- 238000010146 3D printing Methods 0.000 title claims abstract description 33
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 25
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 25
- 239000004014 plasticizer Substances 0.000 claims abstract description 23
- 239000012745 toughening agent Substances 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 19
- 238000002791 soaking Methods 0.000 claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 239000000155 melt Substances 0.000 claims abstract description 14
- 230000000655 anti-hydrolysis Effects 0.000 claims abstract description 13
- 238000005520 cutting process Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000003365 glass fiber Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- QZCLKYGREBVARF-UHFFFAOYSA-N Acetyl tributyl citrate Chemical compound CCCCOC(=O)CC(C(=O)OCCCC)(OC(C)=O)CC(=O)OCCCC QZCLKYGREBVARF-UHFFFAOYSA-N 0.000 claims description 6
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 5
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 5
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 claims description 5
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 5
- 239000004917 carbon fiber Substances 0.000 claims description 5
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 claims description 5
- 239000004609 Impact Modifier Substances 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- 238000007639 printing Methods 0.000 abstract description 3
- 230000007062 hydrolysis Effects 0.000 description 6
- 238000006460 hydrolysis reaction Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 239000003112 inhibitor Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000004790 ingeo Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000008832 zhongfu Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
Abstract
The invention provides a preparation method of a polylactic acid fiber composite 3D printing material, which comprises the following steps: s1, fully soaking long fibers in a melt of polylactic acid through soaking equipment; s2, cutting the infiltrated long fibers into short fibers with preset lengths through a cutting machine; s3, fully drying the polylactic acid, the short fibers, the toughening agent, the plasticizer, the antioxidant and the anti-hydrolysis agent by a dryer; s4, fully mixing the fully dried polylactic acid, the short fibers, the toughening agent, the plasticizer, the antioxidant and the anti-hydrolysis agent according to a preset ratio by a high-speed mixer to obtain a blending raw material; s5, preparing the blending raw materials into 3D printing materials with preset wire diameters through a screw extruder. On the basis of keeping the original excellent performance of the polylactic acid, the mechanical property of the polylactic acid serving as a printing material is improved, so that the polylactic acid can be widely applied.
Description
Technical Field
The invention relates to the field of 3D printing materials, in particular to a preparation method of a polylactic acid fiber composite 3D printing material.
Background
3D printing, i.e. additive manufacturing technology, is an emerging technology in the manufacturing industry that is honored as a manufacturing technology with industrial revolution significance. The technology has many advantages such as no limitation of the shape of the product parts, small machining allowance, high material utilization rate, fine structure of the formed parts, excellent performance, short production period of the parts and the like. With the development of society, 3D printing is becoming more and more popular, and has been widely used in various fields such as rapid mold manufacturing, biomedical science, aerospace, technical design, automobile machinery, communication electronics, and construction industry.
Polylactic acid is used as a common 3D printing material, and has the advantages of no unpleasant odor during melting, biological source and complete degradation. However, brittle fracture is liable to occur due to poor mechanical properties of polylactic acid, which greatly limits the application of polylactic acid printed articles.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a preparation method of a polylactic acid fiber composite 3D printing material. On the basis of keeping the original excellent performance of the polylactic acid, the method improves the mechanical property of the polylactic acid as a printing material, so that the polylactic acid can be widely applied.
The invention adopts the following technical scheme.
A preparation method of a polylactic acid fiber composite 3D printing material comprises the following steps:
s1, fully soaking long fibers in a melt of polylactic acid through soaking equipment;
s2, cutting the infiltrated long fibers into short fibers with preset lengths through a cutting machine;
S3, fully drying the polylactic acid, the short fibers, the toughening agent, the plasticizer, the antioxidant and the anti-hydrolysis agent by a dryer;
s4, fully mixing the fully dried polylactic acid, the short fibers, the toughening agent, the plasticizer, the antioxidant and the anti-hydrolysis agent according to a preset ratio by a high-speed mixer to obtain a blending raw material;
S5, preparing the blending raw materials into 3D printing materials with preset wire diameters through a screw extruder.
Further, in step S1, the long fibers are long glass fibers or long carbon fibers, or a mixture of both.
Further, in step S1, the melt of polylactic acid has a number average molecular weight of 5000 to 10000.
Further, in step S2, the predetermined length of the short fibers is 2 to 3mm.
Further, the drying temperature adopted in the step S3 is 50-80 ℃ and the drying time is 5-12 hours, so that the materials are dried until the moisture is less than or equal to 0.05%.
Further, in step S4, the toughening agent is an acrylic impact modifier added in a weight ratio of 1/100 to 10/100.
Further, in step S4, the plasticizer is any one or a combination of two of PEG400 and ATBC, and the weight ratio of the addition is 1/1000 to 5/100.
Further, in step S4, the antioxidant is any one or a combination of two of the antioxidant 168 and the antioxidant 1010, and the weight ratio of the antioxidant to the antioxidant is 1/1000 to 5/1000.
The beneficial effects of the invention are as follows:
According to the invention, the polylactic acid, the short fiber, the toughening agent, the plasticizer, the antioxidant and the anti-hydrolysis agent are fully mixed to prepare the 3D printing material, and the mechanical property of the polylactic acid serving as the printing material is improved on the basis of keeping the original excellent property of the polylactic acid, so that the polylactic acid can be widely applied.
Detailed Description
The present invention will be described in further detail with reference to examples, but embodiments of the present invention are not limited thereto.
A preparation method of a polylactic acid fiber composite 3D printing material comprises the following steps:
s1, fully soaking long fibers in a melt of polylactic acid through soaking equipment;
s2, cutting the infiltrated long fibers into short fibers with preset lengths through a cutting machine;
S3, fully drying the polylactic acid, the short fibers, the toughening agent, the plasticizer, the antioxidant and the anti-hydrolysis agent by a dryer;
s4, fully mixing the fully dried polylactic acid, the short fibers, the toughening agent, the plasticizer, the antioxidant and the anti-hydrolysis agent according to a preset ratio by a high-speed mixer to obtain a blending raw material;
S5, preparing the blending raw materials into 3D printing materials with preset wire diameters through a screw extruder.
As an example, the melt of polylactic acid may be HISUN REVODE110, natureWorks Ingeo, 4032D, total CorbionLX175, or a mixture of any one or more thereof.
Preferably, in step S1, the long fibers are long glass fibers or long carbon fibers, or a mixture of the two. As an example, the long glass fiber uses boulder 988A and the long carbon fiber uses medium complex hawk SYT49S. In other examples, the long glass fiber may be selected from Taishan glass fiber T635B, and the long carbon fiber may be selected fromT300、/>T700S、/>T700G, zhongfu eagle SYT45S, zhongfu eagle SYT49C.
Preferably, in step S1, the melt of polylactic acid has a number average molecular weight of 5000 to 10000.
Preferably, in step S2, the predetermined length of the short fibers is 2 to 3mm.
Preferably, the drying temperature adopted in the step S3 is 50-80 ℃ and the drying time is 5-12 hours, so that the materials are dried until the moisture is less than or equal to 0.05%.
Preferably, in step S4, the toughening agent is an acrylic impact modifier added in a weight ratio of 1/100 to 10/100. Specifically, the toughening agent can be Paraloid KM355P, paraloid BPM520, novista Topadd TIM812, kaneKane/>Any one or a mixture of a plurality of them.
Preferably, in step S4, the plasticizer is any one or a combination of two of PEG400 and ATBC, and the weight ratio of the plasticizer to the ATBC is 1/1000 to 5/100.
Preferably, in step S4, the antioxidant is any one or a combination of two of the antioxidant 168 and the antioxidant 1010, and the weight ratio of the antioxidant to the antioxidant is 1/1000 to 5/1000.
Preferably, in step S4, the hydrolysis inhibitor is110，/>1010 And/>210, And the weight ratio of the addition of the mixture is 1/1000 to 1/100.
Example 1
The polylactic acid fiber composite 3D printing material is prepared according to the following steps:
(1) Pre-soaking long fibers;
Fully soaking long fibers in a melt of polylactic acid through soaking equipment, wherein the long fibers are made of boulder 988A; the melt of polylactic acid adopts HISUN REVODE to 110 and has the number average molecular weight of 5000;
(2) Preparing short fibers;
dividing the infiltrated long fibers into short fibers with the length of 2-3 mm by a cutter;
(3) Drying raw materials;
adopting a drying temperature of 50 ℃ to continuously dry for 12 hours, and fully drying polylactic acid, short fibers, a toughening agent, a plasticizer, an antioxidant and an anti-hydrolysis agent until the water content is less than or equal to 0.05%;
Wherein, the toughening agent is Paraloid KM355P; PEG400 is selected as the plasticizer; the antioxidant is antioxidant 168; the hydrolysis resisting agent is selected from 110；
(4) Mixing raw materials;
adding a toughening agent with the weight ratio of 1/100, a plasticizer with the weight ratio of 1/1000, an antioxidant with the weight ratio of 1/1000 and an anti-hydrolysis agent with the weight ratio of 1/1000 into a 1:1 mixture of polylactic acid and short fibers, and fully mixing by a high-speed mixer to obtain a blending raw material;
(5) Production of 3D printing material;
The blended raw materials were made into 3D printing materials of 1.75mm wire diameter by a screw extruder.
Example 2
The polylactic acid fiber composite 3D printing material is prepared according to the following steps:
(1) Pre-soaking long fibers;
fully soaking long fibers in a melt of polylactic acid through soaking equipment, wherein the long fibers are Taishan glass fibers T635B; the melt of polylactic acid adopts NatureWorks Ingeo4032D and has a number average molecular weight of 5000;
(2) Preparing short fibers;
dividing the infiltrated long fibers into short fibers with the length of 2-3 mm by a cutter;
(3) Drying raw materials;
Adopting a drying temperature of 80 ℃ to continuously dry for 5 hours, and fully drying polylactic acid, short fibers, a toughening agent, a plasticizer, an antioxidant and an anti-hydrolysis agent until the water content is less than or equal to 0.05%;
Wherein, the toughening agent is Paraloid BPM520; the plasticizer is ATBC; the antioxidant is selected from antioxidant 1010; the hydrolysis resisting agent is selected from 1010；
(4) Mixing raw materials;
Adding 10/100 of toughening agent, 5/100 of plasticizer, 5/1000 of antioxidant and 1/100 of hydrolysis inhibitor into a 1/1 mixture of polylactic acid and short fibers, and fully mixing by a high-speed mixer to obtain a blending raw material;
(5) Production of 3D printing material;
The blended raw materials are made into 3D printing materials with the wire diameter of 2mm through a screw extruder.
Example 3
The polylactic acid fiber composite 3D printing material is prepared according to the following steps:
(1) Pre-soaking long fibers;
Fully soaking long fibers in a melt of polylactic acid through soaking equipment, wherein the long fibers are a mixture of boulder 988A and Mount Taishan glass fiber T635B; the melt of polylactic acid adopts HISUN REVODE, natureWorks Ingeo, 4032D and Total Corbion A mixture of LX175 and having a number average molecular weight of 5000;
(2) Preparing short fibers;
dividing the infiltrated long fibers into short fibers with the length of 2-3 mm by a cutter;
(3) Drying raw materials;
Adopting a drying temperature of 80 ℃ to continuously dry for 5 hours, and fully drying polylactic acid, short fibers, a toughening agent, a plasticizer, an antioxidant and an anti-hydrolysis agent until the water content is less than or equal to 0.05%;
wherein the toughening agent is a mixture of Paraloid BPM520 and Novista Topadd TIM812,812; the plasticizer is a mixture of PEG400 and ATBC; the antioxidant is a mixture of antioxidant 168 and antioxidant 1010; the hydrolysis resisting agent is selected from 110，/>1010 And/>210, A mixture of two or more of the following;
(4) Mixing raw materials;
Adding 10/100 of toughening agent, 5/100 of plasticizer, 5/1000 of antioxidant and 1/100 of hydrolysis inhibitor into a 1/1 mixture of polylactic acid and short fibers, and fully mixing by a high-speed mixer to obtain a blending raw material;
(5) Production of 3D printing material;
The blended raw materials are made into 3D printing materials with the wire diameter of 2mm through a screw extruder.
It is to be understood that the above examples of the present invention are provided by way of illustration only and not by way of limitation of the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (8)
1. The preparation method of the polylactic acid fiber composite 3D printing material is characterized by comprising the following steps of:
s1, fully soaking long fibers in a melt of polylactic acid through soaking equipment;
s2, cutting the infiltrated long fibers into short fibers with preset lengths through a cutting machine;
S3, fully drying the polylactic acid, the short fibers, the toughening agent, the plasticizer, the antioxidant and the anti-hydrolysis agent by a dryer;
s4, fully mixing the fully dried polylactic acid, the short fibers, the toughening agent, the plasticizer, the antioxidant and the anti-hydrolysis agent according to a preset ratio by a high-speed mixer to obtain a blending raw material;
S5, preparing the blending raw materials into 3D printing materials with preset wire diameters through a screw extruder.
2. The method for preparing a polylactic acid fiber composite 3D printing material according to claim 1, wherein in step S1, the long fibers are long glass fibers or long carbon fibers, or a mixture of both.
3. The method for producing a polylactic acid fiber composite 3D printing material according to claim 1, wherein in step S1, the number average molecular weight of the melt of polylactic acid is 5000 to 10000.
4. The method for preparing a polylactic acid fiber composite 3D printing material according to claim 1, wherein in step S2, the predetermined length of the short fiber is 2 to 3mm.
5. The method for preparing the polylactic acid fiber composite 3D printing material according to claim 1, wherein the drying temperature adopted in the step S3 is 50-80 ℃ and the drying time is 5-12 hours, so that the moisture of each material is less than or equal to 0.05%.
6. The method for preparing a polylactic acid fiber composite 3D printing material according to claim 1, wherein in the step S4, the toughening agent is an acrylic impact modifier added in a weight ratio of 1/100 to 10/100.
7. The method for preparing a polylactic acid fiber composite 3D printing material according to claim 1, wherein in the step S4, the plasticizer is any one or a combination of two of PEG400 and ATBC, and the weight ratio of the plasticizer to the air is 1/1000 to 5/100.
8. The method for preparing a polylactic acid fiber composite 3D printing material according to claim 1, wherein in the step S4, the antioxidant is any one or a combination of two of the antioxidant 168 and the antioxidant 1010, and the added weight ratio is 1/1000 to 5/1000.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410102030.7A CN117922009A (en) | 2024-01-25 | 2024-01-25 | Preparation method of polylactic acid fiber composite 3D printing material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410102030.7A CN117922009A (en) | 2024-01-25 | 2024-01-25 | Preparation method of polylactic acid fiber composite 3D printing material |
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| CN117922009A true CN117922009A (en) | 2024-04-26 |
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| CN202410102030.7A Pending CN117922009A (en) | 2024-01-25 | 2024-01-25 | Preparation method of polylactic acid fiber composite 3D printing material |
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| CN (1) | CN117922009A (en) |
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- 2024-01-25 CN CN202410102030.7A patent/CN117922009A/en active Pending
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