CN115584124B - Nylon elastomer powder for selective laser sintering and preparation method thereof - Google Patents
Nylon elastomer powder for selective laser sintering and preparation method thereof Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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Abstract
The invention relates to the technical field of additive manufacturing materials, in particular to nylon elastomer powder for selective laser sintering and a preparation method thereof, wherein the nylon elastomer powder comprises the following raw materials in parts by mass: 100 parts of nylon elastomer, 3-5 parts of potassium titanate whisker, 1-3 parts of modifier, 0.1-0.5 part of glass microsphere, 0.1-0.5 part of dispersing agent and 0.1-0.3 part of flow aid. The nylon elastomer powder is uniform and stable in distribution, high in recycling times, low in energy required by laser sintering, low in sintering temperature, high in compactness of a sintered product and excellent in mechanical strength.
Description
Technical Field
The invention relates to the technical field of additive manufacturing materials, in particular to nylon elastomer powder for selective laser sintering and a preparation method thereof.
Background
The material is one of the keys of the development of additive manufacturing technology and is also the bottleneck limiting the technical development of the material, and the development of a novel material suitable for additive manufacturing has great application prospect and significance. Selective laser sintering technology is one of the most important processing technologies for additive manufacturing. Among materials usable for laser sintering, polymer materials are attracting attention due to their excellent properties, but polymers usable for selective laser sintering processes are limited, and nylon, TPU, PP, etc. are mainly on the market at present.
Nylon elastomers are polyether amide block copolymers composed of rigid polyamide and flexible polyether blocks. Compared with other thermoplastic elastomers, the thermoplastic elastomer has the characteristics of light weight, high rebound resilience, excellent low temperature resistance and the like, and has wide application in the fields of sports equipment, consumer electronics, waterproof clothing, medical treatment and the like. Therefore, developing a nylon elastomer powder suitable for selective laser sintering has very important significance and market prospect.
Disclosure of Invention
The nylon elastomer powder for selective laser sintering is uniform and stable in distribution, high in recycling frequency, low in energy required by laser sintering, low in sintering temperature, high in compactness of a sintered product and excellent in mechanical strength.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the nylon elastomer powder for selective laser sintering comprises the following raw materials in parts by mass: 100 parts of nylon elastomer, 3-5 parts of potassium titanate whisker, 1-3 parts of modifier, 0.1-0.5 part of glass bead, 0.1-0.5 part of dispersing agent and 0.1-0.3 part of flow aid;
the modifier comprises calcium stearate or zinc stearate and N-ethylene bis-stearamide, and the weight ratio of the calcium stearate or the zinc stearate to the N-ethylene bis-stearamide is 1:2.2-3.4.
Preferably, the flow aid is one or a mixture of more than two of fumed silica, fumed aluminum oxide and nanometer titanium dioxide.
Preferably, the nylon is one of PA6, PA12 and PA 11.
Preferably, the dispersing agent is one or more of sodium tripolyphosphate and sodium dodecyl sulfate.
Preferably, the particle size of the glass beads is 10-20 μm.
A preparation method of nylon elastomer powder for selective laser sintering comprises the following steps:
step one: adding the nylon elastomer, the potassium titanate whisker and the modifier into a high-speed mixer according to the ratio, and mixing for 25-30 min at 35-55 ℃; adding glass beads and a dispersing agent, mixing for 25-40min at 35-55 ℃, and extruding and granulating by a bolt screw extruder to obtain nylon elastomer granules;
step two: cryogenic grinding is carried out on the obtained nylon elastomer granules at the temperature of minus 170 ℃ to minus 160 ℃, then drying is carried out for 4 hours at the temperature of 90 ℃ in a blast drying box, and powder particles are obtained after air flow classification screening, wherein the particle size range of the powder particles is 10-150 mu m;
step three: and (3) putting the obtained powder particles and the flow aid into a high-speed mixer according to the ratio, mixing and stirring for 25-30 min at 35-55 ℃, and uniformly mixing and stirring to obtain the nylon elastomer powder for selective laser sintering.
The invention has the following beneficial effects:
the nylon elastomer powder for selective laser sintering provided by the invention is uniform and stable in distribution, high in recycling frequency, low in energy required by laser sintering, low in sintering temperature, high in compactness of a sintered product and excellent in mechanical strength. The addition of the potassium titanate whisker improves the thermal stability of the material and increases the recycling times of the material. The addition of the modifier can induce the advanced crystallization of the nylon elastomer material and reduce the energy required by laser sintering; meanwhile, the lubricating effect is achieved, so that the movement resistance among molecular chains of the material is reduced, and the compactness of the sintered product is improved. The addition of the glass beads and the dispersing agent ensures that all the components are fused uniformly, and the mechanical strength of the material is improved.
Drawings
FIG. 1 is a schematic diagram of the structure of a sintered test strip according to the present invention.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments.
Example 1
5kg of PA12 nylon elastomer, 150g of potassium titanate whisker, 15.6g of calcium stearate and 34.4g of N-ethylene double-hard-ester amide are added into a high-speed mixer, mixed for 30min at 40 ℃, then 5g of glass beads with the particle size of 15um and 5g of sodium tripolyphosphate are added, mixed for 30min at 40 ℃, and extruded and granulated by a double-screw extruder to obtain nylon elastomer granules;
the obtained nylon elastomer granules are subjected to cryogenic grinding at the temperature of minus 170 ℃ to minus 160 ℃, then dried for 4 hours at the temperature of 90 ℃ in a blast drying box, and subjected to air flow classification screening to obtain powder particles with the granularity range of 10-150 mu m;
the obtained powder particles and 5g of fumed silica are placed into a high-speed mixer, and mixed and stirred for 30min at 40 ℃ to obtain the nylon elastomer powder for selective laser sintering.
Example two
5kg of PA12 nylon elastomer, 200g of potassium titanate whisker, 26.4g of calcium stearate and 73.6g of N-ethylene double-hard-ester amide are added into a high-speed mixer, mixed for 30min at 40 ℃, then 15g of glass beads with the particle size of 10um and 15g of sodium tripolyphosphate are added, mixed for 30min at 40 ℃, and extruded and granulated by a double-screw extruder to obtain nylon elastomer granules;
the obtained nylon elastomer granules are subjected to cryogenic grinding at the temperature of minus 170 ℃ to minus 160 ℃, then dried for 4 hours at the temperature of 90 ℃ in a blast drying box, and subjected to air flow classification screening to obtain powder particles with the granularity range of 10-150 mu m;
the obtained powder particles and 10g of fumed silica were placed in a high-speed mixer, and mixed and stirred at 55 ℃ for 25 minutes to obtain nylon elastomer powder for selective laser sintering.
Example III
5kg of PA12 nylon elastomer, 250g of potassium titanate whisker, 34.1g of calcium stearate and 115.9g of N-ethylene double-hard-ester amide are added into a high-speed mixer, mixed for 30min at 40 ℃, then 25g of glass beads with the particle size of 20um and 25g of sodium tripolyphosphate are added, mixed for 30min at 40 ℃, and extruded and granulated by a double-screw extruder to obtain nylon elastomer granules;
the obtained nylon elastomer granules are subjected to cryogenic grinding at the temperature of minus 170 ℃ to minus 160 ℃, then dried for 4 hours at the temperature of 90 ℃ in a blast drying box, and subjected to air flow classification screening to obtain powder particles with the granularity range of 10-150 mu m;
the obtained powder particles and 15g of fumed silica are placed in a high-speed mixer, and mixed and stirred for 30min at 35 ℃ to obtain the nylon elastomer powder for selective laser sintering.
Example IV
5kg of PA11 nylon elastomer, 200g of potassium titanate whisker, 26.4g of calcium stearate and 73.6g of N-ethylene double-hard-ester amide are added into a high-speed mixer, mixed for 40min at 35 ℃, then 15g of glass beads with the particle size of 10um and 15g of sodium dodecyl sulfate are added, mixed for 40min at 35 ℃, and extruded and granulated by a double-screw extruder to obtain nylon elastomer granules;
the obtained nylon elastomer granules are subjected to cryogenic grinding at the temperature of minus 170 ℃ to minus 160 ℃, then dried for 4 hours at the temperature of 90 ℃ in a blast drying box, and subjected to air flow classification screening to obtain powder particles with the granularity range of 10-150 mu m;
the obtained powder particles and 10g of nano titanium dioxide are put into a high-speed mixer, and mixed and stirred for 30min at 45 ℃ to obtain the nylon elastomer powder for selective laser sintering.
Example five
5kg of PA6 nylon elastomer, 200g of potassium titanate whisker, 26.4g of zinc stearate and 73.6g of N-ethylene double-hard-ester amide are added into a high-speed mixer, mixed for 25min at 55 ℃, then 25g of glass beads with the particle size of 20um and 25g of sodium tripolyphosphate are added, mixed for 25min at 55 ℃, and extruded and granulated by a double-screw extruder to obtain nylon elastomer granules;
the obtained nylon elastomer granules are subjected to cryogenic grinding at the temperature of minus 170 ℃ to minus 160 ℃, then dried for 4 hours at the temperature of 90 ℃ in a blast drying box, and subjected to air flow classification screening to obtain powder particles with the granularity range of 10-150 mu m;
the obtained powder particles and 15g of nano aluminum oxide are placed into a high-speed mixer, and mixed and stirred for 30min at 40 ℃ to obtain the nylon elastomer powder for selective laser sintering.
Comparative example one
The difference from example 2 is that the mixture of calcium stearate and N-ethylenebisstearamide is not added as a modifier.
Adding 5kg of PA12 nylon elastomer and 200g of potassium titanate whisker into a high-speed mixer, mixing for 30min at 40 ℃, adding 15g of glass beads with the particle size of 10um and 15g of sodium tripolyphosphate, mixing for 30min at 40 ℃, and extruding and granulating by a double-screw extruder to obtain nylon elastomer granules;
the obtained nylon elastomer granules are subjected to cryogenic grinding at the temperature of minus 170 ℃ to minus 160 ℃, then dried for 4 hours at the temperature of 90 ℃ in a blast drying box, and subjected to air flow classification screening to obtain powder particles with the granularity range of 10-150 mu m;
the obtained powder particles and 10g of fumed silica were placed in a high-speed mixer, and mixed and stirred at 55 ℃ for 25 minutes to obtain nylon elastomer powder for selective laser sintering.
Comparative example two
The difference from example 2 is that no glass beads or dispersing agent are added.
5kg of PA12 nylon elastomer, 200g of potassium titanate whisker, 26.4g of calcium stearate and 73.6g of N-ethylene double-hard ester amide are added into a high-speed mixer, mixed for 30min at 40 ℃, and extruded and granulated by a double-screw extruder to obtain nylon elastomer granules; the obtained nylon elastomer granules are subjected to cryogenic grinding at the temperature of minus 170 ℃ to minus 160 ℃, then dried for 4 hours at the temperature of 90 ℃ in a blast drying box, and subjected to air flow classification screening to obtain powder particles with the granularity range of 10-150 mu m;
the obtained powder particles and 10g of fumed silica were placed in a high-speed mixer, and mixed and stirred at 55 ℃ for 25 minutes to obtain nylon elastomer powder for selective laser sintering.
Selective laser sintering experiment and test
The nylon elastomer powders of the above examples and comparative examples were subjected to selective laser sintering, respectively, and the sintering temperature, the laser energy density for sintering, the tensile strength, the elongation and the density of the sintered product were tested. Sintering the test bars as shown in fig. 1; the energy density of the laser for sintering is according to the formula: laser power/(scan speed x scan pitch) calculation; tensile strength and elongation were measured according to GB/T528 standard; the density was determined according to the method of GB 1033; the test results are shown in Table 1:
TABLE 1
Repeated sintering test
The nylon elastomer powder of examples one to three was subjected to selective laser sintering of the sample bars, repeated 10 times of printing, and the tensile properties of the sintered sample bars after the first, 5 and 10 times of printing were tested, respectively, and the data are shown in table 2:
TABLE 2
As can be seen from tables 1 and 2, the nylon elastomer powder for selective laser sintering provided by the invention has the advantages of high recycling times, low energy required by laser sintering, low sintering temperature, high compactness of sintered products and high mechanical strength. It can be seen from example 2 and comparative example 1 that the addition of the mixed modifier of calcium stearate and N-ethylenebisstearamide reduces the laser energy density required by laser sintering and forming of the material, and improves the compactness of the sintered part, thereby improving the mechanical properties of the sintered part. It can be seen from example 2 and comparative example 2 that the addition of the glass beads and the dispersing agent improves the degree of fusion of the components and improves the mechanical strength of the sintered part.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (6)
1. The nylon elastomer powder for selective laser sintering is characterized by comprising the following raw materials in parts by weight: 100 parts of nylon elastomer, 3-5 parts of potassium titanate whisker, 1-3 parts of modifier, 0.1-0.5 part of glass bead, 0.1-0.5 part of dispersing agent and 0.1-0.3 part of flow aid;
the modifier comprises calcium stearate or zinc stearate and N-ethylene bis-stearamide, and the weight ratio of the calcium stearate or the zinc stearate to the N-ethylene bis-stearamide is 1:2.2-3.4.
2. The nylon elastomer powder for selective laser sintering according to claim 1, wherein the flow aid is one or a mixture of two or more of fumed silica, fumed aluminum oxide and nano titanium dioxide.
3. A nylon elastomer powder for selective laser sintering according to claim 1, wherein the hard segment of the nylon elastomer is one of PA6, PA12, PA 11.
4. A nylon elastomer powder for selective laser sintering as defined in claim 1, wherein the dispersant is one or more of sodium tripolyphosphate and sodium dodecyl sulfate.
5. A nylon elastomer powder for selective laser sintering according to claim 1, wherein the glass beads have a particle size of 10 to 20 μm.
6. A method for producing the nylon elastomer powder for selective laser sintering according to any one of claims 1 to 5, comprising the steps of:
step one: adding the nylon elastomer, the potassium titanate whisker and the modifier into a high-speed mixer according to the ratio, and mixing for 25-30 min at 35-55 ℃; adding glass beads and a dispersing agent, mixing at 35-55 ℃ for 25-40min, and extruding and granulating by a double-screw extruder to obtain nylon elastomer granules;
step two: cryogenic pulverizing nylon elastomer granules at-170 ℃ to-160 ℃, drying in a forced air drying box at 90 ℃ for 4 hours, and carrying out air flow classification screening to obtain powder particles, wherein the particle size range of the powder particles is 10-150 mu m;
step three: and (3) putting the obtained powder particles and the flow aid into a high-speed mixer according to the ratio, and mixing and stirring for 25-30 min at the temperature of 35-55 ℃ to obtain the nylon elastomer powder for selective laser sintering.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0346149A2 (en) * | 1988-06-09 | 1989-12-13 | Tonen Chemical Corporation | Thermoplastic resin composition incorporated with whisker and process for producing the same |
| CN102634191A (en) * | 2012-05-15 | 2012-08-15 | 金发科技股份有限公司 | Permanent antistatic nylon elastomer material and preparation method thereof |
| CN113667130A (en) * | 2021-08-19 | 2021-11-19 | 郑州大学 | Thermoplastic polyamide elastomer powder for selective laser sintering and preparation method thereof |
| CN113930068A (en) * | 2021-11-08 | 2022-01-14 | 万华化学（宁波）有限公司 | Preparation method of hollow glass bead master batch |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPWO2005063876A1 (en) * | 2003-12-25 | 2007-07-19 | Jsr株式会社 | Thermoplastic elastomer composition, method for producing the same, and molded article |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0346149A2 (en) * | 1988-06-09 | 1989-12-13 | Tonen Chemical Corporation | Thermoplastic resin composition incorporated with whisker and process for producing the same |
| CN102634191A (en) * | 2012-05-15 | 2012-08-15 | 金发科技股份有限公司 | Permanent antistatic nylon elastomer material and preparation method thereof |
| CN113667130A (en) * | 2021-08-19 | 2021-11-19 | 郑州大学 | Thermoplastic polyamide elastomer powder for selective laser sintering and preparation method thereof |
| CN113930068A (en) * | 2021-11-08 | 2022-01-14 | 万华化学（宁波）有限公司 | Preparation method of hollow glass bead master batch |
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