CN110591315A - 3D printing wood-plastic composite material with fluorescence effect and preparation method thereof - Google Patents
3D printing wood-plastic composite material with fluorescence effect and preparation method thereof Download PDFInfo
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- CN110591315A CN110591315A CN201910899123.6A CN201910899123A CN110591315A CN 110591315 A CN110591315 A CN 110591315A CN 201910899123 A CN201910899123 A CN 201910899123A CN 110591315 A CN110591315 A CN 110591315A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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Abstract
The invention provides a 3D printing wood-plastic composite material with a fluorescent effect, which comprises the following components in parts by mass: 1-9 wt% of chemical-coated fluorescent powder, 1-20 wt% of modified wood powder, 70-93 wt% of polylactic acid, 1-3 wt% of plasticizer and 1-4 wt% of lubricant; the fluorescent powder is selected from one or two of strontium aluminate doped europium dysprosium, strontium calcium aluminate doped europium dysprosium and europium doped calcium carbonate. According to the invention, the silane coupling agent is used for coating the fluorescent powder, so that the compatibility of the fluorescent powder with the wood-plastic composite material and the additive is good, and the manufactured wood-plastic 3D printing wire has the texture and the fluorescence effect of wood, and has excellent mechanical properties and better processing performance. The material has good mechanical property and luminous effect, and the bending strength of the material is 50-85 MPa; the tensile strength is 45-65 MPa; the elongation at break is 4.5-6%.
Description
Technical Field
The invention belongs to the field of polymer materials and 3D printing materials, and particularly relates to a 3D printing wood-plastic composite material with a fluorescent effect and a preparation method thereof.
Background
The fluorescent powder firstly absorbs various light and heat, converts the light into light energy, then automatically emits light in the dark, can see the light lasting for hours to ten hours, and absorbs various visible light, thereby realizing the illumination function. And can be recycled infinitely, and has strong absorption capacity particularly for short-wave visible light, sunlight and ultraviolet light (UV light) below 450 nm. In real life, people utilize the characteristic of long-time luminescence of fluorescent powder to manufacture weak light sources, and can press various symbols, elements and articles (such as a power switch, a socket, a fishing hook and the like). After illumination, the illuminating parts still illuminate at night or emit light accidentally after power failure, so that people can distinguish surrounding directions, and convenience is brought to work and life. The fluorescent material with ultrafine particles is doped into the wood-plastic 3D material, so that the application field of the wood-plastic 3D material is expanded, and the development of 3D printing is promoted.
In the prior art, a high polymer is usually dyed by an organic fluorescent dye and doped with fluorescent powder, so that the material has a fluorescent light-emitting function. For example, chinese patent application No. 201910127876.5 discloses a 3D printing composite material containing organic fluorescent dye, which is dissolved in an organic solvent and applied to a printed article to obtain a polylactic acid 3D printing wire dyed with the organic fluorescent dye. Printing the article through a 3D printer to obtain a 3D printed article containing the organic fluorescent dye. The preparation method of the 3D printing composite material of the organic fluorescent dye is simple, the artistic expression capacity of 3D printed works is improved, and the practicability is high. The Chinese patent with the application number of 201610424494.5 discloses a noctilucent composite material for 3D printing, which is characterized in that noctilucent powder is subjected to surface treatment, then extruded with high polymer at high temperature, and heated and molded to prepare the noctilucent composite material for 3D printing. The noctilucent composite material keeps good toughness and mechanical property and shows noctilucent luminous performance.
However, the 3D printed composite material dyed by the organic fluorescent dye has an uneven dyeing effect, and the material has poor light emitting stability and affects subsequent processing and forming. The doped fluorescent powder can greatly reduce the processing performance of the material, and the compatibility of the fluorescent powder and most of organic polymer matrixes is poor, so that the preparation process is complex, and the final product is single.
Disclosure of Invention
In view of the above, there is a need to provide a chemically coated fluorescent powder, modified wood powder, a 3D printed wood-plastic composite material with a fluorescent effect, and a preparation method thereof, wherein the wire has both the texture and the fluorescent light emitting effect of wood, and has excellent mechanical properties and good processability.
In order to solve the technical problems, the preparation method of the chemical coating fluorescent powder provided by the technical scheme comprises the following steps:
(1) dissolving 5 wt% of silane coupling agent in 30ml of organic solvent for 10-30 min to obtain a mixed solution;
(2) adding 1-10 g of fluorescent powder into the mixed solution prepared in the step (1), and carrying out ultrasonic separation at normal temperature for 10-40 min;
(3) transferring the suspension prepared in the step (2) to a magnetic stirrer, adding inorganic acid to adjust the pH value to be neutral, and stirring and reacting for 2-6 hours under a sealed condition at normal temperature;
(4) and (3) washing the sticky matter obtained by the reaction in the step (3) with water or ethanol, filtering, removing substances such as residual silane coupling agent and inorganic acid in the reaction, and drying in an oven at 60-85 ℃ for 12-24 h to obtain the chemical coating fluorescent powder with high purity.
Preferably, the organic solvent in step (1) is selected from one or more of absolute ethyl alcohol, 1, 4-dioxane, acetone and chloroform; the silane coupling agent is one or more of 3-glycidoxypropyltrimethoxysilane (KH560), 3- (methacryloyloxy) propyltrimethoxysilane (KH570), vinyltrimethoxysilane (KH171) and vinyltriethoxysilane (KH 151). Most preferably KH 560.
Preferably, the fluorescent powder in the step (2) is selected from one or two of strontium aluminate doped europium dysprosium, strontium calcium aluminate doped europium dysprosium and europium doped calcium carbonate; the granularity of the fluorescent powder is 500-1000 meshes.
Preferably, the inorganic acid in step (3) is one or more of dilute sulfuric acid, dilute hydrochloric acid and carbonic acid.
The invention also aims to provide modified wood flour which comprises the following raw materials in percentage by mass:
5-15 wt% of wood powder, 0.1-1 wt% of hydrogen peroxide, 1-5 wt% of sodium hydroxide and 80-95 wt% of water;
the wood powder is selected from one or more of pine wood powder, poplar wood powder, fir wood powder and oak wood powder, and the mesh number of the wood powder is 50-300 meshes. In a particular embodiment of the invention, the wood flour is selected from poplar wood flour.
The invention provides a preparation method of modified wood flour, which comprises the following steps:
adding wood powder into water, stirring uniformly, adding sodium hydroxide, stirring at normal temperature for 12-24 h, adding hydrogen peroxide, stirring for 10-24 h, filtering to neutrality, and drying for later use.
The invention also aims to provide a 3D printing wood-plastic composite material with a fluorescent effect, which comprises the following components in parts by mass:
1-9 wt% of chemical-coated fluorescent powder, 1-20 wt% of modified wood powder, 70-93 wt% of polylactic acid, 1-3 wt% of plasticizer and 1-4 wt% of lubricant.
Preferably, the molecular weight of the polylactic acid is 105-5 x 106. In a specific embodiment of the present invention, the polylactic acid has a molecular weight of 2 × 106.
Preferably, the plasticizer is selected from one or more of polyethylene glycol, glycerol and dioctyl phthalate. In specific embodiments of the present invention, the plasticizer accounts for 1.5 wt%, 1 wt%, or 2.5 wt% of the wood-plastic 3D printing material.
The lubricant is selected from one or more of zinc stearate, polyethylene wax and butyl stearate. In specific embodiments of the present invention, the lubricant comprises 2.5 wt%, 2 wt%, or 1.5 wt% of the wood-plastic 3D printing material.
The invention provides a preparation method of a 3D printing wood-plastic composite material with a fluorescence effect, which is characterized by comprising the following steps:
mixing the chemically coated fluorescent powder, the modified wood powder, the plasticizer, the lubricant and the polylactic acid to obtain a mixture, granulating, and drying to obtain blended master batch granules; extruding into 1.75 +/-0.05 mm wires, and preparing the 3D printing wood-plastic composite material with the fluorescent effect by an FDM-3D printing technology.
Referring to fig. 1, fig. 1 is a specific process flow diagram of the 3D printing wood-plastic composite material with fluorescent effect provided by the invention, and as can be seen from fig. 1:
reacting a silane coupling agent with the fluorescent powder to obtain coated fluorescent powder; modifying wood flour by a chemical modifier; mixing polylactic acid, chemical coating fluorescent powder, modified wood powder and an additive at a high speed to obtain a mixed material; extruding and dicing the mixed material double screws to obtain master batches, and printing, molding and processing by FDM-3D to obtain the 3D printing wood-plastic composite material with the fluorescent effect.
The method comprises the steps of mixing the chemically coated fluorescent powder, the modified wood powder, the plasticizer, the lubricant and the polylactic acid to obtain a mixture, granulating, and drying to obtain the blended master batch granules. The mixing time of the chemically coated fluorescent powder, the modified wood powder, the plasticizer, the lubricant and the polylactic acid is preferably 5-8 min, and more preferably 6-7 min; in a specific embodiment, the mixing time of the chemical coating fluorescent powder, the modified wood powder, the plasticizer, the lubricant and the polylactic acid is 6 min.
The invention melts and extrudes the mixture through a double-screw extruder and granulates the mixture; the temperatures of sections 1-6 of the extruder are preferably 155-165 ℃, 160-170 ℃, 165-175 ℃, 170-180 ℃, 175-185 ℃ and 170-180 ℃ respectively; the rotating speeds of the main machine and the feeder are 20-30 rpm and 10-15 rpm respectively. In the specific embodiment of the invention, the temperatures of the sections 1-6 of the extruder are 165 ℃, 170 ℃, 175 ℃, 178 ℃, 180 ℃ and 180 ℃.
The drying temperature after granulation is preferably 65 ℃; the drying time is preferably 14-20 h.
The invention provides a 3D printing wood-plastic composite material with a fluorescent effect, which is prepared by granulating the 3D printing wood-plastic composite material with the fluorescent effect or the 3D printing wood-plastic composite material with the fluorescent effect prepared by the preparation method in the technical scheme, extruding and FDM-3D printing and forming.
In the invention, the wood-plastic 3D printing material is prepared by FDM-3D printing type well known to those skilled in the art; the nozzle temperature of the FDM-3D printer is 180-200 ℃. In the specific embodiment of the invention, the temperature of the nozzle is 200 ℃, the printing speed of the FDM-3D printer is 40-60 mm/min, in the specific embodiment of the invention, the printing speed is 50mm/min, the printing wall thickness of the FDM-3D printer is 0.8-1.6 mm, and in the specific embodiment of the invention, the printing wall thickness is 1.2mm.
The reagents used in the examples of the present invention are conventional raw materials or reagents unless otherwise specified, and the experimental methods used are conventional in the art unless otherwise specified. The specific method for testing the mechanical property of the composite material is as follows: the tensile test is executed according to the national standard GB/T1040-; the bending test is carried out according to the national standard GB/T9341-2008, and the bending speed is 5 mm/min.
Compared with the prior art, the invention has the following advantages and effects:
(1) the silane coupling agent is used for coating the fluorescent powder, so that the compatibility of the fluorescent powder with the wood-plastic composite material and the additive is good, and the manufactured wood-plastic 3D printing wire has the texture and the fluorescent light-emitting effect of wood and has good processing performance; also has better mechanical properties (such as bending strength, tensile strength and elongation at break)
(2) The mechanical property of the wood-plastic 3D material is adjusted by adjusting the adding proportion of the chemical coating fluorescent powder so as to adapt to the same working environment and application field.
(3) The wood flour is treated by the chemical modifier, so that hemicellulose and impurities are removed, the color and luster degree of the material are improved, and the thermal stability of the composite material is enhanced.
Drawings
FIG. 1 is a specific process flow diagram of the 3D printing wood-plastic composite material with fluorescence effect provided by the invention;
FIG. 2 is a scanning electron microscope image of KH 560-coated phosphor prepared in example 1 of the present invention;
FIG. 3 is a graph showing the fluorescent effect of a wood-plastic composite printed article prepared in example 1 and added with KH560 coated fluorescent powder;
fig. 4 is a graph of a printed article of the wood-plastic 3D printing material added with the KH 570-coated fluorescent powder and a fluorescent effect thereof, which are prepared in embodiment 2 of the invention;
fig. 5 shows that the wood-plastic 3D printing material added with KH171 coated phosphor prepared in embodiment 3 of the present invention prints splines and wires;
FIG. 6 is a graph of the fluorescent effect of a printed sample strip of the wood-plastic 3D printing material with the addition of unmodified sky blue fluorescent powder prepared in the embodiment 1 of the invention and a wire rod;
fig. 7 is a fluorescence effect diagram and a wire rod of a printed article of the wood-plastic 3D printing material prepared in the embodiment of the invention and comparative example 2.
Detailed Description
For further illustration of the present invention, the following examples are provided to describe the 3D printed wood-plastic composite with fluorescence effect in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
A KH560 coated fluorescent powder and a preparation method of a 3D printing wood-plastic composite material with sky blue fluorescence effect comprise the following steps:
(1) adding 3g of strontium calcium aluminate doped europium dysprosium fluorescent powder into a silane coupling agent KH560 solution with the concentration of 5 wt%, ultrasonically dispersing for 20min at 25 ℃ by using 30ml of absolute ethyl alcohol as a solvent, transferring to a magnetic stirrer for reaction for 4h, filtering, washing, and drying for 12h at 80 ℃. Taking out, crushing to 1500 meshes, and sieving to obtain the chemically coated fluorescent powder for later use;
(2) 100g of poplar powder was sieved through a 1500 mesh sieve. Adding the sieved wood powder into 964ml of water, stirring uniformly, adding 30g of sodium hydroxide, continuing stirring for 24h, adding 6g of hydrogen peroxide, continuing stirring for 20h, filtering, washing until the wood powder is neutral, drying at 80 ℃, and crushing for later use;
(3) mixing 5 wt% of sky blue chemically-coated fluorescent powder obtained in the step (2), 5 wt% of modified wood powder, 1.5 wt% of plasticizer, 2.5 wt% of flexibilizer and 86 wt% of polylactic acid for 15min by a high-speed mixer to form a mixed material, and drying for 4h at 85 ℃ for later use;
(4) and (4) enabling the blend obtained in the step (3) to pass through a double-screw extruder, and cooling and granulating after melt extrusion, wherein the temperature of the double-screw extruder is as follows: the first zone is 160 ℃, the second zone is 165 ℃, the third zone is 165 ℃, the fourth zone is 175 ℃, the fifth zone is 180 ℃, the nose is 175 ℃, and the rotating speeds of the main machine and the feeding machine are respectively 20r/min and 10 r/min. Drying the obtained granules at 85 ℃ for 5h for later use;
(5) and (3) extruding, drawing, wire drawing and forming the granules obtained in the step (4) through a single-screw extruder, and rolling and processing the granules into 3D printing wires, wherein the temperatures of 1-4 sections of the single-screw extruder are 165 ℃, 170 ℃, 175 ℃, 180 ℃, and the drawing speed is 60mm/s, so as to obtain the printing wires.
(6) Carrying out a standard spline printing test on the wound wire rod by using a desktop FDM type 3D printer, wherein the printing temperature (nozzle) is 190 ℃, the diameter of the nozzle is 0.4mm, the printing speed is 60mm/min, and the temperature of a printing platform is not fixed;
a scanning electron microscope image of the cross section of the wood-plastic 3D printing wire with the sky blue fluorescence effect prepared by the embodiment is shown in fig. 2, and a printing sample and the fluorescence effect thereof are shown in fig. 3. And (3) testing the mechanical properties of the 3D printing wood-plastic composite standard sample strip with the sky blue fluorescence effect prepared by 3D printing according to the national standard, wherein the test results of the mechanical properties and the 3D printing properties are shown in Table 1.
Example 2
A preparation method of a KH 570-coated fluorescent powder 3D printing wood-plastic composite material with a light sky blue fluorescent effect comprises the following steps:
(1) adding 4g of strontium calcium aluminate doped europium dysprosium fluorescent powder into a silane coupling agent KH570 solution with the concentration of 5 wt%, taking 30ml of absolute ethyl alcohol as a solvent, carrying out ultrasonic dispersion at 25 ℃ for 20min, transferring to a magnetic stirrer for reaction for 4h, filtering, washing, and drying at 80 ℃ for 12 h. Taking out, crushing to 1500 meshes, and sieving to obtain the chemically coated fluorescent powder for later use;
(2) 100g of poplar powder was sieved through a 1500 mesh sieve. Adding the sieved wood powder into 955ml water, stirring uniformly, adding 35g sodium hydroxide, stirring for 24h, adding 10g hydrogen peroxide, stirring for 20h, filtering, washing until the wood powder is neutral, drying at 80 ℃, and pulverizing for later use;
(3) mixing 3 wt% of the sky blue chemically-coated fluorescent powder obtained in the step (2), 5 wt% of modified wood powder, 1 wt% of plasticizer, 2 wt% of flexibilizer and 89 wt% of polylactic acid for 15min by a high-speed mixer to form a mixed material, and drying for 4h at 85 ℃ for later use;
the experimental procedures for the rest of (4), (5) and (6) were the same as those of example 1. The 3D printing wood-plastic composite material with the fluorescent effect prepared in the embodiment is shown in figure 4, and the mechanical property and the 3D printing material energy test result are shown in table 1.
Example 3
A preparation method of a KH171 coated fluorescent powder 3D printing wood-plastic composite material with a yellow-green fluorescent effect comprises the following steps:
(1) adding 5g of strontium aluminate doped europium dysprosium fluorescent powder into a silane coupling agent KH171 solution with the concentration of 5 wt%, using 30ml of acetone as a solvent, carrying out ultrasonic dispersion at 25 ℃ for 20min, transferring to a magnetic stirrer for reaction for 4h, filtering, washing, and drying at 80 ℃ for 12 h. Taking out, crushing to 1500 meshes, and sieving to obtain the chemically coated fluorescent powder for later use;
(2) the experimental procedure was the same as in (2) in example 1;
(3) mixing the sky blue chemically-coated fluorescent powder obtained in the step (2) by 5 wt%, the modified wood powder by 3 wt%, the plasticizer by 2.5 wt%, the toughening agent by 1.5 wt% and the polylactic acid by 88 wt% for 15min through a high-speed mixer to form a mixed material, and drying for 4h at 85 ℃ for later use;
the experimental procedures for the rest of (4), (5) and (6) were the same as those of example 1. The 3D printing wood-plastic composite material with the fluorescent effect prepared in the embodiment is shown in figure 5, and the mechanical property and the 3D printing material energy test result are shown in table 1.
Comparative example 1
A preparation method of an unmodified sky blue fluorescent powder/wood plastic 3D printing material comprises the following steps:
(1) mixing 5 wt% of unmodified strontium calcium aluminate doped europium dysprosium fluorescent powder, 5 wt% of modified wood powder, 1.5 wt% of plasticizer, 2.5 wt% of flexibilizer and 86 wt% of polylactic acid for 15min by a high-speed mixer according to the mass ratio to form a mixed material, and drying for 4h at 85 ℃ for later use;
the remaining experimental procedure was the same as in example 1. The unmodified sky blue fluorescent powder/wood plastic 3D printing material prepared by the comparative example is shown in figure 6, and the mechanical property and the 3D printing material energy test result are shown in table 1.
Comparative example 2
A preparation method of a wood-plastic 3D printing material without adding fluorescent powder comprises the following steps:
(1) mixing 5 wt% of modified wood powder, 1.5 wt% of plasticizer, 2.5 wt% of flexibilizer and 91 wt% of polylactic acid for 15min by a high-speed mixer according to the mass ratio to form a mixed material, and drying for 4h at 85 ℃ for later use;
the remaining experimental procedure was the same as in example 1. The unmodified yellow-green fluorescent powder/wood plastic 3D printing material prepared by the comparative example is shown in figure 7, and the mechanical property and the 3D printing material energy test result are shown in table 1.
TABLE 1 3D printing wood-plastic composite material with fluorescent effect appearance and performance
The detection result shows that the fluorescent wood-plastic 3D printing material prepared by the invention has excellent mechanical property, good fluorescent effect and wood texture, meets the mechanical strength and appearance requirements of the polylactic acid 3D printing material required in the market, and meets the technical requirements of FDM type 3D printing.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A3D printing wood-plastic composite material with a fluorescent effect is characterized by comprising a blend of chemically coated fluorescent powder, modified wood powder, polylactic acid, a plasticizer and a lubricant; the fluorescent powder comprises, by weight, 1-9% of fluorescent powder, 1-20% of modified wood powder, 70-93% of polylactic acid, 1-3% of plasticizer, 1-4% of lubricant and the balance water.
2. The 3D printing wood-plastic composite material with the fluorescent effect as claimed in claim 1, wherein the plasticizer is selected from one or more of polyethylene glycol, glycerol and dioctyl phthalate; the lubricant is selected from one or more of zinc stearate, polyethylene wax and butyl stearate.
3. The 3D printing wood-plastic composite material with the fluorescent effect as claimed in claim 1, wherein the molecular weight of the polylactic acid is 105～5×106。
4. The 3D printing wood-plastic composite material with the fluorescent effect is characterized in that the particle size of the modified wood powder is 50-300 meshes.
5. The 3D printing wood-plastic composite material with the fluorescent effect according to claim 1, characterized in that the specific steps of modifying wood flour with a chemical modifier are as follows: adding wood powder into water, stirring uniformly, adding sodium hydroxide, stirring at normal temperature for 12-24 h, adding hydrogen peroxide, stirring for 10-24 h, filtering to neutrality, and drying for later use.
6. The 3D printed wood-plastic composite material with the fluorescent effect according to claim 5, wherein the modified wood flour is selected from one or more of pine wood flour, poplar wood flour, fir wood flour and oak wood flour.
7. The 3D printing wood-plastic composite material with the fluorescent effect as claimed in claim 1, wherein the fluorescent powder is selected from one of strontium aluminate doped with europium dysprosium, strontium calcium aluminate doped with europium dysprosium, and europium doped calcium carbonate.
8. A preparation method of a 3D printing wood-plastic composite material with a fluorescence effect is characterized by comprising the following steps:
s1, coating the fluorescent powder with a silane coupling agent;
s2, modifying the wood powder by using a chemical modifier;
s3, forming a blend by the fluorescent powder modified in the step S1, the wood powder modified in the step S2, polylactic acid, a plasticizer and a lubricant through a high-speed mixer;
s4, melting, extruding and granulating the blend obtained in the step S3 through a double-screw extruder, wherein the temperature of 1-6 sections of the extruder is 155-165 ℃, 160-170 ℃, 165-175 ℃, 170-180 ℃, 175-185 ℃ and 170-180 ℃, and the rotating speed of a host and a feeding machine is 20-30 rpm and 10-15 rpm respectively, so that the 3D printing wood-plastic composite particles with the fluorescence effect are obtained;
s5, drying the particles prepared in the step S4, and preparing the particles into a 3D printing wire through a single-screw extruder; the diameter of the prepared 3D printing wire rod is 1.75mm, and the diameter error is within +/-0.05.
9. The preparation method of the 3D printing wood-plastic composite material with the fluorescent effect according to claim 8, wherein the step of preparing the coated fluorescent powder comprises the following steps:
s11, dissolving 5 wt% of silane coupling agent in 30ml of organic solvent for 10-30 min to obtain a mixed solution;
s12, adding 1-10 g of fluorescent powder into the mixed solution prepared in the step S11, and carrying out ultrasonic separation at normal temperature for 10-40 min;
s13, transferring the suspension prepared in the step S12 to a magnetic stirrer, adding inorganic acid to adjust the pH value to be neutral, and stirring and reacting for 2-6 hours under a sealed condition at normal temperature;
and S14, washing the sticky matter obtained in the step S13 with water or ethanol, filtering, removing residual silane coupling agent, inorganic acid and other substances in the reaction, and drying in an oven at 60-85 ℃ for 12-24 h to obtain the chemical coating fluorescent powder with high purity.
10. The preparation method of 3D printing wood plastic composite material with fluorescence effect according to claim 8, wherein the silane coupling agent is one of 3-glycidoxypropyltrimethoxysilane (KH560), 3- (methacryloyloxy) propyltrimethoxysilane (KH570), vinyltrimethoxysilane (KH171) and vinyltriethoxysilane (KH 151);
the method comprises the following steps of coating fluorescent powder with a silane coupling agent: adding fluorescent powder into an organic solvent, adding a silane coupling agent after ultrasonic dispersion, wherein the absolute dry mass ratio of the silane coupling agent to the fluorescent powder is 0.1-2; adding dilute acid to regulate pH value to neutrality, vacuum filtering, and stoving at 60 deg.c.
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| CN115821423A (en) * | 2022-12-06 | 2023-03-21 | 江南大学 | Polylactic acid fluorescent solar energy collection optical fiber and preparation method and application thereof |
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