CN110885491A - Conductive photosensitive resin for photocuring 3D printing and preparation method thereof - Google Patents
Conductive photosensitive resin for photocuring 3D printing and preparation method thereof Download PDFInfo
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
- C08L23/0853—Vinylacetate
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
- C08F255/026—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms on to ethylene-vinylester copolymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
- C08F283/008—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00 on to unsaturated polymers
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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
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
- C08L75/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a conductive photosensitive resin for photocuring 3D printing, which comprises the following components in parts by weight: 25-40 parts of ethylene-vinyl acetate copolymer, 20-35 parts of urethane acrylate, 15-30 parts of conductive filler, 1-5 parts of titanate coupling agent, 10-25 parts of neopentyl glycol diacrylate, 0.5-5 parts of dimethyl polysiloxane, 0.5-5 parts of BYK-306 flatting agent and 2-10 parts of benzophenone. The conductive photosensitive resin for 3D printing in the invention takes ethylene-vinyl acetate copolymer and polyurethane acrylate as matrixes, conductive filler is added, and the interaction of the ethylene-vinyl acetate copolymer and the conductive filler is utilized to further enhance the conductivity, so that the conductive photosensitive resin not only maintains the fast curing efficiency, but also has good conductivity.
Description
Technical Field
The invention belongs to the technical field of photocuring 3D printing, and particularly relates to a conductive photosensitive resin for photocuring 3D printing and a preparation method thereof.
Background
In recent years, with the rapid progress of polymer material technology, various novel polymer materials, especially high-strength and multifunctional resin materials, are developing in the directions of safety, environmental protection, recycling and multi-purpose compounding. However, the pure polymer material is an insulating material, and may cause damages such as electrostatic accumulation and electromagnetic interference during use. If the resin pipe is used for manufacturing products such as mining pipes, powder particle conveying pipelines or oil conveying pipelines, logistics pallets and goods shelves and is used in high-risk environments, the resin pipe or the goods carrying framework is easy to cause a large amount of static electricity to accumulate due to friction with the loaded objects, so that explosion or fire is easily caused. Fire accidents caused by electrostatic sparks are common in China during transportation, loading and unloading or production of mineral resources. Therefore, it is necessary to develop a composite conductive resin with stable conductivity and excellent wear resistance and weather resistance.
Photocuring refers to the process of curing and shaping a monomer, oligomer or polymer matrix under the induction of light. The activation energy generated by ultraviolet rays with higher energy in the spectrum can break carbon-carbon bonds in unsaturated resin to generate free radicals, and the matrix can be rapidly cured under the action of an initiator. Laser with specific wavelength and intensity is focused on the surface of the photocuring material, and the photocuring 3D printing is a mode of realizing rapid molding by utilizing the curing process from point to line and from line to surface and the adjustment of vertical height.
Disclosure of Invention
The invention aims to provide a conductive photosensitive resin for photocuring 3D printing and a preparation method thereof, wherein the conductive photosensitive resin has high forming speed and high mechanical strength.
The conductive photosensitive resin for photocuring 3D printing comprises the following components in parts by weight: 25-40 parts of ethylene-vinyl acetate copolymer, 20-35 parts of urethane acrylate, 15-30 parts of conductive filler, 1-5 parts of titanate coupling agent, 10-25 parts of neopentyl glycol diacrylate, 0.5-5 parts of dimethyl polysiloxane, 0.5-5 parts of BYK-306 flatting agent and 2-10 parts of benzophenone.
Preferably, the conductive photosensitive resin for photocuring 3D printing comprises the following components in parts by mass: 30-35 parts of ethylene-vinyl acetate copolymer, 20-25 parts of urethane acrylate, 15-20 parts of conductive filler, 1-3 parts of titanate coupling agent, 20-25 parts of neopentyl glycol diacrylate, 0.5-2 parts of dimethyl polysiloxane, 0.5-2 parts of BYK-306 flatting agent and 2-5 parts of benzophenone.
Further preferably, the conductive photosensitive resin for photocuring 3D printing comprises the following components in parts by mass: 35 parts of ethylene-vinyl acetate copolymer, 25 parts of polyurethane acrylate, 15 parts of conductive filler, 1 part of titanate coupling agent, 21 parts of neopentyl glycol diacrylate, 0.5 part of dimethyl polysiloxane, 0.5 part of BYK-306 flatting agent and 2 parts of benzophenone.
The conductive filler is nano conductive carbon black or copper-aluminum-iron-nickel alloy micron powder; preferably, the copper-aluminum-iron-nickel alloy micron powder comprises CuAl9.5Fe2.5Ni1 micron powder.
The preparation method of the conductive photosensitive resin for photocuring 3D printing comprises the following steps:
(1) sequentially adding ethylene-vinyl acetate copolymer, urethane acrylate, conductive filler, titanate coupling agent, neopentyl glycol diacrylate, dimethyl polysiloxane, BYK-306 flatting agent and benzophenone according to a ratio into a glass three-necked bottle provided with a stirrer and a condenser pipe to obtain a mixed solution;
(2) and (2) heating the mixed solution obtained in the step (1) to a set temperature, and stirring to obtain uniform liquid, namely the conductive photosensitive resin for photocuring 3D printing.
In the step (2), the set temperature is 40-50 ℃, and the stirring time is 60-90 min.
The principle of the invention is as follows: the invention aims to provide a photosensitive resin with conductivity, the interior of an added conductive filler polymer is generally distributed in an amorphous region, the higher the crystallinity of the polymer is, the smaller the proportion of the amorphous region is, the higher the dispersion concentration of the conductive filler in the amorphous region is, the better the conductivity of the composite material is, and the ethylene-vinyl acetate copolymer has higher crystallinity, so the composite resin adopting the ethylene-vinyl acetate copolymer has better conductivity; meanwhile, the ethylene-vinyl acetate copolymer has larger polarity, so the ethylene-vinyl acetate copolymer has better conductivity; therefore, the ethylene-vinyl acetate copolymer and the conductive filler are matched with each other, so that the photosensitive resin has excellent conductive performance.
The invention has the beneficial effects that: 1) the conductive photosensitive resin for 3D printing in the invention takes ethylene-vinyl acetate copolymer and polyurethane acrylate as matrixes, conductive filler is added, and the interaction of the ethylene-vinyl acetate copolymer and the conductive filler is utilized to further enhance the conductivity, so that the conductive photosensitive resin not only maintains the fast curing efficiency, but also has good conductivity. 2) The conductive photosensitive resin of the invention can ensure the conductivity and the mechanical strength by using the neopentyl glycol diacrylate, and simultaneously improve the forming speed. 3) The photosensitive resin prepared by the invention has the characteristics of high molding speed, high mechanical strength and the like, and can be directly applied to photocuring molding to prepare a conductive resin product with a complex structure.
Detailed Description
The present invention will be further described with reference to the following specific examples, which are not intended to limit the spirit of the present invention, and any simple changes or equivalents thereof based on the spirit of the present invention should fall within the scope of the present invention as claimed. Unless otherwise specified, the parts are parts by weight in each example.
Example 1
(1) Preparing raw materials according to the following proportion:
35 parts of ethylene-vinyl acetate copolymer,
25 parts of polyurethane acrylic ester, namely 25 parts of polyurethane acrylic ester,
15 parts of copper-aluminum-iron-nickel alloy micron powder,
1 part of titanate coupling agent, namely 1 part of titanate coupling agent,
21 parts of neopentyl glycol diacrylate ester,
0.5 part of dimethyl polysiloxane, and the like,
0.5 part of BYK-306 leveling agent,
and 2 parts of benzophenone.
(2) Sequentially adding ethylene-vinyl acetate copolymer, urethane acrylate, conductive filler, titanate coupling agent, neopentyl glycol diacrylate, dimethyl polysiloxane, BYK-306 flatting agent and benzophenone according to a ratio into a glass three-necked bottle provided with a stirrer and a condenser pipe;
(3) and (3) heating the mixed solution to 50 ℃, and stirring for about 60min by using a stirrer to obtain uniform liquid, namely the conductive photosensitive resin for photocuring 3D printing is prepared. The test performance of the prepared conductive photosensitive resin after photocuring 3D printing is shown in Table 1.
Example 2
(1) Preparing raw materials according to the following proportion:
20 parts of ethylene-vinyl acetate copolymer,
10 parts of polyurethane acrylic ester, namely 10 parts of polyurethane acrylic ester,
30 parts of copper-aluminum-iron-nickel alloy micron powder,
2 parts of a titanate coupling agent, namely,
30 parts of neopentyl glycol diacrylate ester,
2 parts of dimethyl polysiloxane, namely 2 parts of dimethyl polysiloxane,
2 parts of BYK-306 leveling agent,
4 parts of benzophenone.
(2) Sequentially adding ethylene-vinyl acetate copolymer, urethane acrylate, conductive filler, titanate coupling agent, neopentyl glycol diacrylate, dimethyl polysiloxane, BYK-306 flatting agent and benzophenone according to a ratio into a glass three-necked bottle provided with a stirrer and a condenser pipe;
(3) and (3) heating the mixed solution to 40 ℃, and stirring for about 80min by using a stirrer to obtain uniform liquid, namely the conductive photosensitive resin for photocuring 3D printing is prepared.
The test performance of the prepared conductive photosensitive resin after photocuring 3D printing is shown in Table 1.
Example 3
(1) Preparing raw materials according to the following proportion:
25 parts of ethylene-vinyl acetate copolymer,
25 parts of polyurethane acrylic ester, namely 25 parts of polyurethane acrylic ester,
20 parts of carbon black, namely 20 parts of carbon black,
3 parts of a titanate coupling agent, namely,
15 parts of neopentyl glycol diacrylate ester,
3.5 parts of dimethyl polysiloxane, namely,
3.5 parts of BYK-306 leveling agent,
5 parts of benzophenone.
(2) Sequentially adding ethylene-vinyl acetate copolymer, urethane acrylate, conductive filler, titanate coupling agent, neopentyl glycol diacrylate, dimethyl polysiloxane, BYK-306 flatting agent and benzophenone according to a ratio into a glass three-necked bottle provided with a stirrer and a condenser pipe;
(3) and (3) heating the mixed solution to 45 ℃, and stirring for about 90min by using a stirrer to obtain uniform liquid, namely the conductive photosensitive resin for photocuring 3D printing is prepared.
The test performance of the prepared conductive photosensitive resin after photocuring 3D printing is shown in Table 1.
Example 4
(1) Preparing raw materials according to the following proportion:
20 parts of ethylene-vinyl acetate copolymer,
20 parts of polyurethane acrylic ester, namely 20 parts of polyurethane acrylic ester,
25 parts of carbon black, namely 25 parts of carbon black,
5 parts of a titanate coupling agent, namely,
10 parts of neopentyl glycol diacrylate ester,
5 parts of dimethyl polysiloxane, namely 5 parts of dimethyl polysiloxane,
5 parts of a BYK-306 flatting agent,
10 parts of benzophenone.
(2) Sequentially adding ethylene-vinyl acetate copolymer, urethane acrylate, conductive filler, titanate coupling agent, neopentyl glycol diacrylate, dimethyl polysiloxane, BYK-306 flatting agent and benzophenone according to a ratio into a glass three-necked bottle provided with a stirrer and a condenser pipe;
(3) and (3) heating the mixed solution to 45 ℃, and stirring for about 60min by using a stirrer to obtain uniform liquid, namely the conductive photosensitive resin for photocuring 3D printing is prepared.
The test performance of the prepared conductive photosensitive resin after photocuring 3D printing is shown in Table 1.
Example 5
(1) Preparing raw materials according to the following proportion:
25 parts of ethylene-vinyl acetate copolymer,
25 parts of polyurethane acrylic ester, namely 25 parts of polyurethane acrylic ester,
26 parts of copper-aluminum-iron-nickel alloy micron powder,
1 part of titanate coupling agent, namely 1 part of titanate coupling agent,
20 parts of neopentyl glycol diacrylate ester, namely,
0.5 part of dimethyl polysiloxane, and the like,
0.5 part of BYK-306 leveling agent,
and 2 parts of benzophenone.
(2) Sequentially adding ethylene-vinyl acetate copolymer, urethane acrylate, conductive filler, titanate coupling agent, neopentyl glycol diacrylate, dimethyl polysiloxane, BYK-306 flatting agent and benzophenone according to a ratio into a glass three-necked bottle provided with a stirrer and a condenser pipe;
(3) and (3) heating the mixed solution to 50 ℃, and stirring for about 75min by using a stirrer to obtain uniform liquid, namely the conductive photosensitive resin for the photocuring 3D printing is prepared.
The test performance of the prepared conductive photosensitive resin after photocuring 3D printing is shown in Table 1.
Performance evaluation method:
the tensile property test of the sample is carried out according to the GB/T1040.3 standard, the size of the sample is 100 x 6 x 4mm, the tensile speed is 50mm/min, and the unit is MPa;
the peel strength test of the sample is carried out according to the GB/T2791 standard, and the unit is N/mm;
the conductivity test is carried out according to the GB/T2425and the unit u omega m.
TABLE 1
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 | |
| Tensile strength | 19.2 | 20.5 | 20.3 | 20.9 | 19.9 | 21.5 |
| Peel strength | 6.12 | 5.31 | 5.34 | 5.43 | 5.30 | 6.20 |
| Resistivity of | 6300 | 7200 | 6700 | 8100 | 7600 | 25400 |
Comparative example 1
35 parts of phenolic epoxy resin,
25 parts of polyurethane acrylic ester, namely 25 parts of polyurethane acrylic ester,
15 parts of copper-aluminum-iron-nickel alloy micron powder,
1 part of titanate coupling agent, namely 1 part of titanate coupling agent,
21 parts of neopentyl glycol diacrylate ester,
0.5 part of dimethyl polysiloxane, and the like,
0.5 part of BYK-306 leveling agent,
and 2 parts of benzophenone.
(2) Sequentially adding phenolic epoxy resin, urethane acrylate, conductive filler, titanate coupling agent, neopentyl glycol diacrylate, dimethyl polysiloxane, BYK-306 flatting agent and benzophenone according to a ratio into a glass three-neck flask provided with a stirrer and a condenser pipe;
(3) and (3) heating the mixed solution to 50 ℃, and stirring for about 60min by using a stirrer to obtain uniform liquid, namely the conductive photosensitive resin for photocuring 3D printing is prepared. The test performance of the prepared conductive photosensitive resin after photocuring 3D printing is shown in Table 1.
As can be seen from table 1: the ethylene-vinyl acetate copolymer can be matched with the conductive filler, so that the conductivity of the photosensitive resin is obviously improved.
The embodiments described above are intended to facilitate one of ordinary skill in the art in understanding and using the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (7)
1. The conductive photosensitive resin for photocuring 3D printing is characterized by comprising the following components in parts by mass: 25-40 parts of ethylene-vinyl acetate copolymer, 20-35 parts of urethane acrylate, 15-30 parts of conductive filler, 1-5 parts of titanate coupling agent, 10-25 parts of neopentyl glycol diacrylate, 0.5-5 parts of dimethyl polysiloxane, 0.5-5 parts of BYK-306 flatting agent and 2-10 parts of benzophenone.
2. The conductive photosensitive resin for photocuring 3D printing according to claim 1, which is characterized by comprising the following components in parts by mass: 30-35 parts of ethylene-vinyl acetate copolymer, 20-25 parts of urethane acrylate, 15-20 parts of conductive filler, 1-3 parts of titanate coupling agent, 20-25 parts of neopentyl glycol diacrylate, 0.5-2 parts of dimethyl polysiloxane, 0.5-2 parts of BYK-306 flatting agent and 2-5 parts of benzophenone.
3. The conductive photosensitive resin for photocuring 3D printing according to claim 2, which comprises the following components in parts by mass: 35 parts of ethylene-vinyl acetate copolymer, 25 parts of polyurethane acrylate, 15 parts of conductive filler, 1 part of titanate coupling agent, 21 parts of neopentyl glycol diacrylate, 0.5 part of dimethyl polysiloxane, 0.5 part of BYK-306 flatting agent and 2 parts of benzophenone.
4. The conductive photosensitive resin for photocuring 3D printing as claimed in any one of claims 1 to 3, wherein the conductive filler is nano conductive carbon black or copper aluminum iron nickel alloy micro powder.
5. The conductive photosensitive resin for photocuring 3D printing as recited in claim 4, wherein the copper aluminum iron nickel alloy micropowder is CuAl9.5Fe2.5Ni1 micropowder.
6. A method for preparing the conductive photosensitive resin for photocuring 3D printing according to claim 1, comprising the steps of:
(1) sequentially adding ethylene-vinyl acetate copolymer, urethane acrylate, conductive filler, titanate coupling agent, neopentyl glycol diacrylate, dimethyl polysiloxane, BYK-306 flatting agent and benzophenone according to a ratio into a glass three-necked bottle provided with a stirrer and a condenser pipe to obtain a mixed solution;
(2) and (2) heating the mixed solution obtained in the step (1) to a set temperature, and stirring to obtain uniform liquid, namely the conductive photosensitive resin for photocuring 3D printing.
7. The method for preparing the conductive photosensitive resin for photocuring 3D printing according to claim 1, wherein in the step (2), the temperature is set to be 40-50 ℃, and the stirring time is 60-90 min.
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| CN113105737A (en) * | 2021-03-23 | 2021-07-13 | 湖南创瑾技术研究院有限公司 | Conductive 3D printing material, preparation method and application |
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