CN113817324A - Photocuring 3D printing silicone rubber ink and preparation method thereof - Google Patents
Photocuring 3D printing silicone rubber ink and preparation method thereof Download PDFInfo
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- CN113817324A CN113817324A CN202111262836.5A CN202111262836A CN113817324A CN 113817324 A CN113817324 A CN 113817324A CN 202111262836 A CN202111262836 A CN 202111262836A CN 113817324 A CN113817324 A CN 113817324A
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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
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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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
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
Abstract
The invention provides photocuring 3D printing silicone rubber ink and a preparation method thereof, and belongs to the technical field of 3D printing high-molecular silicone rubber. The paint comprises the following components in parts by mass: 30-50 parts of polysiloxane, wherein the end part of the polysiloxane contains vinyl; 1.25-10 parts of a siloxane crosslinking agent, wherein the siloxane crosslinking agent contains 2-3 sulfydryl groups; 0.5-2 parts of a photoinitiator; 40-60 parts of addition type thermosetting silicone rubber; 0.1-2 parts of an inhibitor. The photocuring 3D printing silicone rubber ink disclosed by the invention integrates the advantages of high-precision forming of photocuring printing and high mechanical property of thermosetting silicone rubber forming, is a compatible silicone rubber system, and can improve the mechanical strength by adding the thermosetting silicone rubber. The invention has scientific formula, has higher photocuring speed, can be cured within 5s at normal temperature, and has no obvious peculiar smell and shrinkage after curing.
Description
Technical Field
The invention relates to the technical field of 3D printing high-molecular silicone rubber, in particular to photocuring 3D printing silicone rubber ink and a preparation method thereof.
Background
The silicon rubber is prepared by taking Si-O-Si bond as a main chain and taking-CH as a side chain3The linear polysiloxane polymer of (1). At normal temperature, the silicon rubber has the typical characteristics of high elasticity, and also has the properties of fatigue resistance, electric insulation, wear resistance, corrosion resistance, solvent resistance, air impermeability, water impermeability and the like. The silicon rubber can be prepared into a porous polymer elastomer material after foaming, has the characteristics of low relative density, high specific surface area, large compressible deformation, excellent damping performance and the like, can be used as damping, sound insulation, shock absorption and buffering materials, and has common application in the fields of medical treatment and the like.
The 3D printing technology, also called additive manufacturing technology, is a method for preparing three-dimensional materials by layer-by-layer accumulation of raw materials, is a bottom-up manufacturing method, can realize digital compounding or combination of materials from the material aspect, can realize the manufacturing from a nanometer level to a meter level structure from the scale aspect, and provides a brand-new and flexible scheme for the preparation and molding of silicon rubber materials.
At present, 3D prints silicon rubber main forming mode and prints and the photocuring shaping for directly writing 3D, for directly writing 3D and printing, photocuring shaping has higher printing precision, can realize the high accuracy shaping to complicacy, thin wall and other hollow out construction homoenergetic. Therefore, in recent years, light-cured 3D printing silicone rubber attracts more and more attention of researchers, such as light-cured 3D printing molding of silicone rubber by a desktop Digital Light Processing (DLP) printer using silicone methacrylate; the vinyl-terminated polydimethylsiloxane mixed with the mercaptan functionalized polysiloxane is used for carrying out photocuring 3D printing, and the silicon dioxide particles are used for improving the performance, so that the photocuring printing forming of the silicon rubber is also realized. However, the existing photocuring 3D printing silicone rubber still has the problem of poor mechanical properties.
Disclosure of Invention
In view of this, the present invention provides a photocuring 3D printing silicone rubber ink and a preparation method thereof. The photocuring 3D printing silicone rubber ink provided by the invention is excellent in mechanical property.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides photocuring 3D printing silicone rubber ink which comprises the following components in parts by mass:
30-50 parts of polysiloxane, wherein the end part of the polysiloxane contains vinyl;
1.25-10 parts of a siloxane crosslinking agent, wherein the siloxane crosslinking agent contains 2-3 sulfydryl groups;
0.5-2 parts of a photoinitiator;
40-60 parts of addition type thermosetting silicone rubber;
0.1-2 parts of an inhibitor.
Preferably, the photocuring 3D printing silicone rubber ink comprises the following components in parts by mass:
30-50 parts of polysiloxane, 2-5 parts of siloxane cross-linking agent, 0.5-1.2 parts of photoinitiator, 40-60 parts of addition type thermosetting silicone rubber and 0.5-1 part of inhibitor.
Preferably, the photocuring 3D printing silicone rubber ink comprises the following components in parts by mass:
50 parts of polysiloxane, 3 parts of siloxane cross-linking agent, 1.5 parts of photoinitiator, 45 parts of addition type thermosetting silicone rubber and 0.5 part of inhibitor.
Preferably, the viscosity of the addition type thermosetting silicone rubber is 1000 to 6000 cps.
Preferably, the addition type heat-curable silicone rubber comprises a ceramic Sylgard-184 silicone rubber.
Preferably, the polysiloxane has the viscosity of 500-10000 cst and the vinyl content of 0.1-0.8 mmol/g.
Preferably, the silicone crosslinker comprises one or more of (mercapto) methylsiloxane-dimethylsiloxane copolymer, trimethylolpropane tris (2-mercaptoacetate), 2-mercapto-N-methylbenzamide, mercaptopolyethylene glycol maleimide, mercaptopolyethylene glycol acrylamide, hydroxypolyethylene glycol mercapto, methyl 2-mercaptobenzoate, and trimethylolpropane tris (3-mercaptopropionate).
Preferably, the photoinitiator is a free radical photoinitiator comprising one or more of TOP-35819, IRGACURE 184 and IRGACURE 1173.
Preferably, the inhibitor is a heat-curing addition type inhibitor comprising one or more of 2-methyl-3-yn-2-ol, 3-methyl-1-yn-3-ol, phenylacetylene, tert-butyl peroxide, dimethyl sulfoxide, diphenyl sulfoxide, ethynyl cyclohexanol, diallyl maleate, diethyl fumarate and vinylcyclo bodies.
The invention also provides a preparation method of the photocuring 3D printing silicone rubber ink, which comprises the following steps:
and mixing polysiloxane, a siloxane cross-linking agent, a photoinitiator, addition type thermosetting silicone rubber and an inhibitor to obtain the photocuring 3D printing silicone rubber ink.
The invention provides photocuring 3D printing silicone rubber ink which comprises the following components in parts by mass: 30-50 parts of polysiloxane, wherein the end part of the polysiloxane contains vinyl; 1.25-10 parts of a siloxane crosslinking agent, wherein the siloxane crosslinking agent contains 2-3 sulfydryl groups; 0.5-2 parts of a photoinitiator; 40-60 parts of addition type thermosetting silicone rubber; 0.1-2 parts of an inhibitor.
The photocuring 3D printing silicone rubber ink disclosed by the invention integrates the advantages of high-precision forming of photocuring printing and high mechanical property of thermosetting silicone rubber forming, is a compatible silicone rubber system, and can improve the mechanical strength by adding the thermosetting silicone rubber. According to the formula, the polysiloxane containing vinyl at the end, the siloxane cross-linking agent containing 2-3 sulfydryl, the photoinitiator, the addition type thermosetting silicone rubber and the inhibitor are scientifically mixed to enable the curing agent to have a high photocuring speed, can be cured within 5 seconds at normal temperature, and is free of obvious peculiar smell and shrinkage after curing.
Further, the ceramic Sylgard-184 silicon rubber can be replaced by other addition type thermosetting silicon rubber with different mechanical strengths, so that 3D printing and forming of different silicon rubber systems under different application environments are realized.
Drawings
FIG. 1 is a stress-strain curve of a material product printed with the photocuring 3D printing silicone rubber ink prepared in examples 1-3;
fig. 2 is a pictorial view of a 3D-printed silicone rubber molded sample prepared in example 1.
Detailed Description
The invention provides photocuring 3D printing silicone rubber ink which comprises the following components in parts by mass:
30-50 parts of polysiloxane, wherein the end part of the polysiloxane contains vinyl;
1.25-10 parts of a siloxane crosslinking agent, wherein the siloxane crosslinking agent contains 2-3 sulfydryl groups;
0.5-2 parts of a photoinitiator;
40-60 parts of addition type thermosetting silicone rubber;
0.1-2 parts of an inhibitor.
In the invention, the photocuring 3D printing silicone rubber ink preferably comprises the following components in parts by mass:
30-50 parts of polysiloxane, 2-5 parts of siloxane cross-linking agent, 0.5-1.2 parts of photoinitiator, 40-60 parts of addition type thermosetting silicone rubber and 0.5-1 part of inhibitor, and more preferably comprises the following components in parts by mass:
50 parts of polysiloxane, 3 parts of siloxane cross-linking agent, 1.5 parts of photoinitiator, 45 parts of addition type thermosetting silicone rubber and 0.5 part of inhibitor.
In the present invention, unless otherwise specified, all the raw materials used are commercially available in the art.
In the present invention, the addition type heat-curable silicone rubber preferably includes Toxicogard-184 and/or other heat-curable silicone rubber of different mechanical strength, more preferably, Toxicogard-184 silicone rubber. When the addition type heat-curing silicone rubber is preferably a mixture of a plurality of addition type heat-curing silicone rubbers, the amount of each addition type heat-curing silicone rubber used in the present invention is not particularly limited, and any mixture ratio can be used.
In the invention, the addition type thermosetting silicone rubber comprises a precursor and a curing agent, the proportion of the precursor and the curing agent in the invention is only required to be prepared according to the requirements of commercial silicone rubber, and the specific proportion of the precursor and the curing agent in the ceramic Sylgard-184 silicone rubber is 10: 1.
in the invention, the viscosity of the addition type thermosetting silicone rubber is preferably 1000-6000 cps, and more preferably 2500-3500 cps.
In the present invention, the mass part of the addition type thermosetting silicone rubber contains the mass of the curing agent.
In the invention, the viscosity of the polysiloxane is preferably 500-10000 cst, more preferably 5000cst, and the vinyl content is preferably 0.1-0.8 mmol/g, more preferably 0.35-0.6 mmol/g.
In the present invention, the silicone crosslinking agent preferably includes one or more of (mercapto) methylsiloxane-dimethylsiloxane copolymer, trimethylolpropane tris (2-mercaptoacetate), 2-mercapto-N-methylbenzamide, mercaptopolyethylene glycol maleimide, mercaptopolyethylene glycol acrylamide, hydroxypolyethylene glycol mercapto, methyl 2-mercaptobenzoate, and trimethylolpropane tris (3-mercaptopropionate). When the silicone crosslinking agent is preferably a mixture of a plurality of kinds, the ratio of the substances in the mixture is not particularly limited, and the mixture may be used in any ratio.
In the present invention, the photoinitiator is preferably a radical type photoinitiator, and the radical type photoinitiator preferably includes one or more of TOP-L, IRGACURE 819, IRGACURE 184 and IRGACURE 1173. When the photoinitiator is preferably a mixture of a plurality of photoinitiators, the ratio of the amounts of the respective substances in the mixture is not particularly limited, and the mixture may be used in any ratio.
In the present invention, the inhibitor is preferably a heat-curing addition type inhibitor, and the heat-curing addition type inhibitor preferably includes one or more of 2-methyl-3-yn-2-ol, 3-methyl-1-yn-3-ol, phenylacetylene, tert-butyl peroxide, dimethyl sulfoxide, diphenyl sulfoxide, ethynyl cyclohexanol, diallyl maleate, diethyl fumarate, and vinylcyclo. When the inhibitor is preferably a mixture of a plurality of substances, the ratio of the substances in the mixture is not particularly limited, and the mixture may be used in any ratio.
The invention also provides a preparation method of the photocuring 3D printing silicone rubber ink, which comprises the following steps:
and mixing polysiloxane, a siloxane cross-linking agent, a photoinitiator, addition type thermosetting silicone rubber and an inhibitor to obtain the photocuring 3D printing silicone rubber ink. The specific mixing mode is not particularly limited, and the method is known to those skilled in the art, specifically, stirring for 15-45 min in the dark, then vacuumizing to remove bubbles, and finally sealing and storing in the dark.
The application of the photo-curing 3D printing silicone rubber ink is not particularly limited, and the method known to those skilled in the art can be adopted, and specifically, the method comprises the following steps:
and printing the photocuring 3D printing silicone rubber ink by using a photocuring 3D printer, removing the residual ink on the surface of the obtained sample, and then carrying out heat treatment.
In the invention, the temperature of the heat treatment is preferably 100-150 ℃, more preferably 130 ℃, and the time is preferably 2-8 h, more preferably 4 h.
In order to further illustrate the present invention, the following describes the photo-curing 3D printing silicone rubber ink and the preparation method thereof in detail with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Taking 50 parts by mass of polysiloxane (with the viscosity of 5000cst and the vinyl content of 0.6mmol/g) containing vinyl at the end, adding 5 parts by mass of cross-linking agent (mercapto) methyl siloxane-dimethyl siloxane copolymer, adding 0.5 part by mass of photoinitiator TPO-L, and mixing uniformly; weighing 50 parts by mass of Sylgard-184 silicon rubber (containing 0.5 part of curing agent) and adding 0.4 part by mass of inhibitor diallyl maleate; mixing the above materials, stirring at room temperature in dark for 25min, and vacuumizing to remove bubbles. And sealing and keeping away from light to obtain the final product.
And (3) printing the prepared printing ink on a complex lattice-shaped structural member by using a photocuring 3D printer (DLP molding), cleaning for 10min by using n-hexane ultra-clear after printing, and then curing for 6h in an oven at 140 ℃ to obtain a sample shown in figure 2.
Example 2
Taking 50 parts by mass of polysiloxane (with the viscosity of 5000cst and the vinyl content of 0.6mmol/g) containing vinyl at the end, adding 2.5 parts by mass of cross-linking agent (mercapto) methyl siloxane-dimethyl siloxane copolymer, adding 0.5 part by mass of photoinitiator TPO-L, and mixing uniformly; weighing 50 parts by mass (containing 25 parts by mass of curing agent) of thermocuring silica gel (Shenzhen red leaf silica gel, Q630, viscosity of 6000cp), and adding 0.3 part by mass of inhibitor diallyl maleate; stirring the solution at normal temperature in dark for 25min, and vacuumizing to remove bubbles. And sealing and keeping away from light to obtain the final product.
Printing the prepared printing ink on a structural part by using a photocuring 3D printer (DLP molding), cleaning for 10min by using n-hexane after printing, and then curing for 8h in a 100 ℃ oven to obtain a sample.
Example 3
Taking 50 parts by mass of polysiloxane (viscosity is 2500 cst; vinyl content is 0.35mmol/g) containing vinyl at the end, adding 1.67 parts by mass of cross-linking agent (mercapto) methyl siloxane-dimethyl siloxane copolymer, adding 0.5 parts by mass of photoinitiator TPO-L, and mixing uniformly; weighing 50 parts by weight of Sylgard 184 silicon rubber (containing 0.5 part by weight of curing agent) and adding 0.2 part by weight of inhibitor diallyl maleate; stirring the solution at normal temperature in dark for 25min, and vacuumizing to remove bubbles. And sealing and keeping away from light to obtain the final product.
Printing the prepared printing ink on a structural part by using a photocuring 3D printer (DLP molding), cleaning for 10min by using n-hexane after printing, and then curing for 2h in a 150 ℃ oven to obtain a sample.
The test results of the product performance of the material printed by the photocuring 3D printing silicone rubber ink prepared in the examples 1-3 are shown in table 1, and fig. 1 is a stress-strain curve of the material printed by the photocuring 3D printing silicone rubber ink prepared in the examples 1-3. As can be seen from Table 1, the photocuring 3D printing silicone rubber ink prepared by the invention has good mechanical properties after photocuring forming.
Table 1 results of performance test of printed material products of photocuring 3D printing silicone rubber inks prepared in examples 1-3
| Sample (I) | Modulus of elasticity (MPa) | Tensile Strength (MPa) | Elongation at Break (%) |
| Example 1 | 0.19 | 0.51 | 275 |
| Example 2 | 0.3 | 0.55 | 214 |
| Example 3 | 0.22 | 0.56 | 245 |
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications can be made, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (10)
1. The photocuring 3D printing silicone rubber ink is characterized by comprising the following components in parts by mass:
30-50 parts of polysiloxane, wherein the end part of the polysiloxane contains vinyl;
1.25-10 parts of a siloxane crosslinking agent, wherein the siloxane crosslinking agent contains 2-3 sulfydryl groups;
0.5-2 parts of a photoinitiator;
40-60 parts of addition type thermosetting silicone rubber;
0.1-2 parts of an inhibitor.
2. The photocuring 3D printing silicone rubber ink as claimed in claim 1, which is characterized by comprising the following components in parts by mass:
30-50 parts of polysiloxane, 2-5 parts of siloxane cross-linking agent, 0.5-1.2 parts of photoinitiator, 40-60 parts of addition type thermosetting silicone rubber and 0.5-1 part of inhibitor.
3. The photocuring 3D printing silicone rubber ink as claimed in claim 1, which is characterized by comprising the following components in parts by mass:
50 parts of polysiloxane, 3 parts of siloxane cross-linking agent, 1.5 parts of photoinitiator, 45 parts of addition type thermosetting silicone rubber and 0.5 part of inhibitor.
4. The photo-curing 3D printing silicone rubber ink according to any one of claims 1 to 3, wherein the viscosity of the addition type thermosetting silicone rubber is 1000 to 6000 cps.
5. The light-curable 3D printing silicone rubber ink according to claim 4, wherein the addition type heat-curable silicone rubber comprises ceramic Sylgard-184 silicone rubber.
6. The photocuring 3D printing silicone rubber ink according to any one of claims 1 to 3, wherein the polysiloxane has a viscosity of 500 to 10000cst and a vinyl content of 0.1 to 0.8 mmol/g.
7. The photocurable 3D printing silicone rubber ink according to any one of claims 1 to 3, wherein the silicone crosslinker comprises one or more of (mercapto) methylsiloxane-dimethylsiloxane copolymer, trimethylolpropane tris (2-mercaptoacetate), 2-mercapto-N-methylbenzamide, mercaptopolyethyleneglycol maleimide, mercaptopolyethyleneglycol acrylamide, hydroxypolyethyleneglycol mercapto, methyl 2-mercaptobenzoate, and trimethylolpropane tris (3-mercaptopropionate).
8. The photocurable 3D printing silicone rubber ink according to any one of claims 1-3, wherein the photoinitiator is a radical photoinitiator comprising one or more of TOP-L, IRGACURE 819, IRGACURE 184 and IRGACURE 1173.
9. The photocurable 3D printing silicone rubber ink according to any one of claims 1 to 3, wherein the inhibitor is a thermosetting additive inhibitor comprising one or more of 2-methyl-3-yn-2-ol, 3-methyl-1-yn-3-ol, phenylacetylene, t-butyl peroxide, dimethyl sulfoxide, diphenyl sulfoxide, ethynyl cyclohexanol, diallyl maleate, diethyl fumarate and vinyl ring bodies.
10. The preparation method of the photocuring 3D printing silicone rubber ink as claimed in claim 1 to 9, characterized by comprising the following steps:
and mixing polysiloxane, a siloxane cross-linking agent, a photoinitiator, addition type thermosetting silicone rubber and an inhibitor to obtain the photocuring 3D printing silicone rubber ink.
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| CN202111262836.5A CN113817324A (en) | 2021-10-28 | 2021-10-28 | Photocuring 3D printing silicone rubber ink and preparation method thereof |
| CN202211100819.6A CN115637048A (en) | 2021-10-28 | 2022-09-09 | Photocuring 3D printing silicone rubber ink and preparation method thereof |
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- 2021-10-28 CN CN202111262836.5A patent/CN113817324A/en active Pending
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- 2022-09-09 CN CN202211100819.6A patent/CN115637048A/en active Pending
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Application publication date: 20211221 |