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CN119592073A - Organic silicon flexible material and preparation method thereof - Google Patents

Organic silicon flexible material and preparation method thereof Download PDF

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Publication number
CN119592073A
CN119592073A CN202411951829.XA CN202411951829A CN119592073A CN 119592073 A CN119592073 A CN 119592073A CN 202411951829 A CN202411951829 A CN 202411951829A CN 119592073 A CN119592073 A CN 119592073A
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parts
solution
organic silicon
flexible material
pdms
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张栩畅
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Jiangmen Jin Xin Heng Technology Co ltd
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Jiangmen Jin Xin Heng Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions 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
    • C08L83/04Polysiloxanes
    • C08L83/06Polysiloxanes containing silicon bound to oxygen-containing groups
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F299/00Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers
    • C08F299/02Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers from unsaturated polycondensates
    • C08F299/08Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers from unsaturated polycondensates from polysiloxanes

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Silicon Polymers (AREA)

Abstract

The invention belongs to the field of flexible materials, and particularly relates to an organic silicon flexible material and a preparation method thereof, wherein the organic silicon flexible material comprises, by weight, 60-80 parts of acrylic acid modified siloxane, 10-30 parts of plant fibers, 2-6 parts of silane coupling agent, 2-5 parts of photoinitiator and 0.5-4 parts of PEG 400, the crosslinking density and mechanical property of the modified siloxane are obviously improved after the siloxane is modified by acrylic acid, and the functional groups of an acrylic group and a silane modified layer on the surface of the plant fibers are connected through a photo-curing reaction, so that efficient interface combination is realized, the integral strength and toughness of the organic silicon material are further improved, in addition, the photo-curing effect can realize the optical transparency of the material, the environmental pollution caused by a traditional curing agent is avoided, and the organic silicon flexible material is expected to provide strong functional material support for complex intelligent applications such as electronic skin, biosensors and soft robots.

Description

Organic silicon flexible material and preparation method thereof
Technical Field
The invention belongs to the field of flexible materials, and particularly relates to an organic silicon flexible material and a preparation method thereof.
Background
The organic silicon material has excellent flexibility, chemical stability and biocompatibility due to the unique chemical structure and silicon-oxygen bond advantages. It has great potential in the fields of flexible electronics, wearable devices, biomedical implants, aerospace, and the like. However, conventional silicone materials have low mechanical strength and toughness, are prone to fracture under tensile and flexural conditions, and are difficult to meet high strength requirements in dynamic applications. By introducing the reinforcing filler, although mechanical properties can be improved, it tends to result in reduced flexibility and light transmittance, while the filler is less uniformly dispersed and stress concentration points are easily formed. Meanwhile, the existing siloxane material curing is dependent on chemical curing agents. These chemicals not only present a risk of toxicity or environmental pollution, but may also create residues in the material that affect its biocompatibility. Along with the development of society, how to endow flexible materials with multi-functionality through structural and component design while guaranteeing the flexibility and dispersion uniformity of the flexible materials becomes a hot spot and a difficult point of research.
Therefore, it is important to develop a multifunctional and high-performance organic silicon flexible material to solve the problems of low mechanical property, single function and insufficient environmental stability of the existing material.
Disclosure of Invention
Aiming at the situation, the invention provides the organic silicon flexible material and the preparation method thereof, acrylic acid groups are introduced into PDMS (polydimethylsiloxane) molecular chains, and the cross-linking reaction of the acrylic acid groups is initiated under the catalysis of a photoinitiator, so that the curing is realized, the use of a traditional chemical curing agent is avoided, the plant fiber is modified through a silane coupling agent, the interface combination of the fiber and a siloxane matrix is enhanced, the flexibility, the strength and the sensibility of the material are endowed, and simultaneously, the distribution of the plant fiber in the matrix is optimized by utilizing a micronization technology and a dispersing agent, the uniformity of the performance of the composite material is ensured, and finally, the problems of insufficient mechanical property, environmental pollution, single function and the like of the traditional organic silicon material are solved, and a new solution is provided for the application of the organic silicon flexible material in the field of multifunctional electronic devices.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
The invention provides an organosilicon flexible material which comprises, by weight, 60-80 parts of acrylic modified siloxane, 10-30 parts of plant fibers, 2-6 parts of a silane coupling agent, 2-5 parts of a photoinitiator and 0.5-4 parts of PEG 400 (polyethylene glycol 400).
Further, the acrylic modified siloxane comprises 50-70 parts by weight of PDMS, 20-40 parts by weight of acrylic ester, 1 part by weight of Karstedt catalyst and 5 parts by weight of toluene.
Further, the plant fiber is selected from one or more of CNC (cellulose nanocrystalline), flax fiber, cotton fiber, coconut fiber and bamboo fiber.
Further, the silane coupling agent is selected from one or more of a151 (vinyltriethoxysilane), a171 (vinyltrimethoxysilane), isobutyltriethoxysilane and KH-550 (γ -aminopropyl triethoxysilane), preferably a151.
Further, the photoinitiator is selected from one or more of Irgacure 2959 (2-hydroxy-4' - (2-hydroxyethoxy) -2-methylpropaneketone), darocur 1173 (2-hydroxy-2-methylpropaneketone), and TPO-L (ethyl 2,4, 6-trimethylbenzoyl phosphonate).
Further, the PDMS is hydroxyl terminated.
Further, the acrylate is selected from one or more of MMA (methacrylate), PHEA (2-phenoxyethyl acrylate), PEGDA (polyethylene glycol diacrylate), HDDA (1, 6-hexanediol diacrylate) and GPTA (propoxylated glycerol triacrylate).
The preparation method of the acrylic modified siloxane comprises the following steps:
S1, weighing 50-70 parts of PDMS and 5 parts of toluene, adding the PDMS and the 5 parts of toluene into n-hexane, stirring the mixture in a magnetic stirrer for 20 min dissolution in a mass ratio of PDMS to n-hexane of 1:6 to obtain a PDMS solution;
S2, weighing 20-40 parts of acrylic ester, dissolving the acrylic ester in ethyl acetate according to a mass ratio of 1:3 to obtain an acrylic ester solution, adding the acrylic ester solution into the PDMS solution obtained in the step S1, and stirring and uniformly mixing the 100 rpm to obtain a mixed solution of 5 min;
S3, weighing 1 part of Karstedt catalyst, adding the Karstedt catalyst into the mixed solution obtained in the step S2 under the protection of nitrogen, and reacting at 150 rpm and 40-50 ℃ for 4h to obtain a reaction solution;
And S4, removing the organic solvent in the reaction liquid obtained in the step S3 by using a rotary evaporator, wherein the water bath temperature is set to be 30 ℃, and the cold trap temperature is set to be-20 ℃ to obtain the acrylic modified siloxane.
The invention also provides a preparation method of the organic silicon flexible material, which comprises the following steps:
weighing 10-30 parts of plant fibers, soaking the plant fibers in a 5% (w/v) NaOH solution according to a mass-volume ratio of 1g to 5 mL, treating the plant fibers at 80 ℃ for 2h, filtering to obtain soaked plant fibers, washing the soaked plant fibers with purified water until the pH is neutral, and drying the plant fibers at 60 ℃ for 4h to obtain pretreated plant fibers;
Step 2, weighing 2-6 parts of silane coupling agent, dissolving the silane coupling agent in 90% (v/v) ethanol water solution according to the mass-volume ratio of 1g to 20mL, and regulating the pH value to 4.0-5.0 by using 0.1 mol/L HCl solution to obtain a silane coupling agent solution;
Step 3, adding the pretreated plant fiber obtained in the step 1 into the silane coupling agent solution obtained in the step 2, carrying out ultrasonic treatment on the plant fiber by 200W for 30min, carrying out stirring reaction for 3 h under the magnetic stirring condition of 40 ℃ and 150rpm, and carrying out vacuum drying at 60 ℃ for 12h to obtain a modified plant fiber;
Step 4, weighing 60-80 parts of acrylic modified siloxane, heating to 50 ℃, adding 2-5 parts of photoinitiator and 0.5-4 parts of PEG 400 in a dark place, uniformly stirring, adding the modified plant fiber obtained in the step 3 to obtain a mixture, and putting the mixture into a high-shear homogenizer for dispersion treatment at 10 min, rotating speed 10000 rpm and power 3.5 kW to obtain a homogeneous solution;
And 5, placing the homogeneous liquid obtained in the step 4 in a vacuum drying oven for removing bubbles at 30 min, pouring the homogeneous liquid into a mould, and irradiating and curing the homogeneous liquid with ultraviolet light at 3 min to obtain the organic silicon flexible material.
The beneficial effects obtained by the invention are as follows:
The organic silicon flexible material prepared by the invention takes the acrylic acid modified siloxane as a flexible matrix, overcomes the defects of the traditional flexible material in terms of mechanical strength, environmental protection and functional diversity by introducing plant fibers and a photo-curing technology, realizes high-efficiency interface bonding of the plant fibers and the organic silicon matrix through a silane coupling agent, enhances the crosslinking density of the siloxane, obviously improves the mechanical property and the surface energy of the siloxane by introducing the acrylic acid groups, ensures the matrix to have better interface bonding capability and toughness, adopts a photoinitiator to enable the acrylic acid groups on the modified siloxane to be quickly crosslinked, avoids the environmental pollution and residue problems caused by the traditional curing agent and the influence of the filler on the integral performance of the silicon material, and can also realize the optical transparency of the material, ensure the photosensitive responsiveness of the material in the electronic skin and the flexible sensor by the photo-curing technology, and further improve the integral strength and the adhesive property of the material by the crosslinking reaction of the acrylic acid groups and the functional groups of the silane modified layer on the surface of the plant fibers, obviously improves the tensile strength and the tensile strength of the plant fibers after being subjected to the modification treatment of the micro-and the silane coupling agent, and ensures the stress-resistant stress-concentrating resistance of the material to be uniform and the stress-resistant-dispersing agent 400 when the material is used as a dispersing agent is added, and the dispersing agent is formed, so that the network-distributed has the stress-resistant performance-enhancing performance is ensured.
The organic silicon flexible material prepared by the invention realizes high integration of mechanical, optical and electrical properties through structural design, and provides powerful functional material support for complex intelligent application scenes such as electronic skin, biological sensors, soft robots and the like.
Drawings
FIG. 1 is a flow chart of the preparation of a silicone flexible material of the present invention;
FIG. 2 shows the FTIR (Fourier IR) results of the acrylic-modified silicone prepared in example 1;
FIG. 3 shows the results of mechanical property detection of the silicone flexible materials prepared in examples 1-5;
FIG. 4 shows the results of thermogravimetric analysis of the silicone flexible materials prepared in examples 1-5.
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by those skilled in the art without making any inventive effort based on the embodiments of the present invention are within the scope of protection of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the present application. The preferred methods and materials described herein are illustrative only and should not be construed as limiting the application.
In the following examples, the preparation process of the organosilicon flexible material refers to fig. 1, and the organosilicon flexible material is a conventional method unless otherwise specified, and the materials used in the following examples are new materials purchased in the market unless otherwise specified.
Example 1 this example provides a silicone flexible material comprising, by weight, 70 parts of an acrylic modified silicone, 20 parts of CNC, 2 parts of A151, 2959 parts of Irgacure and 400 parts of PEG.
The acrylic modified siloxane comprises the following raw materials in parts by weight, namely 50 parts of PDMS, 40 parts of MMA, 1 part of Karstedt's catalyst and 5 parts of toluene, wherein the specific preparation method comprises the following steps:
S1, weighing 50 parts of PDMS and 5 parts of toluene, adding the PDMS and the 5 parts of toluene into n-hexane, and stirring the mixture 20min in a magnetic stirrer at a mass ratio of PDMS to n-hexane of 1:6 to obtain a PDMS solution;
S2, weighing 40 parts of MMA, dissolving in ethyl acetate according to a mass ratio of 1:3 to obtain an MMA solution, adding the MMA solution into the PDMS solution obtained in the step S1, and stirring and uniformly mixing the MMA solution with 100 rpm for 5min to obtain a mixed solution;
S3, weighing 1 part of Karstedt catalyst, adding the Karstedt catalyst into the mixed solution obtained in the step S2 under the protection of nitrogen, and reacting at 150 rpm and 40 ℃ for 4 h to obtain a reaction solution;
And S4, removing the organic solvent in the reaction liquid obtained in the step S3 by using a rotary evaporator, wherein the water bath temperature is set to be 30 ℃, and the cold trap temperature is set to be-20 ℃ to obtain the acrylic modified siloxane.
The embodiment also provides a preparation method of the organic silicon flexible material, which specifically comprises the following steps:
Weighing 20 parts of CNC, soaking in a 5% NaOH solution according to a mass-volume ratio of 1g to 5 mL, filtering after 80 ℃ treatment of 2h to obtain soaked CNC, washing purified water until the pH is neutral, and drying at 60 ℃ for 4: 4h to obtain pretreated CNC;
2, weighing 2 parts of A151, dissolving in a 90% ethanol water solution according to a mass-volume ratio of 1g to 20 mL, and regulating the pH value to 4.5 by using 0.1 mol/L HCl solution to obtain an A151 solution;
Step 3, adding the pretreated CNC obtained in the step 1 into the solution A151 obtained in the step 2, performing ultrasonic treatment on the solution A by 200W for 30min, performing stirring reaction for 3h under the magnetic stirring condition of 40 ℃ and 150 rpm, and performing vacuum drying at 60 ℃ for 12h to obtain modified CNC;
Step 4, weighing 70 parts of acrylic modified siloxane, heating to 50 ℃, weighing 5 parts of Irgacure 2959 and 3 parts of PEG 400 in a dark place, adding the mixture into the mixture, stirring uniformly, adding the modified CNC obtained in the step 3 to obtain a mixture, and putting the mixture into a high-shear homogenizer for dispersion treatment for 10 min, wherein the rotating speed is 10000 rpm, and the power is 3.5 kW to obtain a homogeneous solution;
and 5, placing the homogenized liquid obtained in the step 4 in a vacuum drying oven for removing bubbles at 30min, pouring the homogenized liquid into a die, and irradiating with ultraviolet light with the wavelength of 365-nm to cure 3-min to obtain the organosilicon flexible material.
Example 2 this example provides a silicone flexible material comprising, by weight, 80 parts of an acrylic modified silicone, 10 parts of CNC, 151A 4 parts, 2959 Irgacure and 400 PEG.
The acrylic modified siloxane comprises the following raw materials by weight parts of 70 parts of PDMS, 20 parts of MMA, 1 part of Karstedt catalyst and 5 parts of toluene, wherein the specific preparation steps refer to the preparation method of the acrylic modified siloxane in the example 1.
The embodiment also provides a preparation method of the organic silicon flexible material, and specific preparation steps refer to the preparation method of the organic silicon flexible material in embodiment 1.
Example 3 this example provides a silicone flexible material comprising, by weight, 60 parts of an acrylic modified silicone, 30 parts of CNC, 6 parts of A151, 2959 parts of Irgacure and 0.5 part of PEG 400.
The acrylic modified siloxane comprises the following raw materials by weight parts of 60 parts of PDMS, 30 parts of MMA, 1 part of Karstedt catalyst and 5 parts of toluene, wherein the specific preparation steps refer to the preparation method of the acrylic modified siloxane in the example 1.
The embodiment also provides a preparation method of the organic silicon flexible material, and specific preparation steps refer to the preparation method of the organic silicon flexible material in embodiment 1.
Example 4 this example provides a silicone flexible material comprising, by weight, 70 parts of an acrylic modified silicone, 20 parts of cotton fibers, 2 parts of a151, 1173 parts of Darocur, and 400 parts of PEG.
The acrylic modified siloxane comprises the following raw materials in parts by weight: 50 parts of PDMS, 40 parts of PEGDA, 1 part of Karstedt catalyst and 5 parts of toluene, and the specific preparation method is as follows:
S1, weighing 50 parts of PDMS and 5 parts of toluene, adding the PDMS and the 5 parts of toluene into n-hexane, and stirring the mixture 20min in a magnetic stirrer at a mass ratio of PDMS to n-hexane of 1:6 to obtain a PDMS solution;
S2, weighing 40 parts of PEGDA, dissolving in ethyl acetate according to a mass ratio of 1:3 to obtain a PEGDA solution, adding the PEGDA solution into the PDMS solution obtained in the step S1, and stirring and uniformly mixing the 100: rpm to obtain a mixed solution;
S3, weighing 1 part of Karstedt catalyst, adding the Karstedt catalyst into the mixed solution obtained in the step S2 under the protection of nitrogen, and reacting at 150 rpm and 50 ℃ for 4 h to obtain a reaction solution;
And S4, removing the organic solvent in the reaction liquid obtained in the step S3 by using a rotary evaporator, wherein the water bath temperature is set to be 30 ℃, and the cold trap temperature is set to be-20 ℃ to obtain the acrylic modified siloxane.
The embodiment also provides a preparation method of the organic silicon flexible material, which specifically comprises the following steps:
Step 1, weighing 20 parts of cotton fibers, soaking the cotton fibers in a 5% NaOH solution according to a mass-volume ratio of 1g to 5 mL, filtering the soaked cotton fibers after treatment at 80 ℃ for 2h, washing the cotton fibers with purified water until the pH is neutral, and drying the cotton fibers at 60 ℃ for 4h to obtain pretreated cotton fibers;
2, weighing 2 parts of A151, dissolving in a 90% ethanol water solution according to a mass-volume ratio of 1g to 20 mL, and regulating the pH value to 4.2 by using 0.1 mol/L HCl solution to obtain an A151 solution;
Step 3, adding the pretreated cotton fiber obtained in the step 1 into the solution A151 obtained in the step 2, carrying out ultrasonic treatment on the pretreated cotton fiber by 200W for 30 min, carrying out stirring reaction for 3h under the magnetic stirring condition of 40 ℃ and 150 rpm, and carrying out vacuum drying at 60 ℃ for 12h to obtain a modified cotton fiber;
step 4, weighing 70 parts of acrylic modified siloxane, heating to 50 ℃, weighing 5 parts of Darocur 1173 and 3 parts of PEG 400 in a dark place, adding the mixture into the mixture, stirring uniformly, adding the modified cotton fiber obtained in the step 3 to obtain a mixture, and putting the mixture into a high-shear homogenizer for dispersion treatment at 10min, rotating speed 10000 rpm and power of 3.5 kW to obtain a homogeneous solution;
And 5, placing the homogenized liquid obtained in the step 4 in a vacuum drying oven for removing bubbles at 30 min, pouring the homogenized liquid into a die, and irradiating with ultraviolet light with the wavelength of 322 to nm to cure 3 to min to obtain the organosilicon flexible material.
Example 5 this example provides a silicone flexible material comprising, by weight, 70 parts of an acrylic modified silicone, 20 parts of coconut fiber, 2 parts of A151, 5 parts of TPO-L, and 400 parts of PEG.
The acrylic modified siloxane comprises the following raw materials in parts by weight: 50 parts of PDMS, 40 parts of GPTA, 1 part of Karstedt catalyst and 5 parts of toluene, and the specific preparation method is as follows:
S1, weighing 50 parts of PDMS and 5 parts of toluene, adding the PDMS and the 5 parts of toluene into n-hexane, and stirring the mixture 20min in a magnetic stirrer at a mass ratio of PDMS to n-hexane of 1:6 to obtain a PDMS solution;
s2, weighing 40 parts of GPTA, dissolving in ethyl acetate according to a mass ratio of 1:3 to obtain a GPTA solution, adding the GPTA solution into the PDMS solution obtained in the step S1, and stirring and uniformly mixing the mixture with 100: rpm to obtain a mixed solution;
S3, weighing 1 part of Karstedt catalyst, adding the Karstedt catalyst into the mixed solution obtained in the step S2 under the protection of nitrogen, and reacting at 150 rpm and 45 ℃ for 4 h to obtain a reaction solution;
And S4, removing the organic solvent in the reaction liquid obtained in the step S3 by using a rotary evaporator, wherein the water bath temperature is set to be 30 ℃, and the cold trap temperature is set to be-20 ℃ to obtain the acrylic modified siloxane.
The embodiment also provides a preparation method of the organic silicon flexible material, which specifically comprises the following steps:
Step 1, weighing 20 parts of coconut fibers, soaking the coconut fibers in a 5% NaOH solution according to a mass-volume ratio of 1g to 5 mL, filtering the soaked coconut fibers after treatment at 80 ℃ for 2h, washing the coconut fibers with purified water until the pH is neutral, and drying the coconut fibers at 60 ℃ for 4h to obtain pretreated coconut fibers;
2, weighing 2 parts of A151, dissolving in a 90% ethanol water solution according to a mass-volume ratio of 1g to 20 mL, and regulating the pH value to 5.0 by using 0.1 mol/L HCl solution to obtain an A151 solution;
Step 3, adding the pretreated coconut fiber obtained in the step 1 into the A151 solution obtained in the step 2, carrying out ultrasonic treatment on the pretreated coconut fiber by 200W for 30min, carrying out stirring reaction for 3 h under the magnetic stirring condition of 40 ℃ and 150 rpm, and carrying out vacuum drying at 60 ℃ for 12h to obtain modified coconut fiber;
Step 4, weighing 70 parts of acrylic modified siloxane, heating to 50 ℃, weighing 5 parts of TPO-L and 3 parts of PEG 400 in a dark place, adding the mixture into the mixture, stirring uniformly, adding the modified coconut fiber obtained in the step 3 to obtain a mixture, and putting the mixture into a high-shear homogenizer for dispersion treatment at 10min, rotating speed 10000 rpm and power of 3.5 kW to obtain a homogeneous solution;
And 5, placing the homogenized liquid obtained in the step 4 in a vacuum drying oven for removing bubbles at 30 min, pouring the homogenized liquid into a die, and irradiating with ultraviolet light with wavelength of 273 nm to cure 3 min to obtain the organosilicon flexible material.
FTIR investigation
The acrylic modified siloxane prepared in example 1 was taken and placed in an oven and dried to constant weight, and the acrylic binding condition was examined on FTIR using KBr tabletting to prepare a mixture of MMS and PDMS of the same amount as the acrylic modified siloxane as a control, and the result is shown in fig. 2.
Mechanical property test
The silicone flexible materials prepared in examples 1 to 5 were tested with reference to the fiber reinforced plastic tensile property test method GB/T1447-2005, and the results are shown in FIG. 3.
Thermal stability investigation
The organic silicon flexible materials prepared in examples 1-5 were tested by referring to the thermal flow meter standard GB/T10295-2008 for measuring the steady-state thermal resistance and related characteristics of the heat insulation materials, and the thermal weight loss analysis results are shown in FIG. 4.
The FTIR results of fig. 2 show that in the MMA and PDMS mixture, the organosilicon Si-O-Si bond absorption peaks at both 1033 and 1131 cm -1 are present, while the characteristic peaks of the acrylic modified siloxane, si-C and C-H organic functional groups, etc. typically disappeared, and an amorphous SiO 2 absorption peak appears at 1089 cm -1, indicating that the PDMS modification was successful.
The mechanical property results of the organosilicon flexible materials prepared in examples 1-5 in fig. 3 show that the elongation at break of the organosilicon flexible materials prepared in examples 1-4 is greater than 150%, and the tensile stress is strong, because the whole mechanical property of the materials is greatly improved after the added flexible long-chain plant fibers are crosslinked with the modified siloxane.
The results of thermal weight loss analysis in fig. 4 show that the silicone flexible materials prepared in examples 1-5 all have a slow downward trend, and when the temperature continues to rise, the weight drops sharply until stable, the silicone flexible material prepared in example 1 has less volatilization loss along with high temperature, the final weight is still at a higher level, and the thermal stability is good.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
The invention and its embodiments have been described above with no limitation, and the invention is illustrated in the figures of the accompanying drawings as one of its embodiments, without limitation in practice. In summary, those skilled in the art, having benefit of this disclosure, will appreciate that the invention can be practiced without the specific details disclosed herein.

Claims (8)

1. 一种有机硅柔性材料,其特征在于,所述有机硅柔性材料包括以下重量份原料:丙烯酸改性硅氧烷60-80份、植物纤维10-30份、硅烷偶联剂2-6份、光引发剂2-5份和PEG 4000.5-4份;1. A flexible organosilicon material, characterized in that the flexible organosilicon material comprises the following raw materials in parts by weight: 60-80 parts of acrylic modified siloxane, 10-30 parts of plant fiber, 2-6 parts of silane coupling agent, 2-5 parts of photoinitiator and 0.5-4 parts of PEG 4000; 所述丙烯酸改性硅氧烷包括以下原料:PDMS、丙烯酸酯、Karstedt催化剂和甲苯,具体制备方法如下:The acrylic modified siloxane comprises the following raw materials: PDMS, acrylate, Karstedt catalyst and toluene, and the specific preparation method is as follows: S1:称取PDMS和甲苯加入到正己烷中,搅拌、溶解,得到PDMS溶液;S1: Weigh PDMS and toluene, add them into n-hexane, stir and dissolve to obtain a PDMS solution; S2:称取丙烯酸酯溶解于乙酸乙酯,得到丙烯酸酯溶液,将丙烯酸酯溶液加入到步骤S1得到的PDMS溶液中,搅拌,得到混合液;S2: Weigh acrylate and dissolve it in ethyl acetate to obtain an acrylate solution, add the acrylate solution to the PDMS solution obtained in step S1, stir, and obtain a mixed solution; S3:称取Karstedt催化剂加入到步骤S2得到的混合液中,搅拌、加热,得到反应液;S3: weighing a Karstedt catalyst and adding it to the mixed solution obtained in step S2, stirring and heating to obtain a reaction solution; S4:去除步骤S3得到的反应液中的有机溶剂,得到丙烯酸改性硅氧烷。S4: removing the organic solvent in the reaction solution obtained in step S3 to obtain acrylic modified siloxane. 2.根据权利要求1所述的一种有机硅柔性材料,其特征在于,步骤S1-S4中,所述PDMS、丙烯酸酯、Karstedt催化剂和甲苯分别为重量份50-70份、20-40份、1份和5份;2. The organic silicon flexible material according to claim 1, characterized in that in steps S1-S4, the PDMS, acrylate, Karstedt catalyst and toluene are 50-70 parts by weight, 20-40 parts by weight, 1 part and 5 parts by weight respectively; 步骤S1中,所述PDMS和正己烷质量比例为1:6;In step S1, the mass ratio of PDMS to n-hexane is 1:6; 步骤S2中,所述丙烯酸酯和乙酸乙酯质量比例为1:3;In step S2, the mass ratio of the acrylic acid ester to the ethyl acetate is 1:3; 步骤S3中,所述搅拌、加热过程在氮气保护下进行。In step S3, the stirring and heating process is carried out under nitrogen protection. 3.根据权利要求1所述的一种有机硅柔性材料,其特征在于,所述植物纤维选自CNC、亚麻纤维、棉纤维、椰壳纤维和竹原纤维中的一种或多种。3. The organic silicon flexible material according to claim 1, characterized in that the plant fiber is selected from one or more of CNC, flax fiber, cotton fiber, coconut shell fiber and bamboo fiber. 4.根据权利要求1所述的一种有机硅柔性材料,其特征在于,所述硅烷偶联剂选自A151、A171、异丁基三乙氧基硅烷和KH-550中的一种或多种。4. The organic silicon flexible material according to claim 1, characterized in that the silane coupling agent is selected from one or more of A151, A171, isobutyltriethoxysilane and KH-550. 5. 根据权利要求1所述的一种有机硅柔性材料,其特征在于,所述光引发剂选自Irgacure 2959、Darocur 1173和TPO-L中的一种或多种。5. The organic silicone flexible material according to claim 1, characterized in that the photoinitiator is selected from one or more of Irgacure 2959, Darocur 1173 and TPO-L. 6.根据权利要求1所述的一种有机硅柔性材料,其特征在于,所述丙烯酸酯选自MMA、PHEA、PEGDA、HDDA和GPTA中的一种或多种。6 . The organic silicon flexible material according to claim 1 , wherein the acrylate is selected from one or more of MMA, PHEA, PEGDA, HDDA and GPTA. 7.一种根据权利要求1-6任一项所述的一种有机硅柔性材料的制备方法,其特征在于,具体制备方法如下:7. A method for preparing a flexible silicone material according to any one of claims 1 to 6, characterized in that the specific preparation method is as follows: 步骤1:称取植物纤维,浸泡于5%NaOH溶液中,加热、过滤得到浸泡过的植物纤维,冲洗、烘干得到预处理植物纤维;Step 1: Weigh the plant fiber, soak it in a 5% NaOH solution, heat and filter to obtain the soaked plant fiber, and rinse and dry to obtain the pretreated plant fiber; 步骤2:称取硅烷偶联剂溶解于90%乙醇水溶液,调pH,得到硅烷偶联剂溶液;Step 2: Weigh a silane coupling agent and dissolve it in a 90% ethanol aqueous solution, and adjust the pH to obtain a silane coupling agent solution; 步骤3:向步骤2得到的硅烷偶联剂溶液中加入步骤1得到的预处理植物纤维,超声、加热、搅拌、干燥后,得到改性植物纤维;Step 3: adding the pretreated plant fiber obtained in step 1 to the silane coupling agent solution obtained in step 2, and obtaining modified plant fiber after ultrasonication, heating, stirring and drying; 步骤4:称取丙烯酸改性硅氧烷并加热,称取光引发剂和PEG 400加入其中搅拌,再加入步骤3得到的改性植物纤维,得到混合物,均质分散,得到均质液;Step 4: Weigh acrylic modified siloxane and heat it, weigh a photoinitiator and PEG 400, add them thereto and stir, then add the modified plant fiber obtained in step 3 to obtain a mixture, and homogenize and disperse it to obtain a homogenous liquid; 步骤5:将步骤4得到的均质液除气泡,紫外光固化,得到有机硅柔性材料。Step 5: Remove bubbles from the homogenized liquid obtained in step 4, and cure it with ultraviolet light to obtain a flexible silicone material. 8. 根据权利要求7所述的一种有机硅柔性材料的制备方法,其特征在于,步骤1中,所述植物纤维和5%NaOH溶液质量体积比为1 g:5 mL;8. The method for preparing a flexible organosilicon material according to claim 7, characterized in that in step 1, the mass volume ratio of the plant fiber to the 5% NaOH solution is 1 g:5 mL; 步骤2中,所述硅烷偶联剂和90%乙醇水溶液质量体积比为1 g:20 mL;In step 2, the mass volume ratio of the silane coupling agent to the 90% ethanol aqueous solution is 1 g: 20 mL; 步骤4中,所述操作避光进行,所述均质分散过程使用高剪切均质机。In step 4, the operation is performed in the dark, and a high shear homogenizer is used in the homogenization and dispersion process.
CN202411951829.XA 2024-12-27 2024-12-27 Organic silicon flexible material and preparation method thereof Pending CN119592073A (en)

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CN111108148A (en) * 2017-07-31 2020-05-05 美国陶氏有机硅公司 Processing additives for silicone elastomer binders
CN109054061A (en) * 2018-07-12 2018-12-21 南京林业大学 A kind of dimethyl silicone polymer/nano cellulose composite film and preparation method thereof
CN116253998A (en) * 2022-12-23 2023-06-13 中国医学科学院整形外科医院 Cost cartilage mold, preparation method and application thereof
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Application publication date: 20250311