CN110776719A - Method for dispersing nano inorganic particle filler in solid epoxy resin - Google Patents
Method for dispersing nano inorganic particle filler in solid epoxy resin Download PDFInfo
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- CN110776719A CN110776719A CN201910994827.1A CN201910994827A CN110776719A CN 110776719 A CN110776719 A CN 110776719A CN 201910994827 A CN201910994827 A CN 201910994827A CN 110776719 A CN110776719 A CN 110776719A
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- epoxy resin
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- particle filler
- inorganic particle
- solid epoxy
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
- C08J3/2053—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the additives only being premixed with a liquid phase
- C08J3/2056—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the additives only being premixed with a liquid phase the polymer being pre-melted
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
- C08J2363/02—Polyglycidyl ethers of bis-phenols
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention provides a method for dispersing nano inorganic particle filler in solid epoxy resin, which comprises the steps of adding the nano inorganic particle filler and liquid epoxy resin into a ball mill, blending and dispersing to obtain a uniformly dispersed low-viscosity mixed solution; and adding the low-viscosity mixed solution into the molten liquid of the solid epoxy resin, and stirring to obtain a uniformly dispersed molten mixed solution. By the dispersion method, the nano inorganic particle filler is fully and uniformly dispersed in the solid epoxy resin, the defect of stress concentration in the cured nano inorganic particle/epoxy resin composite material is overcome, and the mechanical and electrical properties of the epoxy composite material are improved.
Description
Technical Field
The invention relates to the technical field of efficient dispersion of nano inorganic particles in high-viscosity molecular materials, in particular to a method for dispersing a nano inorganic particle filler in solid epoxy resin.
Background
The epoxy resin has excellent performances of bonding, wear resistance, electrical insulation, chemical stability, high and low temperature resistance and the like, and is widely applied to the fields of adhesives, electronic instruments, aerospace, coatings, electronic and electrical insulation materials, advanced composite materials and the like. However, the pure epoxy resin has a high crosslinking structure after being cured, so that the pure epoxy resin has the defects of brittle quality, poor fatigue resistance, poor impact toughness and the like. Therefore, the toughness, modulus, heat resistance and the like of the epoxy resin can be improved by adding the inorganic nano filler. However, since the nanoparticles have high surface energy and are easy to agglomerate, the performance of the composite material is determined by the dispersibility of the inorganic filler in the polymer matrix and the interface action between the inorganic filler and the organic matrix.
Because the nano particles are easy to agglomerate, the epoxy resin has high viscosity, so that the nano particles are difficult to uniformly disperse in the epoxy resin. At present, the problem of dispersing nano inorganic particles in solid epoxy resin is mainly that a stirrer is used for high-speed stirring for dispersing, but the dispersing method cannot fully disperse the nano inorganic particles in the solid epoxy resin, so that the nano inorganic particles have the problem of agglomeration in the solid epoxy resin, the internal stress concentration defect of the cured nano inorganic particle/epoxy resin composite material is caused, and the mechanical and electrical properties of the epoxy composite material are reduced.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a method for dispersing a nano inorganic particle filler in a solid epoxy resin.
The technical scheme adopted by the invention is as follows:
a method for dispersing nanometer inorganic particle filler in solid epoxy resin comprises the following steps:
(1) adding the inorganic nano-particle filler and the liquid epoxy resin into a ball mill, blending and dispersing to obtain a uniformly dispersed low-viscosity mixed solution;
(2) and adding the low-viscosity mixed solution into the molten liquid of the solid epoxy resin, and stirring to obtain a uniformly dispersed molten mixed solution.
Further, the blending and dispersing time in the step (1) is 1-2 h; the grain diameter of the nano inorganic particle filler is 25-35 nm.
In the further scheme, the adding mass percent of the nano inorganic particle filler in the step (1) is 2-3%.
In a further scheme, the mass ratio of the solid epoxy resin to the liquid epoxy resin is 8-10: 1.
In a further scheme, the nano inorganic particle filler is nano aluminum oxide, nano SiO2 or nano ZnO.
Further, the stirring in the step (2) means stirring for at least 1h under the conditions of the temperature of 130-.
Liquid epoxy resin means epoxy resin which is liquid at normal temperature, such as E51, E44; wherein the E44 epoxy resin represents an epoxy resin having an average epoxy value of 44/100, (0.41-0.47), and E51 represents an epoxy resin having an average epoxy value (51/100=0.51, epoxy value N/100 is 0.48-0.54). The melt of the solid epoxy resin is a melt obtained by melting a solid at normal temperature and at high temperature, and specifically includes CT5531 (hensman brand in usa) and E20 (bisphenol a epoxy resin, epoxy equivalent/100 g is 0.18 to 0.23). Namely, each of the above products is a commercially available product.
The nano inorganic particle filler and the liquid epoxy resin are blended and dispersed to obtain a uniformly dispersed low-viscosity mixed solution, and then the mixed solution is added into the molten liquid of the solid epoxy resin and stirred to obtain a molten mixed solution. Therefore, the method fully and uniformly disperses the nano inorganic particle filler in the solid epoxy resin, overcomes the defect of stress concentration in the cured nano inorganic particle/epoxy resin composite material, and improves the mechanical and electrical properties of the epoxy composite material.
Compared with the prior art, the invention has the beneficial effects of realizing the high-efficiency dispersion of the nano inorganic particle filler in the solid epoxy resin and improving the mechanical strength and the performance stability of the nano inorganic particle filler and the solid epoxy resin composite material.
Detailed Description
Example 1:
a method for dispersing nanometer inorganic particle filler in solid epoxy resin comprises the following steps:
(1) adding nano alumina with the particle size of 25nm and E51 into a ball mill, blending and dispersing for 1h to obtain a uniformly dispersed low-viscosity mixed solution, wherein the mass percent of the nano alumina is 2%;
(2) and adding the low-viscosity mixed solution into the molten liquid of the CT5531, wherein the mass ratio of the solid epoxy resin to the liquid epoxy resin is 8:1, and stirring for 1h at the temperature of 130 ℃ and the stirring speed of 1000 revolutions per minute to obtain a uniformly dispersed molten mixed solution.
Example 2:
a method for dispersing nanometer inorganic particle filler in solid epoxy resin comprises the following steps:
(1) adding nano SiO2 with the particle size of 35nm and liquid epoxy resin E44 into a ball mill, and carrying out blending and dispersion for 2 hours to obtain a uniformly dispersed low-viscosity mixed solution, wherein the mass percent of the nano SiO2 is 3%;
(2) and adding the low-viscosity mixed solution into the molten liquid of the solid epoxy resin E20, wherein the mass ratio of the solid epoxy resin to the liquid epoxy resin is 10:1, and stirring for 2 hours at the temperature of 150 ℃ and the stirring speed of 1100 r/min to obtain a uniformly dispersed molten mixed solution.
Example 3:
a method for dispersing nanometer inorganic particle filler in solid epoxy resin comprises the following steps:
(1) adding nano ZnO with the particle size of 30nm and liquid epoxy resin E51 into a ball mill, blending and dispersing for 1.5h to obtain a uniformly dispersed low-viscosity mixed solution, wherein the mass percent of the nano ZnO is 2.5%;
(2) and adding the low-viscosity mixed solution into the molten liquid of the solid epoxy resin CT5531, wherein the mass ratio of the solid epoxy resin to the liquid epoxy resin is 9:1, and stirring for 3 hours at the temperature of 140 ℃ and the stirring speed of 1000 revolutions per minute to obtain uniformly dispersed molten mixed solution.
Comparative example:
adding nano ZnO with the particle size of 30nm and solid epoxy resin CT5531 into a ball mill, blending and dispersing for 1.5h to obtain uniformly dispersed mixed powder, wherein the mass percent of the nano ZnO is 2.5%.
The composite materials prepared in the example 3 and the comparative example are respectively dried and then the performances of the composite materials are detected, and the comparison shows that the impact strength, the tensile strength and the breakdown field strength of the composite material prepared in the example 3 are improved by 5.2%, 3.4% and 4.2% respectively compared with the composite material prepared in the comparative example.
The technical solution protected by the present invention is not limited to the above embodiment, and other dispersion techniques obtained by the same or similar method as the above embodiment are within the scope of the present invention.
Claims (6)
1. A method for dispersing inorganic nano particle filler in solid epoxy resin is characterized in that: the method comprises the following steps:
(1) adding the inorganic nano-particle filler and the liquid epoxy resin into a ball mill, blending and dispersing to obtain a uniformly dispersed low-viscosity mixed solution;
(2) and adding the low-viscosity mixed solution into the molten liquid of the solid epoxy resin, and stirring to obtain a uniformly dispersed molten mixed solution.
2. A dispersion method according to claim 1, characterized in that: the time for blending and dispersing in the step (1) is 1-2 h; the grain diameter of the nano inorganic particle filler is 25-35 nm.
3. A dispersion method according to claim 1, characterized in that: in the step (1), the adding mass percentage of the nano inorganic particle filler is 2-3%.
4. A dispersion method according to claim 1, characterized in that: the mass ratio of the solid epoxy resin to the liquid epoxy resin is 8-10: 1.
5. A dispersion method according to claim 1, characterized in that: the nano inorganic particle filler is nano aluminum oxide, nano SiO2 or nano ZnO.
6. A dispersion method according to claim 1, characterized in that: the stirring in the step (2) refers to stirring for at least 1h under the conditions that the temperature is 130-150 ℃ and the stirring speed is 1000-1100 r/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910994827.1A CN110776719A (en) | 2019-10-18 | 2019-10-18 | Method for dispersing nano inorganic particle filler in solid epoxy resin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910994827.1A CN110776719A (en) | 2019-10-18 | 2019-10-18 | Method for dispersing nano inorganic particle filler in solid epoxy resin |
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| CN110776719A true CN110776719A (en) | 2020-02-11 |
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| CN201910994827.1A Pending CN110776719A (en) | 2019-10-18 | 2019-10-18 | Method for dispersing nano inorganic particle filler in solid epoxy resin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112341759A (en) * | 2020-11-18 | 2021-02-09 | 重庆大学 | Modified nano-alumina composite epoxy resin insulating material and preparation method thereof |
| CN115069112A (en) * | 2022-06-27 | 2022-09-20 | 广东电网有限责任公司 | Charged dispersing device for nano powder filler |
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| CN102675826A (en) * | 2012-04-25 | 2012-09-19 | 北京化工大学常州先进材料研究院 | Temperature-resistant high-strength high-toughness composite epoxy resin and manufacturing method thereof |
| CN102725323A (en) * | 2010-05-26 | 2012-10-10 | 京瓷化成株式会社 | Sheet-like resin composition, circuit component using the sheet-like resin composition, method for sealing electronic component, method for connecting electronic component, method for affixing electronic component, composite sheet, electronic component |
| CN103396656A (en) * | 2013-08-27 | 2013-11-20 | 连云港神鹰碳纤维自行车有限责任公司 | Preparation method of epoxy resin system for nanometer modified carbon fiber prepreg |
| CN104356605A (en) * | 2014-12-11 | 2015-02-18 | 哈尔滨广龙通用航空科技有限公司 | Light prepreg for unmanned aerial vehicle shell and preparation method of prepreg |
| CN108264727A (en) * | 2016-12-30 | 2018-07-10 | 比亚迪股份有限公司 | A kind of composition epoxy resin and epoxy resin composition and preparation method thereof and epoxy prepreg and composite material |
-
2019
- 2019-10-18 CN CN201910994827.1A patent/CN110776719A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102725323A (en) * | 2010-05-26 | 2012-10-10 | 京瓷化成株式会社 | Sheet-like resin composition, circuit component using the sheet-like resin composition, method for sealing electronic component, method for connecting electronic component, method for affixing electronic component, composite sheet, electronic component |
| CN102675826A (en) * | 2012-04-25 | 2012-09-19 | 北京化工大学常州先进材料研究院 | Temperature-resistant high-strength high-toughness composite epoxy resin and manufacturing method thereof |
| CN103396656A (en) * | 2013-08-27 | 2013-11-20 | 连云港神鹰碳纤维自行车有限责任公司 | Preparation method of epoxy resin system for nanometer modified carbon fiber prepreg |
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| CN108264727A (en) * | 2016-12-30 | 2018-07-10 | 比亚迪股份有限公司 | A kind of composition epoxy resin and epoxy resin composition and preparation method thereof and epoxy prepreg and composite material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112341759A (en) * | 2020-11-18 | 2021-02-09 | 重庆大学 | Modified nano-alumina composite epoxy resin insulating material and preparation method thereof |
| CN115069112A (en) * | 2022-06-27 | 2022-09-20 | 广东电网有限责任公司 | Charged dispersing device for nano powder filler |
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Application publication date: 20200211 |