CN111909485A - Epoxy resin composite board and preparation method thereof - Google Patents
Epoxy resin composite board and preparation method thereof Download PDFInfo
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- CN111909485A CN111909485A CN201910390209.6A CN201910390209A CN111909485A CN 111909485 A CN111909485 A CN 111909485A CN 201910390209 A CN201910390209 A CN 201910390209A CN 111909485 A CN111909485 A CN 111909485A
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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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
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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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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- 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
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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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
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
Abstract
The invention relates to an epoxy resin composite board which comprises the following raw materials in parts by weight: 20-30 parts of epoxy resin, 3-8 parts of amine curing agent, 55-70 parts of silicon micropowder, 5-9 parts of graphene, 0.1-0.3 part of color paste, 0.1-0.3 part of flame retardant additive, 0.05-0.2 part of silane coupling agent and 0.5-2 parts of natural mineral substance; the particle size of the silicon micro powder is 300-500 meshes, and the particle size of the natural mineral substance is 50-250 meshes. The invention also relates to a preparation method of the epoxy resin composite board. According to the invention, graphene is added into an epoxy resin system to participate in reaction, and natural mineral substances with different particle sizes are added to fill the gaps of the silicon micropowder, so that the plate is more compact, and the surface scratch resistance, wear resistance and temperature resistance of the plate are obviously improved. According to the invention, the product is not easy to warp and deform by adding the graphene and the silane coupling agent.
Description
Technical Field
The invention relates to the field of epoxy resin, in particular to a preparation method of an epoxy resin profile.
Background
Epoxy resin plates on the market at present are all single-color (namely pure color), quartz stone particles can be considered to be added for changing the color, but the quartz stone particles added in the processing process are easy to settle, so that the product particles are not uniformly dispersed. In addition, the scratch resistance and the temperature resistance of the surface of the obtained epoxy resin plate are not ideal.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides the epoxy resin composite board with good surface scratch resistance and temperature resistance and obvious improvement on color and luster and the preparation method thereof.
The specific technical scheme of the invention is as follows:
the epoxy resin composite board comprises the following raw materials in parts by weight:
the particle size of the silicon micro powder is 300-500 meshes, and the particle size of the natural mineral substance is 50-250 meshes.
The natural mineral substance can also be mixed by adopting the natural mineral substance with the particle size of 50-150 meshes and the natural mineral substance with the particle size of 150-250 meshes according to any proportion.
Preferably, the epoxy resin composite board comprises the following raw materials in parts by weight:
preferably, the amine curing agent is diethylenetriamine.
Preferably, the natural minerals are of the quartz granule type.
The invention also relates to a preparation method of the epoxy resin composite board, which comprises the following steps:
uniformly dispersing graphene into epoxy resin, and respectively preheating an amine curing agent and silicon micropowder; putting the epoxy resin, the amine curing agent and the color paste dispersed with the graphene into a reaction kettle, stirring, adding the flame-retardant auxiliary agent and the silane coupling agent, uniformly stirring, uniformly putting the silicon micropowder into the reaction kettle, and sufficiently and uniformly stirring to obtain a mixture; preheating the mould; putting natural mineral substances into the mixture, and stirring and mixing to obtain a mixed material; uniformly spreading the mixed material on a preheated mould, heating, then cooling, and demoulding to obtain a semi-finished product; and (4) carrying out secondary heating, heat preservation and cooling on the semi-finished product to obtain the epoxy resin composite board.
Preferably, the epoxy resin is heated to 80-120 ℃, the graphene is added into the epoxy resin at the speed of 50-70g/min and is stirred at a high speed in a dispersion kettle, so that the graphene is uniformly dispersed into the epoxy resin, the graphene and the epoxy resin can be completely fused, and the natural mineral substances are prevented from settling in the next step; respectively preheating the amine curing agent and the silicon micropowder to 50-70 ℃.
Preferably, the epoxy resin, the amine curing agent and the color paste dispersed with the graphene are put into a reaction kettle, the temperature in the reaction kettle is kept at 60-80 ℃, the mixture is stirred, the flame-retardant auxiliary agent and the silane coupling agent are added, the mixture is uniformly stirred, then the silicon micropowder is uniformly put into the reaction kettle, and the mixture is fully and uniformly stirred to obtain the mixture. When the temperature in the reaction kettle is lower than 60 ℃, the viscosity of the mixture is too thick, which is not beneficial to stirring of the stirrer; when the temperature is higher than 80 ℃, the mixture can react, so that the mixture can be solidified in the stirrer, and the subsequent operation can not be carried out.
Preferably, the mold is preheated to 110-; the mixture has good fluidity on the die, and the obtained product is smoother.
Preferably, the mixed material is evenly spread on a preheated mold, the temperature is raised to 70-90 ℃, the temperature is kept for 1-3 hours, then the temperature is reduced, and the semi-finished product is obtained after demolding; at which temperature the mix begins to set, converting the mix from a viscous state to a solid (i.e., a shaped slab).
Preferably, the semi-finished product is heated for the second time to 140-160 ℃, then is kept warm for 2-4 hours and is cooled to obtain the epoxy resin composite board; and (3) carrying out secondary curing on the semi-finished product, and carrying out secondary reaction on the epoxy resin and the curing agent to ensure that the reaction is more complete so as to ensure that the product achieves the optimal effect.
Putting natural mineral substances into the mixture, stirring and mixing to obtain a mixed material, and controlling the time to finish stirring within 5 minutes; if the stirring time is too long, natural mineral substances can be precipitated, the forming plate can be easily deformed, and the bending step is smooth; the short stirring time can cause uneven dispersion of quartz particles (natural minerals), which can cause the particles on the surface of the plate to be agglomerated and the surface to have no texture.
According to the invention, graphene is added into an epoxy resin system to participate in reaction, and natural mineral substances with different particle sizes are added to fill the gaps of the silicon micropowder, so that the plate is more compact, and the surface scratch resistance, wear resistance and temperature resistance of the plate are obviously improved. According to the invention, the product is not easy to warp and deform by adding the graphene and the silane coupling agent. In addition, after the preparation method disclosed by the invention is adopted, the graphene and the natural mineral substances (quartz stone particles) are uniformly dispersed in the epoxy resin plate, so that the texture is obviously improved.
Drawings
FIG. 1 is a schematic diagram showing the appearance of an epoxy resin composite board obtained in example 1;
fig. 2 is an appearance diagram of the epoxy resin composite panel manufactured in comparative example 1.
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are not part of the present invention but are prior art.
Example 1
The epoxy resin composite board comprises the following substances in parts by weight:
24 parts of epoxy resin, 5.5 parts of diethylenetriamine, 62 parts of silica powder, 7 parts of graphene, 0.2 part of color paste, 0.2 part of flame retardant additive, UP-5600.1 parts of silane coupling agent and 1 part of quartz particles, wherein the particle size of the silica powder is 400 meshes, and the particle size of the quartz particles is 100-200 meshes.
The preparation method of the epoxy resin composite board comprises the following steps:
(1) heating the epoxy resin to 100 ℃, adding graphene into the epoxy resin at a speed of 60g/min, and stirring at a high speed in a dispersion kettle to uniformly disperse the graphene into the epoxy resin; respectively preheating diethylenetriamine and silicon micropowder to 60 ℃;
(2) putting the epoxy resin, the diethylenetriamine and the color paste dispersed with the graphene into a reaction kettle, keeping the temperature in the reaction kettle at 60 ℃, stirring, adding the flame-retardant auxiliary agent and the silane coupling agent, uniformly stirring, then uniformly putting the silicon micropowder into the reaction kettle, and fully and uniformly stirring to obtain a mixture;
(3) preheating a mould to 120 ℃;
(4) putting quartz particles into the mixture, stirring and mixing to obtain a mixed material, and controlling the time to complete stirring within 5 minutes;
(5) uniformly spreading the mixed material on a preheated mould, heating to 80 ℃, then preserving heat for 2 hours, then cooling, and demoulding to obtain a semi-finished product;
(6) heating the semi-finished product for the second time to 150 ℃, then preserving heat for 3 hours, and cooling to obtain the epoxy resin composite board; referring to fig. 1, the quartz stone particles are uniformly dispersed in the epoxy resin plate, and the texture is obviously improved.
Example 2
The epoxy resin composite board comprises the following substances in parts by weight:
20 parts of epoxy resin, 4 parts of diethylenetriamine, 70 parts of silicon micropowder, 6 parts of graphene, 0.2 part of color paste, 0.1 part of flame retardant additive, UP-5600.08 parts of silane coupling agent and 0.8 part of quartz particles, wherein the particle size of the silicon micropowder is 300 meshes, and the particle size of the quartz particles is 200-250 meshes.
The preparation method of the epoxy resin composite board comprises the following steps:
(1) heating the epoxy resin to 80 ℃, adding the graphene into the epoxy resin at a speed of 65g/min, and stirring at a high speed in a dispersion kettle to uniformly disperse the graphene into the epoxy resin; respectively preheating diethylenetriamine and silicon micropowder to 50 ℃;
(2) putting the epoxy resin, the diethylenetriamine and the color paste dispersed with the graphene into a reaction kettle, keeping the temperature in the reaction kettle at 80 ℃, stirring, adding the flame-retardant auxiliary agent and the silane coupling agent, uniformly stirring, then uniformly putting the silicon micropowder into the reaction kettle, and fully and uniformly stirring to obtain a mixture;
(3) preheating a mould to 110 ℃;
(4) putting quartz particles into the mixture, stirring and mixing to obtain a mixed material, and controlling the time to complete stirring within 5 minutes;
(5) uniformly spreading the mixed material on a preheated mould, heating to 70 ℃, then preserving heat for 3 hours, then cooling, and demoulding to obtain a semi-finished product;
(6) and (4) heating the semi-finished product for the second time to 155 ℃, then preserving the heat for 1.5 hours, and cooling to obtain the epoxy resin composite board.
Example 3
The epoxy resin composite board comprises the following substances in parts by weight:
30 parts of epoxy resin, 8 parts of diethylenetriamine, 65 parts of silica powder, 5 parts of graphene, 0.3 part of color paste, 0.3 part of flame retardant additive, UP-5600.2 parts of silane coupling agent and 2 parts of quartz particles, wherein the particle size of the silica powder is 500 meshes, and the quartz particles are formed by mixing quartz particles with the particle size of 50-150 meshes and quartz particles with the particle size of 150-250 meshes according to the weight ratio of 1: 1.
The preparation method of the epoxy resin composite board comprises the following steps:
(1) heating the epoxy resin to 120 ℃, adding the graphene into the epoxy resin at the speed of 70g/min, and stirring at a high speed in a dispersion kettle to uniformly disperse the graphene into the epoxy resin; respectively preheating diethylenetriamine and silicon micropowder to 65 ℃;
(2) putting the epoxy resin, the diethylenetriamine and the color paste dispersed with the graphene into a reaction kettle, keeping the temperature in the reaction kettle at 60 ℃, stirring, adding the flame-retardant auxiliary agent and the silane coupling agent, uniformly stirring, then uniformly putting the silicon micropowder into the reaction kettle, and fully and uniformly stirring to obtain a mixture;
(3) preheating a mould to 130 ℃;
(4) putting quartz particles into the mixture, stirring and mixing to obtain a mixed material, and controlling the time to complete stirring within 5 minutes;
(5) uniformly spreading the mixed material on a preheated mould, heating to 75 ℃, then preserving heat for 1.5 hours, then cooling, and demoulding to obtain a semi-finished product;
(6) and (4) heating the semi-finished product for the second time to 160 ℃, then preserving heat for 2 hours, and cooling to obtain the epoxy resin composite board.
Example 4
The epoxy resin composite board comprises the following substances in parts by weight:
28 parts of epoxy resin, 3 parts of diethylenetriamine, 55 parts of silica powder, 9 parts of graphene, 0.1 part of color paste, 0.2 part of flame retardant additive, UP-5600.05 parts of silane coupling agent and 1.5 parts of quartz particles, wherein the particle size of the silica powder is 400 meshes, and the particle size of the quartz particles is 100-200 meshes.
The preparation method of the epoxy resin composite board comprises the following steps:
(1) heating epoxy resin to 115 ℃, adding graphene into the epoxy resin at a speed of 50g/min, and stirring at a high speed in a dispersion kettle to uniformly disperse the graphene into the epoxy resin; respectively preheating diethylenetriamine and silicon micropowder to 70 ℃;
(2) putting epoxy resin, diethylenetriamine and color paste dispersed with graphene into a reaction kettle, keeping the temperature in the reaction kettle at 75 ℃, stirring, adding a flame-retardant auxiliary agent and a silane coupling agent, uniformly stirring, then uniformly putting silicon micropowder into the reaction kettle, and fully and uniformly stirring to obtain a mixture;
(3) preheating a mould to 115 ℃;
(4) putting quartz particles into the mixture, stirring and mixing to obtain a mixed material, and controlling the time to complete stirring within 5 minutes;
(5) uniformly spreading the mixed material on a preheated mould, heating to 90 ℃, then preserving heat for 1 hour, then cooling, and demoulding to obtain a semi-finished product;
(6) and (4) heating the semi-finished product for the second time to 140 ℃, then preserving heat for 4 hours, and cooling to obtain the epoxy resin composite board.
Comparative example 1
The epoxy resin composite board comprises the following substances in parts by weight:
24 parts of epoxy resin, 5.5 parts of diethylenetriamine, 62 parts of silica powder, 0.2 part of color paste, 0.2 part of flame retardant additive, UP-5600.1 parts of silane coupling agent and 1 part of quartz particles, wherein the particle size of the silica powder is 400 meshes, and the particle size of the quartz particles is 100-200 meshes.
The preparation method of the epoxy resin composite board comprises the following steps:
(1) respectively preheating diethylenetriamine and silicon micropowder to 60 ℃;
(2) putting epoxy resin, diethylenetriamine and color paste into a reaction kettle, keeping the temperature in the reaction kettle at 60 ℃, stirring, adding a flame-retardant auxiliary agent and a silane coupling agent, uniformly stirring, then uniformly putting the silicon micropowder into the reaction kettle, and fully and uniformly stirring to obtain a mixture;
(3) preheating a mould to 120 ℃;
(4) putting quartz particles into the mixture, stirring and mixing to obtain a mixed material, and controlling the time to complete stirring within 5 minutes;
(5) uniformly spreading the mixed material on a preheated mould, heating to 80 ℃, then preserving heat for 2 hours, then cooling, and demoulding to obtain a semi-finished product;
(6) heating the semi-finished product for the second time to 150 ℃, then preserving heat for 3 hours, and cooling to obtain the epoxy resin composite board; referring to fig. 2, the surface particles are not uniformly distributed.
Comparative example 2
The epoxy resin composite board comprises the following substances in parts by weight:
24 parts of epoxy resin, 5.5 parts of diethylenetriamine, 62 parts of silicon micropowder, 7 parts of graphene, 0.2 part of color paste, 0.2 part of flame-retardant auxiliary agent, UP-5600.1 parts of silane coupling agent and 1 part of quartz particles.
The preparation method of the epoxy resin composite board comprises the following steps:
(1) heating the epoxy resin to 100 ℃, adding graphene into the epoxy resin at a speed of 60g/min, and stirring at a high speed in a dispersion kettle to uniformly disperse the graphene into the epoxy resin; respectively preheating diethylenetriamine and silicon micropowder to 60 ℃;
(2) putting the epoxy resin, the diethylenetriamine and the color paste dispersed with the graphene into a reaction kettle, keeping the temperature in the reaction kettle at 60 ℃, stirring, adding the flame-retardant auxiliary agent and the silane coupling agent, uniformly stirring, then uniformly putting the silicon micropowder into the reaction kettle, and fully and uniformly stirring to obtain a mixture;
(3) preheating a mould to 120 ℃;
(4) putting quartz particles into the mixture, stirring and mixing to obtain a mixed material, and controlling the time to complete stirring within 5 minutes;
(5) uniformly spreading the mixed material on a preheated mould, heating to 80 ℃, then preserving heat for 2 hours, then cooling, and demoulding to obtain a semi-finished product;
(6) and (4) heating the semi-finished product for the second time to 150 ℃, then preserving heat for 3 hours, and cooling to obtain the epoxy resin composite board.
See table 1 for performance data for each example.
TABLE 1
Claims (10)
1. The epoxy resin composite board is characterized by comprising the following raw materials in parts by weight:
the particle size of the silicon micro powder is 300-500 meshes, and the particle size of the natural mineral substance is 50-250 meshes.
2. The epoxy resin composite board according to claim 1, comprising the following raw materials in parts by weight:
3. the epoxy composite board according to claim 1 or 2, wherein the amine curing agent is diethylenetriamine.
4. The epoxy composite board according to claim 1 or 2, wherein the natural minerals are in the group of quartz particles.
5. A method of making an epoxy composite panel according to any preceding claim, comprising the steps of:
uniformly dispersing graphene into epoxy resin, and respectively preheating an amine curing agent and silicon micropowder;
putting the epoxy resin, the amine curing agent and the color paste dispersed with the graphene into a reaction kettle, stirring, adding the flame-retardant auxiliary agent and the silane coupling agent, uniformly stirring, uniformly putting the silicon micropowder into the reaction kettle, and sufficiently and uniformly stirring to obtain a mixture;
preheating the mould;
putting natural mineral substances into the mixture, and stirring and mixing to obtain a mixed material;
uniformly spreading the mixed material on a preheated mould, heating, then cooling, and demoulding to obtain a semi-finished product;
and (4) carrying out secondary heating, heat preservation and cooling on the semi-finished product to obtain the epoxy resin composite board.
6. The preparation method of the epoxy resin composite board according to claim 5, wherein the epoxy resin is heated to 80-120 ℃, the graphene is added into the epoxy resin at a speed of 50-70g/min, and the graphene is uniformly dispersed into the epoxy resin by high-speed stirring in a dispersion kettle; respectively preheating the amine curing agent and the silicon micropowder to 50-70 ℃.
7. The preparation method of the epoxy resin composite board according to claim 5 or 6, wherein the epoxy resin dispersed with graphene, the amine curing agent and the color paste are put into a reaction kettle, the temperature in the reaction kettle is kept at 60-80 ℃, the mixture is stirred, the flame retardant auxiliary agent and the silane coupling agent are added, the mixture is uniformly stirred, then the silica powder is uniformly put into the reaction kettle, and the mixture is fully and uniformly stirred to obtain the mixture.
8. The method for preparing an epoxy resin composite board according to claim 7, wherein the mold is preheated to 110-130 ℃.
9. The preparation method of the epoxy resin composite board according to claim 8, wherein the mixed material is uniformly spread on a preheated mold, heated to 70-90 ℃, kept warm for 1-3 hours, cooled, and demolded to obtain a semi-finished product.
10. The method for preparing the epoxy resin composite board according to claim 9, wherein the semi-finished product is heated for the second time to 140-160 ℃, then is kept warm for 2-4 hours, and is cooled to obtain the epoxy resin composite board.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113021159A (en) * | 2021-03-12 | 2021-06-25 | 安徽禾臣新材料有限公司 | Polishing pad for fine polishing of electronic display screen and production method thereof |
| CN113429862A (en) * | 2021-07-21 | 2021-09-24 | 安徽博纳新材料科技有限公司 | High-strength modified epoxy resin material and preparation method thereof |
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| CN103554861A (en) * | 2013-11-04 | 2014-02-05 | 哈尔滨市都邦节能科技有限公司 | Graphene high polymer plate as well as preparation method thereof |
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| CN113021159A (en) * | 2021-03-12 | 2021-06-25 | 安徽禾臣新材料有限公司 | Polishing pad for fine polishing of electronic display screen and production method thereof |
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| CN113429862A (en) * | 2021-07-21 | 2021-09-24 | 安徽博纳新材料科技有限公司 | High-strength modified epoxy resin material and preparation method thereof |
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Application publication date: 20201110 |