CN110776669A - Heat-conducting flame retardant and preparation method thereof - Google Patents
Heat-conducting flame retardant and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a heat-conducting flame retardant which consists of nanometer boron nitride coated with polyether amine-polyimide block copolymer and magnesium hydroxide coated with polyether amine-polyimide block copolymer. The invention also relates to a preparation method of the heat-conducting flame retardant. The heat-conducting flame retardant disclosed by the invention can be effectively compatible with a polymer, so that the flame retardant property is improved, the strength of the polymer is not obviously reduced, and the high heat-conducting property can be provided.
Description
Technical Field
The invention relates to the technical field of flame retardants, and particularly relates to a heat-conducting flame retardant and a preparation method thereof.
Background
The flame retardant is widely applied to daily necessities, particularly added into plastic products. However, with the development of society, the application of the heat-conducting plastic is gradually widened, but the existing flame retardant only has a flame retardant effect, when the flame retardant is added into a polymer base material to prepare the heat-conducting plastic, the heat-conducting performance is often difficult to be simultaneously achieved, and the strength of a plastic product is reduced due to too high addition of the flame retardant.
Therefore, technical innovation is needed to prepare a novel heat-conducting flame retardant, so that the flame retardant can be effectively compatible with a polymer, namely, the flame retardant property and the heat-conducting property are improved, and the strength of the polymer cannot be obviously reduced.
Disclosure of Invention
In order to solve the problems, the invention discloses a heat-conducting flame retardant which is characterized by consisting of nanometer boron nitride coated with a polyether amine-polyimide block copolymer and magnesium hydroxide coated with the polyether amine-polyimide block copolymer.
In one embodiment, the nano boron nitride has an average particle size of 100 nm to 500 nm; preferably, the average particle size of the nano boron nitride is 200 nm-500 nm; more preferably, the nano boron nitride has an average particle size of 300 nm.
In one embodiment, the polyetheramine-polyimide block copolymer is prepared by the following steps:
(1) sequentially adding epoxy resin E51105 g, benzylamine 0.255mol and 900ml propylene glycol methyl ether into a dry reaction bottle under the protection of nitrogen, heating to 110 ℃, reacting for 5 hours under mechanical stirring, cooling to room temperature, pouring the reaction solution into deionized water to obtain a large amount of white precipitate, performing suction filtration, and fully drying the white precipitate to obtain epoxy-terminated polyetheramine;
(2) and (2) sequentially adding 21mmol of dodecanediamine, 20mmol of 1, 4, 5, 8-naphthalene tetracarboxylic dianhydride, 125mL of m-cresol and 7mL of triethylamine into a dry three-necked bottle, introducing nitrogen for protection, mechanically stirring for 1h, heating to 80 ℃ for reaction for 4h, cooling to room temperature after reacting at 180 ℃ for 4h, then adding 1mmol of epoxy-terminated polyetheramine obtained in the step (1), 100mL of propylene glycol methyl ether and 50mL of DMF, introducing nitrogen for protection, mechanically stirring for 1h, heating to 80 ℃ for reaction for 4h, pouring the reaction solution into ethanol to obtain a large amount of yellow precipitates, performing suction filtration, and fully drying the yellow precipitates to obtain the polyetheramine-polyimide block copolymer.
The invention also provides a method for preparing the heat-conducting flame retardant, which comprises the step of coating the nanometer boron nitride and the magnesium hydroxide by using the polyether amine-polyimide segmented copolymer.
In one embodiment, the coating is performed in a mixed solvent.
In one embodiment, the mixed solvent is m-cresol and propylene glycol methyl ether in a weight ratio of 1: the mixture of (1-5); preferably, the mixed solvent is m-cresol and propylene glycol methyl ether in a weight ratio of 1: 2, or a mixture thereof.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Firstly, preparing a polyether amine-polyimide segmented copolymer, wherein the method comprises the following steps:
(1) sequentially adding epoxy resin E51105 g, benzylamine 0.255mol and 900ml propylene glycol methyl ether into a dry reaction bottle under the protection of nitrogen, heating to 110 ℃, reacting for 5 hours under mechanical stirring, cooling to room temperature, pouring the reaction solution into deionized water to obtain a large amount of white precipitate, performing suction filtration, and fully drying the white precipitate to obtain epoxy-terminated polyetheramine;
(2) and (2) sequentially adding 21mmol of dodecanediamine, 20mmol of 1, 4, 5, 8-naphthalene tetracarboxylic dianhydride, 125mL of m-cresol and 7mL of triethylamine into a dry three-necked bottle, introducing nitrogen for protection, mechanically stirring for 1h, heating to 80 ℃ for reaction for 4h, cooling to room temperature after reacting at 180 ℃ for 4h, then adding 1mmol of epoxy-terminated polyetheramine obtained in the step (1), 100mL of propylene glycol methyl ether and 50mL of DMF, introducing nitrogen for protection, mechanically stirring for 1h, heating to 80 ℃ for reaction for 4h, pouring the reaction solution into ethanol to obtain a large amount of yellow precipitates, performing suction filtration, and fully drying the yellow precipitates to obtain the polyetheramine-polyimide block copolymer.
Secondly, preparing the heat-conducting flame retardant, wherein the method comprises the following steps:
at 50 ℃, 5 g of the above polyetheramine-polyimide block copolymer was dissolved in 100 g of m-cresol and propylene glycol methyl ether at a weight ratio of 1: 2, then adding 15 g of boron nitride with the average particle size of 300 nanometers and 5 g of magnesium hydroxide with the average particle size of 1 micrometer, maintaining the temperature at 50 ℃, mechanically stirring for 2 hours, carrying out suction filtration on the solution to obtain a large amount of solid, and fully drying the solid to obtain the heat-conducting flame retardant.
Comparative example 1
Firstly, preparing a polyether amine-polyimide segmented copolymer, wherein the method comprises the following steps:
(1) sequentially adding epoxy resin E51105 g, benzylamine 0.255mol and 900ml propylene glycol methyl ether into a dry reaction bottle under the protection of nitrogen, heating to 110 ℃, reacting for 5 hours under mechanical stirring, cooling to room temperature, pouring the reaction solution into deionized water to obtain a large amount of white precipitate, performing suction filtration, and fully drying the white precipitate to obtain epoxy-terminated polyetheramine;
(2) and (2) sequentially adding 21mmol of dodecanediamine, 20mmol of 1, 4, 5, 8-naphthalene tetracarboxylic dianhydride, 125mL of m-cresol and 7mL of triethylamine into a dry three-necked bottle, introducing nitrogen for protection, mechanically stirring for 1h, heating to 80 ℃ for reaction for 4h, cooling to room temperature after reacting at 180 ℃ for 4h, then adding 1mmol of epoxy-terminated polyetheramine obtained in the step (1), 100mL of propylene glycol methyl ether and 50mL of DMF, introducing nitrogen for protection, mechanically stirring for 1h, heating to 80 ℃ for reaction for 4h, pouring the reaction solution into ethanol to obtain a large amount of yellow precipitates, performing suction filtration, and fully drying the yellow precipitates to obtain the polyetheramine-polyimide block copolymer.
Secondly, preparing the heat-conducting flame retardant, wherein the method comprises the following steps:
at 50 ℃, 5 g of the above polyetheramine-polyimide block copolymer was dissolved in 100 g of m-cresol and propylene glycol methyl ether at a weight ratio of 1: 2, then adding 15 g of boron nitride with the average particle size of 100 nanometers and 5 g of magnesium hydroxide with the average particle size of 1 micrometer, maintaining the temperature at 50 ℃, mechanically stirring for 2 hours, carrying out suction filtration on the solution to obtain a large amount of solid, and fully drying the solid to obtain the heat-conducting flame retardant.
Comparative example 2
Firstly, preparing a polyether amine-polyimide segmented copolymer, wherein the method comprises the following steps:
(1) sequentially adding epoxy resin E51105 g, benzylamine 0.255mol and 900ml propylene glycol methyl ether into a dry reaction bottle under the protection of nitrogen, heating to 110 ℃, reacting for 5 hours under mechanical stirring, cooling to room temperature, pouring the reaction solution into deionized water to obtain a large amount of white precipitate, performing suction filtration, and fully drying the white precipitate to obtain epoxy-terminated polyetheramine;
(2) and (2) sequentially adding 21mmol of dodecanediamine, 20mmol of 1, 4, 5, 8-naphthalene tetracarboxylic dianhydride, 125mL of m-cresol and 7mL of triethylamine into a dry three-necked bottle, introducing nitrogen for protection, mechanically stirring for 1h, heating to 80 ℃ for reaction for 4h, cooling to room temperature after reacting at 180 ℃ for 4h, then adding 1mmol of epoxy-terminated polyetheramine obtained in the step (1), 100mL of propylene glycol methyl ether and 50mL of DMF, introducing nitrogen for protection, mechanically stirring for 1h, heating to 80 ℃ for reaction for 4h, pouring the reaction solution into ethanol to obtain a large amount of yellow precipitates, performing suction filtration, and fully drying the yellow precipitates to obtain the polyetheramine-polyimide block copolymer.
Secondly, preparing the heat-conducting flame retardant, wherein the method comprises the following steps:
at 50 ℃, 5 g of the above polyetheramine-polyimide block copolymer was dissolved in 100 g of m-cresol and propylene glycol methyl ether at a weight ratio of 1: 2, then adding 15 g of boron nitride with the average particle size of 1 micron and 5 g of magnesium hydroxide with the average particle size of 1 micron, maintaining the temperature at 50 ℃ and mechanically stirring for 2 hours, then carrying out suction filtration on the solution to obtain a large amount of solid, and fully drying the solid to obtain the heat-conducting flame retardant.
Comparative example 3
Firstly, preparing polyether amine, wherein the method comprises the following steps:
and (2) sequentially adding epoxy resin E51100 g, benzylamine 0.255mol and 900ml propylene glycol methyl ether into a dry reaction bottle under the protection of nitrogen, heating to 110 ℃, reacting for 5 hours under mechanical stirring, cooling to room temperature, pouring the reaction solution into deionized water to obtain a large amount of white precipitate, and performing suction filtration and full drying on the white precipitate to obtain the polyetheramine.
Secondly, preparing the heat-conducting flame retardant, wherein the method comprises the following steps:
at 50 ℃, dissolving 5 g of the polyether amine in 100 g of propylene glycol methyl ether, then adding 15 g of boron nitride with the average particle size of 300 nanometers and 5 g of magnesium hydroxide with the average particle size of 1 micrometer, maintaining the temperature at 50 ℃, mechanically stirring for 2 hours, carrying out suction filtration on the solution to obtain a large amount of solid, and fully drying the solid to obtain the heat-conducting flame retardant.
Comparative example 4
Firstly, preparing polyimide, comprising the following steps:
and sequentially adding 20mmol of dodecanediamine, 20mmol of 1, 4, 5, 8-naphthalene tetracarboxylic dianhydride, 125mL of m-cresol and 7mL of triethylamine into a dried three-necked bottle, introducing nitrogen for protection, mechanically stirring for 1h, heating to 80 ℃ for reaction for 4h, cooling to room temperature after reaction for 24h at 180 ℃, pouring the reaction solution into ethanol to obtain a large amount of yellow precipitate, performing suction filtration, and fully drying the yellow precipitate to obtain the polyimide.
Secondly, preparing the heat-conducting flame retardant, wherein the method comprises the following steps:
at 50 ℃, dissolving 5 g of the polyimide in 100 g of m-cresol, then adding 15 g of boron nitride with the average particle size of 300 nanometers and 5 g of magnesium hydroxide with the average particle size of 1 micrometer, maintaining the temperature at 50 ℃, mechanically stirring for 2 hours, carrying out suction filtration on the solution to obtain a large amount of solid, and fully drying the solid to obtain the heat-conducting flame retardant.
Comparative example 5
Firstly, preparing a polyether amine-polyimide segmented copolymer, wherein the method comprises the following steps:
(1) sequentially adding epoxy resin E51105 g, benzylamine 0.255mol and 900ml propylene glycol methyl ether into a dry reaction bottle under the protection of nitrogen, heating to 110 ℃, reacting for 5 hours under mechanical stirring, cooling to room temperature, pouring the reaction solution into deionized water to obtain a large amount of white precipitate, performing suction filtration, and fully drying the white precipitate to obtain epoxy-terminated polyetheramine;
(2) and (2) sequentially adding 21mmol of dodecanediamine, 20mmol of 1, 4, 5, 8-naphthalene tetracarboxylic dianhydride, 125mL of m-cresol and 7mL of triethylamine into a dry three-necked bottle, introducing nitrogen for protection, mechanically stirring for 1h, heating to 80 ℃ for reaction for 4h, cooling to room temperature after reacting at 180 ℃ for 4h, then adding 1mmol of epoxy-terminated polyetheramine obtained in the step (1), 100mL of propylene glycol methyl ether and 50mL of DMF, introducing nitrogen for protection, mechanically stirring for 1h, heating to 80 ℃ for reaction for 4h, pouring the reaction solution into ethanol to obtain a large amount of yellow precipitates, performing suction filtration, and fully drying the yellow precipitates to obtain the polyetheramine-polyimide block copolymer.
Secondly, preparing the heat-conducting flame retardant, wherein the method comprises the following steps:
at 50 ℃, 5 g of the above polyetheramine-polyimide block copolymer was dissolved in 100 g of m-cresol and propylene glycol methyl ether at a weight ratio of 1: 1, then adding 15 g of boron nitride with the average particle size of 300 nanometers and 5 g of magnesium hydroxide with the average particle size of 1 micrometer, maintaining the temperature at 50 ℃, mechanically stirring for 2 hours, carrying out suction filtration on the solution to obtain a large amount of solid, and fully drying the solid to obtain the heat-conducting flame retardant.
Comparative example 6
Firstly, preparing a polyether amine-polyimide segmented copolymer, wherein the method comprises the following steps:
(1) sequentially adding epoxy resin E51105 g, benzylamine 0.255mol and 900ml propylene glycol methyl ether into a dry reaction bottle under the protection of nitrogen, heating to 110 ℃, reacting for 5 hours under mechanical stirring, cooling to room temperature, pouring the reaction solution into deionized water to obtain a large amount of white precipitate, performing suction filtration, and fully drying the white precipitate to obtain epoxy-terminated polyetheramine;
(2) and (2) sequentially adding 21mmol of dodecanediamine, 20mmol of 1, 4, 5, 8-naphthalene tetracarboxylic dianhydride, 125mL of m-cresol and 7mL of triethylamine into a dry three-necked bottle, introducing nitrogen for protection, mechanically stirring for 1h, heating to 80 ℃ for reaction for 4h, cooling to room temperature after reacting at 180 ℃ for 4h, then adding 1mmol of epoxy-terminated polyetheramine obtained in the step (1), 100mL of propylene glycol methyl ether and 50mL of DMF, introducing nitrogen for protection, mechanically stirring for 1h, heating to 80 ℃ for reaction for 4h, pouring the reaction solution into ethanol to obtain a large amount of yellow precipitates, performing suction filtration, and fully drying the yellow precipitates to obtain the polyetheramine-polyimide block copolymer.
Secondly, preparing the heat-conducting flame retardant, wherein the method comprises the following steps:
at 50 ℃, 5 g of the above polyetheramine-polyimide block copolymer was dissolved in 100 g of m-cresol and propylene glycol methyl ether at a weight ratio of 1: 5, then adding 15 g of boron nitride with the average particle size of 300 nanometers and 5 g of magnesium hydroxide with the average particle size of 1 micrometer, maintaining the temperature at 50 ℃, mechanically stirring for 2 hours, carrying out suction filtration on the solution to obtain a large amount of solid, and fully drying the solid to obtain the heat-conducting flame retardant.
Testing
Mixing PA6 resin with the heat-conducting flame retardant of any one of the embodiment 1 and the comparative examples 1-6 according to a mass ratio of 4: 1, putting the mixture into a high-speed dispersion machine, uniformly stirring, and extruding by a screw to obtain the heat-conducting plastic.
Mixing PA6 resin and uncoated inorganic filler (namely boron nitride with the average particle size of 300 nanometers and magnesium hydroxide with the average particle size of 1 micrometer, wherein the weight ratio of the boron nitride to the magnesium hydroxide is 3: 1) according to the weight ratio of 4: 1 was put into a high-speed dispersion machine and stirred uniformly, and then was extruded by a screw to obtain a thermally conductive plastic (comparative example 7).
The thermally conductive plastics obtained as described above were tested and the results are shown in table 1 below.
TABLE 1
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. The heat-conducting flame retardant is characterized by consisting of nanometer boron nitride coated with a polyether amine-polyimide block copolymer and magnesium hydroxide coated with the polyether amine-polyimide block copolymer.
2. The thermally conductive flame retardant of claim 1, wherein the nano boron nitride has an average particle size of 100 nm to 500 nm.
3. The thermally conductive flame retardant of claim 2, wherein the nano boron nitride has an average particle size of 200 nm to 500 nm.
4. The thermally conductive flame retardant of claim 3, wherein the nano boron nitride has an average particle size of 300 nm.
5. The thermally conductive flame retardant of claim 1, wherein the polyetheramine-polyimide block copolymer is prepared by the following steps:
(1) sequentially adding epoxy resin E51105 g, benzylamine 0.255mol and 900ml propylene glycol methyl ether into a dry reaction bottle under the protection of nitrogen, heating to 110 ℃, reacting for 5 hours under mechanical stirring, cooling to room temperature, pouring the reaction solution into deionized water to obtain a large amount of white precipitate, performing suction filtration, and fully drying the white precipitate to obtain epoxy-terminated polyetheramine;
(2) and (2) sequentially adding 21mmol of dodecanediamine, 20mmol of 1, 4, 5, 8-naphthalene tetracarboxylic dianhydride, 125mL of m-cresol and 7mL of triethylamine into a dry three-necked bottle, introducing nitrogen for protection, mechanically stirring for 1h, heating to 80 ℃ for reaction for 4h, cooling to room temperature after reacting at 180 ℃ for 4h, then adding 1mmol of epoxy-terminated polyetheramine obtained in the step (1), 100mL of propylene glycol methyl ether and 50mL of DMF, introducing nitrogen for protection, mechanically stirring for 1h, heating to 80 ℃ for reaction for 4h, pouring the reaction solution into ethanol to obtain a large amount of yellow precipitates, performing suction filtration, and fully drying the yellow precipitates to obtain the polyetheramine-polyimide block copolymer.
6. The method for preparing the heat-conducting flame retardant comprises the step of coating the nanometer boron nitride and the magnesium hydroxide by using the polyether amine-polyimide segmented copolymer.
7. The method of claim 6, wherein the coating is performed in a mixed solvent.
8. The method of claim 7, wherein the mixed solvent is m-cresol and propylene glycol methyl ether in a weight ratio of 1: (1-5).
9. The method of claim 8, wherein the mixed solvent is m-cresol and propylene glycol methyl ether in a weight ratio of 1: 2, or a mixture thereof.
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Cited By (1)
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