CN110760100A - Preparation method of coated efficient flame retardant - Google Patents
Preparation method of coated efficient flame retardant Download PDFInfo
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- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2618—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen
- C08G65/2621—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups
- C08G65/2627—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups containing aromatic or arylaliphatic amine groups
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- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1046—Polyimides containing oxygen in the form of ether bonds in the main chain
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1075—Partially aromatic polyimides
- C08G73/1082—Partially aromatic polyimides wholly aromatic in the tetracarboxylic moiety
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- 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
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- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/34—Silicon-containing compounds
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- C08K9/10—Encapsulated ingredients
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- 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
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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
- C08K2201/003—Additives being defined by their diameter
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Abstract
The invention relates to a preparation method of a coated efficient flame retardant, which comprises the following steps: preparing a polyetheramine-polyimide block copolymer for coating; dissolving the polyether amine-polyimide segmented copolymer in a solvent, and then adding various inorganic fillers and silane coupling agents; heating and fully stirring, carrying out suction filtration, and drying the obtained solid to obtain the coated efficient flame retardant. The coated efficient flame retardant can be effectively compatible with polymers, so that the flame retardant property is improved, and the strength of the polymers cannot be obviously reduced.
Description
Technical Field
The invention relates to the technical field of preparation of flame retardants, in particular to a preparation method of a coated efficient flame retardant.
Background
In recent years, non-halogenation of flame retardants has become the mainstream of development, and inorganic flame retardants have been rapidly developed. However, since inorganic flame retardants seriously affect the mechanical properties of polymers, a single inorganic flame retardant cannot meet the requirements of high-efficiency flame retardance and high strength of materials. The compounding of inorganic flame-retardant fillers has gradually become one of the main development directions of inorganic flame-retardant fillers in recent years. However, simple compounding still fails to solve the above-described problems.
Therefore, there is a need for improvements in the manufacturing process to obtain high performance flame retardant synergists that are effectively compatible with polymers, i.e., improve flame retardant properties, without significantly reducing the strength of the polymer.
Disclosure of Invention
Therefore, the invention discloses a preparation method of a coated efficient flame retardant, which comprises the following steps:
(1) preparing a polyetheramine-polyimide block copolymer for coating;
(2) dissolving the polyether amine-polyimide segmented copolymer in a solvent, and then adding various inorganic fillers and silane coupling agents;
(3) heating and fully stirring, carrying out suction filtration, and drying the obtained solid to obtain the coated efficient flame retardant.
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 ℃, reacting for 4h, cooling to room temperature after reacting for 4h at 180 ℃, then adding 0.9mmol 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 ℃, reacting for 4h, pouring the reaction solution into ethanol to obtain a large amount of yellow precipitates, and performing suction filtration and full drying on the yellow precipitates to obtain the polyetheramine-polyimide block copolymer.
In one embodiment, the solvent is a mixed solvent.
In one embodiment, the mixed solvent is a mixture of m-cresol and propylene glycol methyl ether in a weight ratio of 1 (1-5); preferably, the mixed solvent is a mixture of m-cresol and propylene glycol methyl ether in a weight ratio of 1: 2.
In one embodiment, the plurality of inorganic fillers are hydrotalcite, silica, and titanium dioxide.
In one embodiment, the hydrotalcite has an average particle size of 500 nm to 1 μm, the silica has an average particle size of 50 nm to 150 nm, and the titania has an average particle size of 200 nm to 500 nm; preferably, the hydrotalcite has an average particle size of 1 micrometer, the silica has an average particle size of 100 nanometers, and the titania has an average particle size of 500 nanometers.
In one embodiment, the weight ratio of the hydrotalcite, the silica, and the titanium dioxide is 1 (1-3) to (1-3); preferably, the weight ratio of the hydrotalcite, the silica and the titania is 1:2: 1.
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
The preparation method of the coated efficient flame retardant 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;
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 ℃, reacting for 4h, cooling to room temperature after reacting for 4h at 180 ℃, then adding 0.9mmol 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 ℃, reacting for 4h, pouring the reaction solution into ethanol to obtain a large amount of yellow precipitates, and performing suction filtration and full drying on the yellow precipitates to obtain the polyetheramine-polyimide block copolymer.
(2) At 50 ℃, 10 g of the above polyetheramine-polyimide block copolymer was dissolved in 30 g of m-cresol and propylene glycol methyl ether at a weight ratio of 1:2, then 5 g of hydrotalcite (average particle diameter of 1 μm), 10 g of silica (average particle diameter of 100 nm) and 5 g of titania (average particle diameter of 500 nm) were added thereto, and after maintaining 50 c and mechanically stirring for 2 hours,
(3) and carrying out suction filtration on the solution to obtain a large amount of solid, and fully drying the solid to obtain the coated efficient flame retardant.
Comparative example 1
The preparation method of the coated efficient flame retardant 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;
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 ℃, reacting for 4h, cooling to room temperature after reacting for 4h at 180 ℃, then adding 0.9mmol 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 ℃, reacting for 4h, pouring the reaction solution into ethanol to obtain a large amount of yellow precipitates, and performing suction filtration and full drying on the yellow precipitates to obtain the polyetheramine-polyimide block copolymer.
(2) At 50 ℃, 10 g of the above polyetheramine-polyimide block copolymer was dissolved in 30 g of m-cresol and propylene glycol methyl ether at a weight ratio of 1:2, then 5 g of hydrotalcite (average particle diameter of 1 μm), 10 g of silica (average particle diameter of 150 nm) and 5 g of titania (average particle diameter of 200 nm) were added thereto, and after maintaining 50 c and mechanically stirring for 2 hours,
(3) and carrying out suction filtration on the solution to obtain a large amount of solid, and fully drying the solid to obtain the coated efficient flame retardant.
Comparative example 2
The preparation method of the coated efficient flame retardant 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;
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 ℃, reacting for 4h, cooling to room temperature after reacting for 4h at 180 ℃, then adding 0.9mmol 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 ℃, reacting for 4h, pouring the reaction solution into ethanol to obtain a large amount of yellow precipitates, and performing suction filtration and full drying on the yellow precipitates to obtain the polyetheramine-polyimide block copolymer.
(2) At 50 ℃, 10 g of the polyetheramine-polyimide block copolymer was dissolved in 30 g of m-cresol and propylene glycol methyl ether at a weight ratio of 1:2, then 5 g of hydrotalcite (average particle diameter of 1 μm), 10 g of silica (average particle diameter of 100 nm) and 10 g of titania (average particle diameter of 500 nm) were added thereto, and after maintaining 50 c and mechanically stirring for 2 hours,
(3) and carrying out suction filtration on the solution to obtain a large amount of solid, and fully drying the solid to obtain the coated efficient flame retardant.
Comparative example 3
The preparation method of the coated efficient flame retardant 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;
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 ℃, reacting for 4h, cooling to room temperature after reacting for 4h at 180 ℃, then adding 0.9mmol 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 ℃, reacting for 4h, pouring the reaction solution into ethanol to obtain a large amount of yellow precipitates, and performing suction filtration and full drying on the yellow precipitates to obtain the polyetheramine-polyimide block copolymer.
(2) At 50 ℃, 10 g of the polyetheramine-polyimide block copolymer was dissolved in 30 g of m-cresol and propylene glycol methyl ether at a weight ratio of 1: 5, then 5 g of hydrotalcite (average particle diameter of 1 μm), 10 g of silica (average particle diameter of 150 nm) and 5 g of titania (average particle diameter of 200 nm) were added to the mixed solvent, and after maintaining 50 ℃ and mechanically stirring for 2 hours,
(3) and carrying out suction filtration on the solution to obtain a large amount of solid, and fully drying the solid to obtain the coated efficient flame retardant.
Comparative example 4
The preparation method of the coated flame retardant comprises the following steps:
(1) 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.
(2) At 50 ℃, 10 g of the above polyetheramine was dissolved in 30 g of m-cresol and propylene glycol methyl ether in a weight ratio of 1:2, then 5 g of hydrotalcite (average particle diameter of 1 μm), 10 g of silica (average particle diameter of 100 nm) and 5 g of titania (average particle diameter of 500 nm) were added thereto, and after maintaining 50 c and mechanically stirring for 2 hours,
(3) and carrying out suction filtration on the solution to obtain a large amount of solid, and fully drying the solid to obtain the coated flame retardant.
Comparative example 5
The preparation method of the coated efficient flame retardant comprises the following steps:
(1) adding 20mmol 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 in sequence, introducing nitrogen for protection, mechanically stirring for 1h, heating to 80 ℃ for reaction for 4h, cooling to room temperature after reacting for 24h at 180 ℃, pouring the reaction solution into ethanol to obtain a large amount of yellow precipitate, and performing suction filtration and full drying on the yellow precipitate to obtain polyimide.
(2) At 50 ℃, 10 g of the above polyimide was dissolved in 30 g of m-cresol and propylene glycol methyl ether in a weight ratio of 1:2, then 5 g of hydrotalcite (average particle diameter of 1 μm), 10 g of silica (average particle diameter of 100 nm) and 5 g of titania (average particle diameter of 500 nm) were added thereto, and after maintaining 50 c and mechanically stirring for 2 hours,
(3) and carrying out suction filtration on the solution to obtain a large amount of solid, and fully drying the solid to obtain the coated efficient flame retardant.
Testing
Mixing ethylene-vinyl acetate copolymer (EVA) and the coated high-efficiency flame retardant of any one of the embodiment 1 and the comparative examples 1-5 according to the mass ratio of 5: 2, placing the mixture into a high-speed dispersion machine, stirring the mixture evenly, and obtaining the EVA film material through tape casting extrusion.
Mixing ethylene-vinyl acetate copolymer (EVA) and uncoated inorganic filler (i.e. hydrotalcite with average particle size of 1 micron, silicon dioxide with average particle size of 100 nm and titanium dioxide with average particle size of 500 nm in a weight ratio of 1:2:1) according to a weight ratio of 5: 2, placing the mixture into a high-speed dispersion machine to be uniformly stirred, and then carrying out tape casting extrusion to obtain the EVA film material (comparative example 6).
The EVA film material obtained above was 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. A preparation method of a coated efficient flame retardant comprises the following steps:
(1) preparing a polyetheramine-polyimide block copolymer for coating;
(2) dissolving the polyether amine-polyimide segmented copolymer in a solvent, and then adding various inorganic fillers and silane coupling agents;
(3) heating and fully stirring, carrying out suction filtration, and drying the obtained solid to obtain the coated efficient flame retardant.
2. The method of claim 1, wherein the polyetheramine-polyimide block copolymer is prepared by:
(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 ℃, reacting for 4h, cooling to room temperature after reacting for 4h at 180 ℃, then adding 0.9mmol 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 ℃, reacting for 4h, pouring the reaction solution into ethanol to obtain a large amount of yellow precipitates, and performing suction filtration and full drying on the yellow precipitates to obtain the polyetheramine-polyimide block copolymer.
3. The method of claim 1, wherein the solvent is a mixed solvent.
4. The method according to claim 3, wherein the mixed solvent is a mixture of m-cresol and propylene glycol methyl ether in a weight ratio of 1 (1-5).
5. The method according to claim 4, wherein the mixed solvent is a mixture of m-cresol and propylene glycol methyl ether in a weight ratio of 1: 2.
6. The method of claim 1, wherein the plurality of inorganic fillers are hydrotalcite, silica, and titanium dioxide.
7. The method according to claim 6, wherein the hydrotalcite has an average particle size of 500 nm to 1 μm, the silica has an average particle size of 50 nm to 150 nm, and the titania has an average particle size of 200 nm to 500 nm.
8. The method of claim 6, wherein the weight ratio of the hydrotalcite, the silica and the titanium dioxide is 1 (1-3) to (1-3).
9. The method according to claim 8, wherein the weight ratio of the hydrotalcite, the silica and the titanium dioxide is 1:1: 1.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2557144A1 (en) * | 2011-08-11 | 2013-02-13 | Afton Chemical Corporation | Lubricant compositions containing a functionalized dispersant |
| CN105505289A (en) * | 2015-12-27 | 2016-04-20 | 上海创益中空玻璃材料有限公司 | High-strength polysulfide waterproof structure adhesive and preparing method thereof |
| CN106898802A (en) * | 2017-02-28 | 2017-06-27 | 广州市新稀复合材料有限公司 | A kind of high-performing car hydrogen fuel cell composite nano-powder material and preparation method thereof |
| CN109161147A (en) * | 2018-08-09 | 2019-01-08 | 湖北荆开电气有限公司 | A kind of flame-proof environmental protection insulating materials being used to prepare power distribution cabinet cable |
| CN110093016A (en) * | 2019-05-31 | 2019-08-06 | 北京化工大学 | A kind of preparation method of low dielectric composite material |
-
2019
- 2019-09-24 CN CN201910907061.9A patent/CN110760100A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2557144A1 (en) * | 2011-08-11 | 2013-02-13 | Afton Chemical Corporation | Lubricant compositions containing a functionalized dispersant |
| CN105505289A (en) * | 2015-12-27 | 2016-04-20 | 上海创益中空玻璃材料有限公司 | High-strength polysulfide waterproof structure adhesive and preparing method thereof |
| CN106898802A (en) * | 2017-02-28 | 2017-06-27 | 广州市新稀复合材料有限公司 | A kind of high-performing car hydrogen fuel cell composite nano-powder material and preparation method thereof |
| CN109161147A (en) * | 2018-08-09 | 2019-01-08 | 湖北荆开电气有限公司 | A kind of flame-proof environmental protection insulating materials being used to prepare power distribution cabinet cable |
| CN110093016A (en) * | 2019-05-31 | 2019-08-06 | 北京化工大学 | A kind of preparation method of low dielectric composite material |
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