阅读说明：本技术 一种包覆型高效阻燃剂的制备方法 (Preparation method of coated efficient flame retardant ) 是由 周国庆 严晴 周志鑫 严一丰 于 2019-09-24 设计创作，主要内容包括：本发明涉及一种包覆型高效阻燃剂的制备方法,包括：制备用于包覆的聚醚胺-聚酰亚胺嵌段共聚物；将所述聚醚胺-聚酰亚胺嵌段共聚物溶解在溶剂中,然后加入多种无机填料以及硅烷偶联剂；加热并充分搅拌后,抽滤并将所得固体干燥,得包覆型高效阻燃剂。本发明的包覆型高效阻燃剂可以有效与聚合物兼容,即提高阻燃性能,又不会明显降低聚合物的强度。(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.)

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.

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.