Silicon-containing flame retardant polyether surface treating agent as well as preparation method and application thereof

Abstract

The invention discloses a silicon-containing flame retardant polyether surface treating agent. The silicon-containing flame retardant polyether surface treating agent contains three flame retardant elements including phosphorus, nitrogen and silicon, has the average molecular weight of 1,020-4,720, has the functionality of 6 and is a deep yellow transparent liquid. According to the preparation method, polyether polyol or polyether polyamine reacts with phenyl dichlorophosphate to generate flame retardant polyether, gamma-aminopropyltriethoxysilane is added, and the silicon-containing flame retardant polyether surface treating agent is prepared, wherein the gamma-aminopropyltriethoxysilane chain segment can be combined with a solid inorganic flame retardant through chemical bonds, and the polyether polyol chain segment and a polyether component for preparation of polyurethane resin have good compatibility. The surface treating agent has a flame retardant function, thus, solid inorganic flame retardant particles treated through the silicon-containing flame retardant polyether surface treating agent can be taken as flame retardant master batch and added to a formula material of polyurethane, and polyurethane foam with the solid inorganic flame retardant uniformly dispersed is obtained.

Description

technical field

[0001] The invention belongs to the technical field of polymer materials, and relates to a flame retardant surface treatment agent and its preparation method and application, in particular to a silicon-containing flame-retardant polyether surface treatment for a solid inorganic flame retardant of flame-retardant polyurethane Agents and their preparation methods and applications. Background technique

[0002] Polyurethane foam is widely used in refrigeration, construction, automobile and other industrial fields due to its light weight, high strength, excellent electrical insulation and low thermal conductivity. However, the porous cellular structure of polyurethane foam increases its contact area with air, making it highly flammable. In recent years, there have been more and more reports of fires caused by polyurethane foam igniting, so it is very necessary for it to be flame retardant.

[0003] At present, the flame retardants used in polyurethane foam are ...

Examples

Embodiment 1

[0023] Step (1). Mix polyether polyol with an average molecular weight of 300 and a functionality of 2 with triethylamine at a molar ratio of 1:2, and stir at 40°C for 0.5 hour in a nitrogen atmosphere to obtain a polyether polyol with a functionality of 2. Active hydrogen compounds of polyether polyols;

[0024] Step (2). Under the condition of continuous stirring, the active hydrogen compound of the polyether polyol with a functionality of 2 in the step (1) is added dropwise to the tetrahydrofuran solvent whose concentration of phenyl dichlorophosphate is 0.1mol / L, Make the molar ratio of phenyl dichlorophosphate and polyether polyol in the solution to be 2.1:1, add dropwise for 30 minutes, and react at 40°C for 5 hours;

[0025] Step (3). Add γ-aminopropyltriethoxysilane to the reaction solution, so that the molar ratio of γ-aminopropyltriethoxysilane and polyether polyol in the solution is 2.1:1, and then add three Ethylamine, make the mol ratio of triethylamine and gamma...

Embodiment 2

[0029] Step (1). Mix polyether polyol with an average molecular weight of 4000 and a functionality of 2 with triethylamine at a molar ratio of 1:2, and stir at 80°C for 0.5 hours in nitrogen to obtain a polyol with a functionality of 2. Active hydrogen compounds of ether polyols.

[0030] Step (2). Under the condition of continuous stirring, the active hydrogen compound of the polyether polyol with a functionality of 2 in the step (1) is added dropwise to the dioxane solvent whose concentration of phenyl dichlorophosphate is 1mol / L In the process, the molar ratio of phenyl dichlorophosphate to polyether polyol is 2.5:1, the time for dropping is 90 minutes, and the reaction is carried out at 80° C. for 10 hours;

[0031] Step (3). Add γ-aminopropyltriethoxysilane to the reaction solution, so that the molar ratio of γ-aminopropyltriethoxysilane and polyether polyol in the solution is 2.5:1, and then add three Ethylamine, making the mol ratio of triethylamine and γ-aminopropyltr...

Embodiment 3

[0035] Step (1). Mix the polyether polyamine with an average molecular weight of 1000 and a functionality of 2 with triethylamine at a molar ratio of 1:2, and stir at 50°C for 0.6 hours in a nitrogen atmosphere to obtain a polyether polyamine with a functionality of 2. Active hydrogen compounds of polyether polyamines.

[0036] Step (2). Under the condition of continuous stirring, the active hydrogen compound of the polyether polyamine with a functionality of 2 in the step (1) is added dropwise to the concentration of phenyl dichlorophosphate in the acetone solvent of 0.5mol / L, so that The molar ratio of phenyl dichlorophosphate to polyether polyamine is 2.3:1; the dropping time is 60 minutes, and the reaction is 7 hours at 50°C;

[0037] Step (3). Add γ-aminopropyltriethoxysilane to the reaction solution, so that the molar ratio of γ-aminopropyltriethoxysilane and polyether polyol in the solution is 2.3:1, and then add three Ethylamine, making the mol ratio of triethylamine ...

technical field

[0001] The invention belongs to the technical field of polymer materials, and relates to a flame retardant surface treatment agent and its preparation method and application, in particular to a silicon-containing flame-retardant polyether surface treatment for a solid inorganic flame retardant of flame-retardant polyurethane Agents and their preparation methods and applications. Background technique

[0002] Polyurethane foam is widely used in refrigeration, construction, automobile and other industrial fields due to its light weight, high strength, excellent electrical insulation and low thermal conductivity. However, the porous cellular structure of polyurethane foam increases its contact area with air, making it highly flammable. In recent years, there have been more and more reports of fires caused by polyurethane foam igniting, so it is very necessary for it to be flame retardant.

[0003] At present, the flame retardants used in polyurethane foam are ...

Examples

Embodiment 1

[0023] Step (1). Mix polyether polyol with an average molecular weight of 300 and a functionality of 2 with triethylamine at a molar ratio of 1:2, and stir at 40°C for 0.5 hour in a nitrogen atmosphere to obtain a polyether polyol with a functionality of 2. Active hydrogen compounds of polyether polyols;

[0024] Step (2). Under the condition of continuous stirring, the active hydrogen compound of the polyether polyol with a functionality of 2 in the step (1) is added dropwise to the tetrahydrofuran solvent whose concentration of phenyl dichlorophosphate is 0.1mol / L, Make the molar ratio of phenyl dichlorophosphate and polyether polyol in the solution to be 2.1:1, add dropwise for 30 minutes, and react at 40°C for 5 hours;

[0025] Step (3). Add γ-aminopropyltriethoxysilane to the reaction solution, so that the molar ratio of γ-aminopropyltriethoxysilane and polyether polyol in the solution is 2.1:1, and then add three Ethylamine, make the mol ratio of triethylamine and gamma...

Embodiment 2

[0029] Step (1). Mix polyether polyol with an average molecular weight of 4000 and a functionality of 2 with triethylamine at a molar ratio of 1:2, and stir at 80°C for 0.5 hours in nitrogen to obtain a polyol with a functionality of 2. Active hydrogen compounds of ether polyols.

[0030] Step (2). Under the condition of continuous stirring, the active hydrogen compound of the polyether polyol with a functionality of 2 in the step (1) is added dropwise to the dioxane solvent whose concentration of phenyl dichlorophosphate is 1mol / L In the process, the molar ratio of phenyl dichlorophosphate to polyether polyol is 2.5:1, the time for dropping is 90 minutes, and the reaction is carried out at 80° C. for 10 hours;

[0031] Step (3). Add γ-aminopropyltriethoxysilane to the reaction solution, so that the molar ratio of γ-aminopropyltriethoxysilane and polyether polyol in the solution is 2.5:1, and then add three Ethylamine, making the mol ratio of triethylamine and γ-aminopropyltr...

Embodiment 3

[0035] Step (1). Mix the polyether polyamine with an average molecular weight of 1000 and a functionality of 2 with triethylamine at a molar ratio of 1:2, and stir at 50°C for 0.6 hours in a nitrogen atmosphere to obtain a polyether polyamine with a functionality of 2. Active hydrogen compounds of polyether polyamines.

[0036] Step (2). Under the condition of continuous stirring, the active hydrogen compound of the polyether polyamine with a functionality of 2 in the step (1) is added dropwise to the concentration of phenyl dichlorophosphate in the acetone solvent of 0.5mol / L, so that The molar ratio of phenyl dichlorophosphate to polyether polyamine is 2.3:1; the dropping time is 60 minutes, and the reaction is 7 hours at 50°C;

[0037] Step (3). Add γ-aminopropyltriethoxysilane to the reaction solution, so that the molar ratio of γ-aminopropyltriethoxysilane and polyether polyol in the solution is 2.3:1, and then add three Ethylamine, making the mol ratio of triethylamine ...

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