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Preparation method of halogen-free flame retardant polyurethane-cage type silsesquioxane nanocomposite

A technology of nanocomposite materials and silsesquioxane, which is applied in the field of preparation of nanocomposite materials, can solve the problems of cumbersome preparation methods, no substantial change in flame retardancy, and inability to be used in the field of flame retardancy, so as to reduce the Burning speed, effect of improving flame retardancy

Active Publication Date: 2014-06-25
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this preparation method has shortcomings. First, the flame retardancy of the product has not been substantially changed compared with pure polyurethane, so it cannot be used in the field of flame retardancy; second, the preparation method is not only cumbersome, but also cannot obtain Modified polyurethane with flame retardant properties

Method used

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  • Preparation method of halogen-free flame retardant polyurethane-cage type silsesquioxane nanocomposite
  • Preparation method of halogen-free flame retardant polyurethane-cage type silsesquioxane nanocomposite

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The specific steps of preparation are:

[0021] Step 1: First, add diphenylmethane diisocyanate to the nano-clathrate silsesquioxane N,N-dimethylformamide solution with a concentration of 10%, and stir at 70 ° C for 12 hours; The weight ratio of methane diisocyanate to nano-clathrate silsesquioxane in N,N-dimethylformamide solution is 1:11, and the particle size of nano-clathrate silsesquioxane is 1:11. The diameter is 1 nm, which is a nano-phenyl clathrate silsesquioxane, and a modified clathrate silsesquioxane solution is obtained. The modified clathrate silsesquioxane solution was then dried at 70°C, and after the solvent N,N-dimethylformamide was volatilized, it was ground and passed through a 1000-mesh sieve to obtain a modified clathrate silsesquioxane. Semisiloxane powder.

[0022] Step 2, firstly mix the polytetrahydrofuran ether diol, modified clathrate silsesquioxane powder and N,N-dimethylformamide according to the weight ratio of 98:15:250, and stir at 50°...

Embodiment 2

[0025] The specific steps of preparation are:

[0026] Step 1, firstly add diphenylmethane diisocyanate to the nano-clathrate silsesquioxane N,N-dimethylformamide solution with a concentration of 13%, and stir at 75 ° C for 11 hours; The weight ratio of methane diisocyanate and nano-clathrate silsesquioxane in N,N-dimethylformamide solution is 2:10.5. The diameter is 1 nm, which is a nano-phenyl clathrate silsesquioxane, and a modified clathrate silsesquioxane solution is obtained. The modified clathrate silsesquioxane solution was then dried at 75°C, and after the solvent N,N-dimethylformamide was volatilized, it was ground and passed through a 1000-mesh sieve to obtain the modified clathrate silsesquioxane. Semisiloxane powder.

[0027] Step 2, firstly mix the polytetrahydrofuran ether diol, modified clathrate silsesquioxane powder and N,N-dimethylformamide according to the weight ratio of 99:11:288, and stir at 53°C 0.8h, a mixed solution was obtained. Then, diphenylmet...

Embodiment 3

[0030] The specific steps of preparation are:

[0031]Step 1: First, add diphenylmethane diisocyanate to the nano-clathrate silsesquioxane N,N-dimethylformamide solution with a concentration of 15%, and stir at 80 ° C for 10 h; The weight ratio of methane diisocyanate and nano-clathrate silsesquioxane in N,N-dimethylformamide solution is 3:10. The diameter is 1.5 nm, which is nano-phenyl clathrate silsesquioxane, and a modified clathrate silsesquioxane solution is obtained. The modified clathrate silsesquioxane solution was then dried at 80°C, and after the solvent N,N-dimethylformamide was volatilized, it was ground and passed through a 1000-mesh sieve to obtain the modified clathrate silsesquioxane. Semisiloxane powder.

[0032] Step 2, firstly mix the polytetrahydrofuran ether diol, modified clathrate silsesquioxane powder and N,N-dimethylformamide according to the weight ratio of 100:8:325, and stir at 55°C 0.6h to obtain a mixed solution. Then add diphenylmethane diis...

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Abstract

The invention discloses a preparation method of a halogen-free flame retardant polyurethane-cage type silsesquioxane nanocomposite. The method comprises the following steps: first adding Diphenyl-methane-diisocyanate into a nano cage type silsesquioxane N,N-diphenyl methane diisocyanate solution, and stirring to obtain a modified cage type silsesquioxane solution; then drying the solution and grinding to obtain a modified cage type silsesquioxane powder; then mixing and stirring polyoxytertramethylene glycol, the modified silsesquioxane powder and N, N-diphenyl methane diisocyanate to obtain a mixed solution; and then dropwise adding Diphenyl-methane-diisocyanate into the mixed solution to obtain a modified mixed solution; then adding 1, 4-butanediol into the modified mixed solution for reaction to obtain a reaction liquid; and then placing the reaction liquid in a container, drying and curing at 50-60 DEG C for 10-20 h to prepare the halogen-free flame retardant polyurethane-cage type silsesquioxane nanocomposite. The composite material has excellent halogen-free flame retardant performance, and can be widely used in the fields of artificial leather and cable sheath.

Description

technical field [0001] The invention relates to a preparation method of a nanocomposite material, in particular to a preparation method of a halogen-free flame retardant polyurethane-clathrate silsesquioxane nanocomposite material. Background technique [0002] Cage silsesquioxane (POSS) is a new type of organic-inorganic nano-hybrid system. It is composed of inorganic Si-O to form a cage-shaped skeleton with a three-dimensional size of about 1-2 nm. Linked organic groups surround the core. The inorganic silicon-oxygen skeleton endows the polymer matrix with good heat resistance and mechanical properties, and can also enhance and toughen. The peripheral organic groups can improve the compatibility of POSS with the polymer matrix. This unique property of POSS has made it the preferred filling material for the preparation of high-performance polymer materials. Preparation method of polyurethane". The preparation method disclosed in the patent application document of the inv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/77C08G18/76C08G18/66C08G18/48C08G18/32
Inventor 张献薛萌陈洪莲田兴友包超郑康
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI