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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 problem that modified polyurethane cannot obtain flame retardant properties, the flame retardancy has not been substantially changed, and cannot be used in the field of flame retardancy and other problems, to achieve the effect of being suitable for large-scale industrial production, low cost and high yield

Active Publication Date: 2013-05-15
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 concrete steps of preparation are:

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

[0022] Step 2, first mix polytetrahydrofuran ether glycol, modified clathrate silsesquioxane powder and N,N-dimethylformamide in a weight ratio of 98:15:250, and stir at 50°C 1h, a mixed solut...

Embodiment 2

[0025] The concrete steps of preparation are:

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

[0027] Step 2, first mix polytetrahydrofuran ether glycol, modified clathrate silsesquioxane powder and N,N-dimethylformamide in a weight ratio of 99:11:288, and stir at 53°C After 0.8h...

Embodiment 3

[0030] The concrete steps of preparation are:

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

[0032] Step 2, first mix polytetrahydrofuran ether glycol, modified clathrate silsesquioxane powder and N,N-dimethylformamide in a weight ratio of 100:8:325, and stir at 55°C 0.6h, a mixed so...

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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-cage silsesquioxane nanocomposite material. Background technique [0002] Cage-shaped silsesquioxane (POSS) is a new type of organic-inorganic nano-hybrid system. It is composed of inorganic Si-O as a cage-shaped skeleton. Attached organic groups surround the inner core. The inorganic siloxane skeleton endows the polymer matrix with good heat resistance and mechanical properties, and can also play a role in strengthening and toughening, while the peripheral organic groups can improve the compatibility between POSS and the polymer matrix. This unique property of POSS has made it the first-selected filling material for the preparation of high-performance polymer materials, such as the Chinese invention patent application CN 102617823 A published on August 1, 2012 "a modified hydroxycrate silsesqu...

Claims

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Application Information

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Patent Type & Authority Applications(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
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