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Phosphorus-silicon gel, method for inducing APP (ammonium polyphosphate) to decompose in advance to quickly form charcoal, and application of phosphorus-silicon gel in flame retardant polyurethane

A silicone gel and carbon-forming technology, applied in and inducing APP to decompose and rapidly form carbon, flame-retardant polyurethane, and phosphorus-silicon gel field, can solve problems such as the mismatch of decomposition temperature of polyurethane foam, and improve the resistance to Thermal properties, excellent flame retardant properties, and the effect of improving char formation

Active Publication Date: 2018-06-01
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In view of the deficiencies of ammonium polyphosphate itself and the problem that it does not match the decomposition temperature of polyurethane foam, the object of the present invention is to provide a phosphorus-silicon gel, a method for inducing APP to decompose in advance and quickly form charcoal, and its use in flame-retardant polyurethane. In the application of the present invention, the method of the present invention can improve the heat resistance and char formation of ammonium polyphosphate at high temperature while improving the dispersion of ammonium polyphosphate, and the decomposition of ammonium polyphosphate can be induced by phosphorus-silica gel. The temperature matches the decomposition temperature of polyurethane foam and applies it to flame-retardant polyurethane foam

Method used

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  • Phosphorus-silicon gel, method for inducing APP (ammonium polyphosphate) to decompose in advance to quickly form charcoal, and application of phosphorus-silicon gel in flame retardant polyurethane
  • Phosphorus-silicon gel, method for inducing APP (ammonium polyphosphate) to decompose in advance to quickly form charcoal, and application of phosphorus-silicon gel in flame retardant polyurethane
  • Phosphorus-silicon gel, method for inducing APP (ammonium polyphosphate) to decompose in advance to quickly form charcoal, and application of phosphorus-silicon gel in flame retardant polyurethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Step (1): 21.2g (0.096mol) KH550 and 9.7g (0.096mol) potassium bicarbonate were dissolved in 50ml THF solvent and slowly added dropwise to 24ml THF dissolved in 5.8g (0.016mol) diphenoxyphosphoryl chloride In the solvent, stir at 15°C to complete the dropwise addition process;

[0039] Step (2): after the dropwise addition, raise the temperature to 65°C, and continue stirring for 15 hours;

[0040] Step (3): After the reaction finishes, obtain phosphorus-silica gel through vacuum distillation;

[0041] Step (4): Add 10 g of phosphorus-silica gel to a mixed solution of 11 ml of water and 75 ml of absolute ethanol, and stir at 20° C. for 20 minutes to obtain a hydrolyzed phosphorus-silica gel;

[0042] Step (5): Slowly add the hydrolyzed phosphorus-silica gel obtained in step (4) dropwise into a mixture of 40 g of ammonium polyphosphate and tetrahydrofuran, and stir at 25° C. to complete the dropping process;

[0043]Step (6): placing the mixture obtained in step (5) in...

Embodiment 2

[0048] Step (1): Dissolve 11.49g (0.052mol) KH550 and 5.06g (0.05mol) triethylamine in 45ml tetrahydrofuran solvent and slowly add dropwise to 35ml tetrahydrofuran dissolved in 11.21g (0.0575mol) phenylphosphoryl dichloride In the solvent, stir at 0°C to complete the dropwise addition process;

[0049] Step (2): after the dropwise addition, raise the temperature to 40°C, and continue stirring for 4 hours;

[0050] Step (3): After the reaction finishes, obtain phosphorus-silica gel through vacuum distillation;

[0051] Step (4): Add 12 g of phosphorus-silica gel to a mixed solution of 11 ml of water and 88 ml of absolute ethanol, and stir at 10° C. for 15 minutes to obtain a hydrolyzed phosphorus-silica gel;

[0052] Step (5): Slowly add the hydrolyzed phosphorus-silica gel obtained in step (4) dropwise into a mixture of 40 g of ammonium polyphosphate and absolute ethanol, and stir at 40° C. to complete the dropping process;

[0053] Step (6): placing the mixture obtained in ...

Embodiment 3

[0058] Step (1): 25.4g (0.115mol) KH550 and 11.6g (0.115mol) triethylamine were dissolved in 50ml 1,4-dioxane solvent and slowly added dropwise to 24.26g (0.0115mol) dichloride In 50ml of 1,4-dioxane solvent of phenyl phosphate, stir at 25°C to complete the dropwise addition process;

[0059] Step (2): after the dropwise addition, raise the temperature to 30°C, and continue stirring for 6 hours;

[0060] Step (3): After the reaction finishes, obtain phosphorus-silica gel through vacuum distillation;

[0061] Step (4): Add 24g of phosphorus-silica gel to a mixed solution of 22ml of water and 110ml of absolute ethanol, and stir at 20°C for 25 minutes to obtain a hydrolyzed phosphorus-silica gel;

[0062] Step (5): Slowly add the hydrolyzed phosphorus-silica gel obtained in step (4) dropwise into a mixture of 40 g of ammonium polyphosphate and 1,4-dioxane, and stir at 20° C. to complete the dropping process;

[0063] Step (6): Put the mixture obtained in step (5) in a basket gr...

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Abstract

The invention discloses phosphorus-silicon gel, a method for inducing APP (ammonium polyphosphate) to decompose in advance to quickly form charcoal, and application of the phosphorus-silicon gel in flame retardant polyurethane. The method comprises the following steps: modifying a compound which has intrinsic flame retardant characteristics and contains P-Cl bonds by utilizing a silane coupling agent of which the terminal group is -NH2 so as to obtain the phosphorus-silicon gel; and after hydrolysis, putting the phosphorus-silicon gel together with a mixture of APP and a solvent into a baskettype grinder to be ground so as to obtain novel phosphorus-silicon gel coated APP. The invention also discloses application of the phosphorus-silicon gel in flame retardant polyurethane foam. A phosphorus-silicon gel surface conditioning agent obtained by the invention can effectively improve the heat resistance and the charcoal forming property of the APP at high temperature and can induce the APP to decompose in advance, and the decomposition temperature of the APP is matched with the decomposition temperature of the polyurethane foam. The phosphorus-silicon gel coated APP has good dispersibility and matrix compatibility. By applying the phosphorus-silicon gel coated APP to the polyurethane foam, the polyurethane foam is greatly improved in flame resistance and has certain mechanical properties.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a phosphorus-silicon gel, a method for inducing APP to decompose in advance and quickly form charcoal, and its application in flame-retardant polyurethane. Background technique [0002] As a typical additive flame retardant, ammonium polyphosphate has been widely used in polyurethane foam. However, during the application process, it was found that ammonium polyphosphate has the problems of easy moisture absorption, dispersibility and poor compatibility with the matrix. In addition, the initial decomposition temperature of ammonium polyphosphate is about 300°C, which is about 100°C higher than that of polyurethane foam. The mismatch of decomposition temperature will have a certain impact on the flame retardant effect of ammonium polyphosphate in polyurethane foam. At present, ammonium polyphosphate is used in domestic and foreign journals such as Polymer Degradation and...

Claims

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Application Information

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IPC IPC(8): C07F9/24C07F9/36C07F9/44C07F9/50C08K9/10C08L75/08C08K3/32
CPCC07F9/2458C07F9/36C07F9/4465C07F9/5022C07F9/505C08K3/32C08K9/10C08K2003/323C08L75/08
Inventor 陈雅君李琳珊钱立军
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY