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Phosphorus nitrogen flame retardant containing carbamate structure and preparation method thereof

A phosphorus-nitrogen-based flame retardant and urethane technology, which is applied in the field of phosphorus-nitrogen-based flame retardants containing urethane structure and their preparation, can solve the problem of poor compatibility of polyurethane, uneven distribution of flame retardants, The problem of unstable flame retardant effect, etc., achieves the effect of high phosphorus and nitrogen content, excellent compatibility, and excellent flame retardant effect.

Active Publication Date: 2015-09-09
HUAFON MICROFIBER SHANGHAI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the production process of domestic mainstream microfiber synthetic leather needs to be treated with high-temperature toluene for weight reduction and high-temperature water washing. At present, it is difficult for most phosphorus-nitrogen flame retardants to remain in microfiber synthetic leather after being treated under such conditions. On the other hand, the phosphorus nitrogen flame retardant has poor compatibility with the polyurethane used in the impregnation production process of the superfine fiber synthetic leather, which leads to the uneven distribution of the flame retardant in the superfine fiber synthetic leather, and finally makes the leather The flame retardant effect is unstable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The said phosphorus-containing triol: 215 grams of tris(dipropylene glycol) phosphite, catalyst: 1,3,5-tris(dimethylaminopropyl) hexahydrotriazine 0.2854 grams and solvent two Add 2853.8 grams of methylformamide into the reaction vessel. After stirring, add 250.26 grams of diisocyanate: diphenylmethane-4,4'-diisocyanate. The temperature is raised to 100°C and reacted at this temperature for 2 hours. Add phosphorus-containing monoalcohol: 105.5 grams of N-hydroxymethyl-3-(dimethoxyphosphonyl) propionamide, react for 30 minutes, then evaporate the solvent to dryness to obtain a white powder, which is phosphorus with carbamate structure Nitrogen flame retardant. When the polyurethane microfiber synthetic leather contains 30% (mass percentage) of the flame retardant, when the combustion test is performed according to the method provided by GB8410-2006, the burning speed of the polyurethane microfiber synthetic leather is 51mm / min, which is consistent with The flame retardan...

Embodiment 2

[0028] The diol containing phosphorus element: 150 g (N,N-bis(2-hydroxyethyl) diethyl aminomethyl phosphonate, the triol containing phosphorus element: 37.82 g trimethylol Phosphine oxide, catalyst: 8.81 grams of triethylamine and 400 grams of dioxane as a solvent are added to the reaction vessel. After stirring, add diisocyanate: 250.26 grams of diphenylmethane-4,4'-diisocyanate, and heat to 75 ℃, and react at this temperature for 1.5 hours, then add phosphorus-containing monohydric alcohol: 2.616 g of N-hydroxymethyl-3-(dimethoxyphosphonyl) propionamide, react for 20 minutes, then evaporate the solvent to obtain The white powder is the phosphorus-nitrogen flame retardant with urethane structure. When 30% (mass percentage) of the flame retardant is contained in the polyurethane microfiber synthetic leather, it is burned according to the method provided by GB8410-2006 During the test, the burning speed of polyurethane microfiber synthetic leather is 16mm / min, which meets the re...

Embodiment 3

[0030] The said phosphorus-containing diol: 291.66 g of bis(4-hydroxyphenyl) phenyl phosphine oxide, the phosphorus-containing triol: 8.4 g of trimethylol phosphine oxide, catalyst: cyclohexyl methyl 23.41 grams of tertiary amine and 23.41 grams of solvent propylene glycol methyl ether acetate were added to the reaction vessel. After stirring, add diisocyanate: 168.19 grams of 1,6-hexamethylene diisocyanate, and heat to 50°C, and react at this temperature for 0.5 hours After evaporating the solvent to dryness, a colorless and transparent liquid is obtained, which is a phosphorus-nitrogen flame retardant containing a carbamate structure. When the polyurethane microfiber synthetic leather contains 30% (mass percentage) of the flame retardant, the burning speed of the polyurethane microfiber synthetic leather is 63mm / min when the burning test is performed according to the method provided by GB 8410-2006. It meets the flame retardant performance requirements of automotive interior ...

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Abstract

The invention discloses a nitrogen-phosphorus flame retardant containing a carbamate structure and a preparation method of the flame retardant. The method comprises the following steps: stirring and mixing dihydric alcohol containing a phosphorus element, trihydric alcohol containing the phosphorus element, a catalyst and a solvent, and then adding diisocyanate to react; adding monohydric alcohol containing the phosphorus element to react; and drying the solvent by distillation, so as to obtain the nitrogen-phosphorus flame retardant containing the carbamate structure. The nitrogen-phosphorus flame retardant disclosed by the invention is an environment-friendly flame retardant which does not contain halogen or heavy metals, and is non-toxic; the synthetic process is simple and easy to control, high in nitrogen-phosphorus content, and good in flame retardant effect, has excellent compatibility with polyurethane, can be well dispersed into various polyurethane using systems, and simultaneously has a certain reticular structure, so that the nitrogen-phosphorus flame retardant is not dissolved into a toluene system. Thus, the nitrogen-phosphorus flame retardant can be applied to the field of flame-retardant superfine fiber synthetic leather requiring reducing production by methylbenzene.

Description

Technical field [0001] The invention relates to a phosphorus-nitrogen flame retardant and a preparation method thereof, in particular to a phosphorus-nitrogen flame retardant containing a carbamate structure and a preparation method thereof. Background technique [0002] The application of microfiber synthetic leather (abbreviated as: microfiber leather) in the field of automotive interiors includes leather for high-end automobile steering wheels, leather for high-end automobile seats, leather for high-end automobile door panels and leather for high-end automobile instrument panels. Market space. Flame retardant performance is a key feature of automotive interior products, and various OEMs list this performance as a mandatory performance requirement for automotive interior products. [0003] For the flame-retardant treatment of microfiber leather, the currently known domestic and foreign mainstream technology is the addition of flame retardants in and out of polyurethane to meet t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/38C08G18/32C08G18/20C08G18/18C08L75/04
CPCC08G18/288C08G18/388C08G18/3887C08G18/3889D06M15/579D06M2200/30
Inventor 吴勇王贺玲孙向浩诸葛磊韩芹刘国
Owner HUAFON MICROFIBER SHANGHAI
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