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Cross-linked type insoluble halogen-free flame retardant and preparation method and application thereof

A flame retardant, cross-linked technology, used in the field of halogen-free flame retardants, cross-linked insoluble halogen-free flame retardants

Active Publication Date: 2016-01-06
烟台蓝海博隆超纤新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In the flame retardant synthetic leather manufacturing industry, flame retardants are required to have high flame retardant efficiency and are completely insoluble in hot water, hot toluene, and dimethylformamide. At present, there is no flame retardant that can fully meet the requirements.

Method used

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  • Cross-linked type insoluble halogen-free flame retardant and preparation method and application thereof
  • Cross-linked type insoluble halogen-free flame retardant and preparation method and application thereof
  • Cross-linked type insoluble halogen-free flame retardant and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 216g (0.4mol) 75% solid content tetrakis hydroxymethyl phosphorus sulfate aqueous solution, 78g (1.3mol) urea, 25.2g (0.2mol) melamine, 2.2g hexamethylenetetramine in the bottle mouth detachable flask Mix with 110g of water, stir and heat up to 60°C. After reacting for 60 minutes, add 4.4g of aminopropyl triethoxysiloxane. After heating up to 95°C for 10 minutes, the viscosity of the reactant gradually increases, and gradually fades from milky white. After continuing to stir and react for 2 minutes, a viscous transparent substance was formed, and the viscosity increased rapidly to form a transparent brittle gel. Take out the gel, dry it in a blast drying oven at 120°C for 4 hours, take out the dried white lump, grind it in a grinder to a size above 300 mesh, and obtain a cross-linked insoluble halogen-free flame retardant.

Embodiment 2

[0024] Add 216g (0.4mol) 75% solid content tetrakis hydroxymethyl phosphorus sulfate aqueous solution, 60g (1mol) urea, 37.8g (0.45mol) dicyandiamide, 12.6g (0.1mol) melamine in the detachable flask of bottle mouth , 4g hexamethylenetetramine and 160g water, stir and heat up to 70°C, react for 40min, add 6g of aminopropyltrimethoxysiloxane, heat up to 95°C and react for 10min, the viscosity of the reactant gradually increases, From milky white to light gradually, after continuing to stir and react for 2 minutes, a viscous transparent substance was formed, and the viscosity increased rapidly to form a transparent brittle gel. Take out the gel, dry it in a blast drying oven at 120°C for 4 hours, take out the dried white lump, grind it in a grinder to a size above 300 mesh, and obtain a cross-linked insoluble halogen-free flame retardant.

Embodiment 3

[0026] Add 216g of 75% solid content tetrakis hydroxymethyl phosphorus sulfate aqueous solution, 60g of urea, 50.4g of melamine, 6.48g of hexamethylenetetramine and 216g of water into a flask with a detachable neck, stir and raise the temperature to 70°C, and react for 60min Finally, add 10.8g of aminopropyl trimethoxysiloxane, heat up to 95°C and react for 15 minutes, the viscosity of the reactant gradually increases, and gradually fades from milky white. After continuing to stir and react for 2 minutes, a viscous transparent substance is formed, and the viscosity increases rapidly. Large transparent brittle gels are formed. Take out the gel, dry it in a blast drying oven at 100°C for 6 hours, take out the dried white lump, grind it in a grinder to a size above 300 mesh, and obtain a cross-linked insoluble halogen-free flame retardant.

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Abstract

The invention discloses a cross-linked type insoluble halogen-free flame retardant and a preparation method and application thereof, and belongs to the technical field of flame retardants. The flame retardant is a cross-linked polymer formed when a methylol group of tetrakis hydroxymethyl phosphonium sulfate, difunctional amine compounds with amido groups and trifunctional melamine react under the effect of a catalyst hexamethylenetetramine, wherein the phosphorus content is larger than or equal to 10%, the nitrogen content is larger than or equal to 25%, the decomposition temperature is larger than or equal to 300 DEG C, solubility in water at the temperature of 25 DEG C is smaller than 0.01 g per 100 ml, the weight loss rate is smaller than 0.05 g per 100 ml after hot water at the temperature of 100 DEG C is boiled for 2 hours, and the flame retardant is not dissolved in conventional solvent such as ethyl alcohol, acetone, methylbenzene, petroleum ether and ethyl acetate at a temperature within the boiling point range. The flame retardant is used for superfine fiber synthetic leather and textile polyurethane coatings; the horizontal burning rate of the flame retardant is far lower than the flame retardance requirement of superfine fiber synthetic leather in the industry for the horizontal burning rate of smaller than 10 cm / min.

Description

technical field [0001] The invention relates to a halogen-free flame retardant, in particular to a cross-linked insoluble halogen-free flame retardant, a preparation method of the flame retardant, and its application in the fields of superfine fiber synthetic leather and textile polyurethane coating . The invention belongs to the technical field of flame retardants. Background technique [0002] Flame retardants are indispensable additives in the processing and production of polymer products, textiles, building materials and other products. Since the research on flame retardants in the middle of last century, halogen flame retardants mainly containing bromine have been widely used because of their high flame retardant efficiency and low price. Since 1986, the toxicity and environmental issues of polybrominated diphenyl ether flame retardants have been debated in the field of flame retardants. Restriction and banning of halogen flame retardants have become an international ...

Claims

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Application Information

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IPC IPC(8): C08G73/06C08L75/04C08L79/04D06N3/14
Inventor 卢丽燕
Owner 烟台蓝海博隆超纤新材料有限公司
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