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Phosphoric acid-modified nano beta molecular sieve-ammonium polyphosphate composite flame retardant and preparation method thereof

A technology of composite flame retardant and β molecular sieve, which is applied in the field of halogen-free flame retardants, can solve the problems of serious hazards, low flame retardant effect, and limited application, and achieve good flame retardant performance, smoke suppression performance, and excellent toughening , Good dispersion and compatibility

Active Publication Date: 2014-08-13
慧科高新科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The biggest disadvantage of halogenated flame retardants is that the price is high, and the second is that carcinogens such as dioxin are released during combustion. High molecular polymers containing halogenated flame retardants will produce a large amount of toxic and corrosive gases when burned. Such as smog, it is easy to suffocate people, and its harm is more serious than the fire itself, which greatly limits its application
The flame retardant effect of simply using ammonium polyphosphate is still low, and further improvement of the process or compounding is required

Method used

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  • Phosphoric acid-modified nano beta molecular sieve-ammonium polyphosphate composite flame retardant and preparation method thereof
  • Phosphoric acid-modified nano beta molecular sieve-ammonium polyphosphate composite flame retardant and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Weigh 4kg of nano-beta molecular sieve with a particle size of 90nm, add 20L of phosphoric acid aqueous solution with a concentration of 0.5mol / L, put it in an ultrasonic oscillator for 8 minutes, heat and reflux and stir for 25 minutes, filter, and put the filter residue in an oven to dry at 100°C Dry it, put it into a muffle furnace and bake it at 400°C for 3 hours, and then pulverize it to obtain phosphoric acid-modified nano-β molecular sieve.

[0019] First, add 70L of concentrated phosphoric acid with a concentration of 80% into a reaction kettle with a volume of 1000L, heat to 95°C, slowly add 90kg of urea under stirring, heat up to 130°C after the urea dissolves, then add 20kg of phosphoric acid modified nano-β molecular sieve, and stir After 8 minutes, the temperature was raised to 170°C for pre-polymerization, and the temperature was kept until the reactant was viscous, then transferred to an oven at 250°C for further polymerization reaction for 30 minutes, the...

Embodiment 2

[0021] Weigh 5kg of nano-beta molecular sieve with a particle size of 100nm, add 20L of phosphoric acid aqueous solution with a concentration of 0.9mol / L, put it in an ultrasonic oscillator for 10 minutes, heat and reflux and stir for 28 minutes, filter, and put the filter residue in an oven for drying at 105°C Dry it, put it into a muffle furnace and bake it at 450°C for 3.5 hours, and then pulverize it to obtain phosphoric acid-modified nano-β molecular sieve.

[0022] Add 50L of concentrated phosphoric acid with a concentration of 85% into a reactor with a volume of 1000L, heat to 85°C, slowly add 80kg of urea under stirring, heat up to 120°C after the urea dissolves, then add 10kg of phosphoric acid-modified nano-β molecular sieve, and stir for 10 minutes Finally, heat up to 150°C for pre-polymerization, keep warm until the reactants are viscous, transfer to an oven at 220°C for further polymerization for 20 minutes, discharge the material, cool and pulverize, sieve, and pa...

Embodiment 3

[0024] Weigh 6kg of nano-beta molecular sieve with a particle size of 120nm, add 20L of phosphoric acid aqueous solution with a concentration of 1.0mol / L, put it in an ultrasonic oscillator for 12min, heat and reflux and stir for 35min, filter, and put the filter residue in an oven for drying at 120°C Dry it, put it into a muffle furnace and bake it at 500°C for 4 hours, and then pulverize it to obtain phosphoric acid-modified nano-β molecular sieve.

[0025] Add 60L of concentrated phosphoric acid with a concentration of 82% into a reactor with a volume of 1000L, heat to 90°C, slowly add 85kg of urea under stirring, heat up to 125°C after the urea dissolves, then add 15kg of phosphoric acid modified nano-β molecular sieve, and stir for 12min Finally, the temperature was raised to 160°C for pre-polymerization, and the temperature was kept until the reactants were viscous, then transferred to an oven at 230°C for further polymerization for 25 minutes, the discharged material was...

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Abstract

The invention belongs to the technical field of halogen-free flame retardants and particularly relates to a phosphoric acid-modified nano beta molecular sieve-ammonium polyphosphate composite flame retardant and a preparation method thereof. The preparation method comprises the following steps: first, adding strong phosphoric acid into a reaction kettle; heating to 85-95 DEG C; adding urea while stirring; after urea is dissolved, heating to 120-130 DEG C; then, adding the phosphoric acid-modified nano beta molecular sieve; after stirring for 8-12 minutes, heating to 150-170 DEG C for prepolymerization; insulating heat till the reactants get thick, transferring to a drying oven for further carrying out polymerization reaction for 20-30 minutes at 220-250 DEG C; discharging, cooling and smashing; and sieving and packaging. Used in a high molecular material such as polyethylene, the phosphoric-acid modified nano beta molecular sieve-ammonium polyphosphate composite flame retardant prepared by the invention has the excellent characteristics of good dispersibility and compatibility, excellent flame retardant performance and smoke suppression performance and the like and meanwhile further has excellent polymer toughening and enhancing performance. The preparation method is pollution-free and low in energy consumption.

Description

technical field [0001] The invention belongs to the technical field of halogen-free flame retardants, and in particular relates to a phosphoric acid-modified nano-beta molecular sieve-ammonium polyphosphate composite flame retardant and a preparation method thereof. Background technique [0002] At present, more and more polymer materials are used in indoor and outdoor decoration and industrial production. Most of the commonly used polymer materials are flammable, such as the commonly used thermal insulation material polystyrene. Therefore, the development of flame retardants for polymer materials is of great significance. [0003] Conventional flame retardants can be divided into halogenated flame retardants and halogen-free flame retardants. Halogenated flame retardants have the advantages of good flame retardant effect, good dispersibility and compatibility with polymer materials, easy processing, and no frosting. The representative products are polybrominated diphenyl e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/02C08K7/26C08K3/32C08L23/06
Inventor 李德刚唐守余
Owner 慧科高新科技股份有限公司
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