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Preparation method for expansion type melamine hypophosphite fire retardant

A technology of melamine hypophosphite and melamine, applied in the direction of organic chemistry and the like, can solve the problems of flame retardant effect, many reaction by-products, complicated reaction process, etc., and achieves good compatibility, simple waste water recycling, and simple preparation method. Effect

Inactive Publication Date: 2009-11-04
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, most of the existing phosphorus-based flame retardants have the disadvantages of complex reaction process, many by-products or low yield without industrial production value.
CN 1396924A describes the synthesis reaction of condensation products of melamine and phosphate-containing salts, the reaction temperature is 250-400°C, and there are many reaction by-products, which may affect the flame retardant effect
CN 1721423A describes the synthesis method of pentaerythritol diphosphate melamine salt, the synthesis of the intermediate product pentaerythritol phosphate needs to react for 7-10 hours, the reaction time is too long, and the solvent is benzene, which has a great impact on the environment

Method used

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  • Preparation method for expansion type melamine hypophosphite fire retardant

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Get 126g of melamine (1mol) and 132g of hypophosphorous acid (1mol) with a concentration of 50%, add hypophosphorous acid and 1L of water into a 2000ml beaker, place in a water bath at 25°C, stir with a constant speed electric stirrer at a speed of 300r / min , Add melamine in batches and react for 2 hours. The reaction product was suction-filtered, washed with an appropriate amount of water, dried in a vacuum oven at 150° C. for 3 hours, weighed and the yield of melamine hypophosphite MHP was 170.1 g, and the reaction yield was 88.54%. The expected reaction product structure is:

[0016]

[0017] Elemental analysis (%): the main element N is 43.38 (43.75), P is 16.09 (16.15), the theoretical content is in brackets, and the structure of the synthesized product has been confirmed by infrared spectrum analysis.

Embodiment 2

[0019] Get 126g of melamine (1mol) and 132g of hypophosphorous acid (1mol) with a concentration of 50%, add hypophosphorous acid and 1L of water into a 2000ml beaker, place in a 50°C water bath, stir with a constant speed electric stirrer at a speed of 300r / min , Add melamine in batches and react for 2 hours. The reaction product was suction-filtered, washed with an appropriate amount of water, dried in a vacuum oven at 150° C. for 3 hours, weighed and the yield of melamine hypophosphite MHP was 164.9 g, and the reaction yield was 85.93%.

Embodiment 3

[0021] Get 126g of melamine (1mol) and 264g of hypophosphorous acid (2mol) with a concentration of 50%. Add hypophosphorous acid and 1L of water into a 2000ml beaker, place in a water bath at 25°C, and stir with a constant speed electric stirrer at a speed of 300r / min , Add melamine in batches and react for 2 hours. The reaction product was suction-filtered, washed with an appropriate amount of water, dried in a vacuum oven at 150° C. for 3 hours, weighed and the yield of melamine hypophosphite MHP was 213.6 g, and the reaction yield was 82.79%.

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Abstract

The invention relates to a preparation method for an expansion type melamine hypophosphite fire retardant. The preparation method comprises the following steps: adopting a water phase synthesis method, adding melamine and hypophosphorous acid with the molar ratio of 1:0.5 to 3 into water, stirring the mixture for reaction for 2 hours at 0 to 100 DEG C at a stirring speed of 300r / min, then carrying out the suction filtration and washing of the reaction product, and drying the reaction product for 3 hours at 150 DEG C to obtain the melamine hypophosphite fire retardant. The preparation method has simplicity, quickness, high efficiency, no halogen, environmental friendliness, low cost and high economic benefits. In addition, the prepared fire retardant has high phosphorus content, is a solid at room temperature, and has high thermal stability and high compatibility with high polymers. The fire retardant not only can be used for a polyolefin halogen-free fire retardation system, but also can be used for the halogen-free fire retardation of engineering plastics such as polyester, polyamide, and the like.

Description

technical field [0001] The invention belongs to the field of preparation of intumescent flame retardants, in particular to a preparation method of intumescent melamine hypophosphite flame retardants. Background technique [0002] Since the 1980s, flame retardants have become the largest additives used in synthetic materials next to plasticizers. With the development of the economy, people's awareness of environmental protection and safety has greatly improved, and they are more concerned about the ecological environment and the value of life. Traditional halogenated flame retardants are widely used in the production of flame retardant materials due to their high flame retardant efficiency. However, due to the combustion of halogen-based flame-retardant products, a large amount of smoke and toxic corrosive gases are produced, which hinders rescue and evacuation of personnel, resulting in secondary disasters. Therefore, the application of halogen flame retardant products is ...

Claims

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Application Information

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IPC IPC(8): C07D251/54C09K21/12C09K21/10C08K5/3492
Inventor 彭治汉陈晓锋
Owner DONGHUA UNIV
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