Preparation method of spherical aluminum hypophosphite

A technology of aluminum hypophosphite and sodium hypophosphite, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as the decline of mechanical properties, reduce the decline of mechanical properties, improve the flame retardant effect, and crystal form regular effect

Active Publication Date: 2014-03-05
JINAN TAIXING FINE CHEM
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Problems solved by technology

[0004] The purpose of the present invention is to overcome the problems of the particle size and crystal form of the above-mentioned aluminum hypophosphite, and provide a method for preparing spherical aluminum hypophosphite, so that the particle size of the synthesized aluminum hypophosphite can reach about 7 microns, and the crystal form is spherical. It avoids problems such as the decline of mechanical properties caused by large particle size and irregular crystal form. At the same time, the addition of seed crystals makes it a phosphorus-nitrogen flame retardant system, which improves the flame retardant effect.

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  • Preparation method of spherical aluminum hypophosphite
  • Preparation method of spherical aluminum hypophosphite
  • Preparation method of spherical aluminum hypophosphite

Examples

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Embodiment 1

[0019] Formula (parts by weight): sodium hypophosphite 90, aluminum sulfate octadecahydrate 110, water 200, melamine cyanurate 5, polyacrylamide 2.5.

[0020] Preparation method: Weigh the raw materials according to the above-mentioned parts by weight, first add water as a solvent into the reaction vessel, start stirring, add aluminum sulfate octadecahydrate and melamine cyanurate into the reaction kettle, add polyacrylamide at the same time, stir evenly and heat up to 60 °C. After ℃, sodium hypophosphite was added, and the temperature was raised to 80 ℃ with stirring, and then the temperature was maintained, and the stirring reaction was continued for 4 hours to generate aluminum hypophosphite slurry. The aluminum hypophosphite slurry is filtered, dried and pulverized to obtain spherical aluminum hypophosphite with a particle size of 3.8 microns. The electron microscope photos of this example are shown in figure 1 .

Embodiment 2

[0022] Formula (parts by weight): 100 sodium hypophosphite, 120 aluminum sulfate octadecahydrate, 250 water, 30 melamine cyanurate, 1.8 sodium dodecylbenzenesulfonate.

[0023] Preparation method: weigh the raw materials according to the above-mentioned parts by weight, firstly add water into the reaction vessel as a solvent, start stirring, add aluminum sulfate octadecahydrate and melamine cyanurate into the reaction kettle, and add sodium dodecylbenzenesulfonate simultaneously, After stirring, the temperature was raised to 65°C, sodium hypophosphite was added, and the temperature was raised to 90°C after stirring, and then the temperature was maintained. The aluminum hypophosphite slurry was filtered, dried and pulverized to obtain spherical aluminum hypophosphite with a particle size of 4.7 microns. The electron microscope photos of this example are shown in figure 2 .

Embodiment 3

[0025] Formulation (parts by weight): 105 sodium hypophosphite, 100 aluminum sulfate octadecahydrate, 230 water, 40 melamine cyanurate, 2 citric acid.

[0026] Preparation method: weigh the raw materials according to the above weight parts, firstly add water as a solvent into the reaction vessel, start stirring, add aluminum sulfate octadecahydrate and melamine cyanurate into the reaction kettle, add citric acid at the same time, stir evenly and heat up to 75 ℃ Then, sodium hypophosphite was added, and the temperature was raised to 95 °C with stirring, and then the temperature was kept warm, and the reaction was continued for 5 h to generate aluminum hypophosphite slurry. The aluminum hypophosphite slurry was filtered, dried and pulverized to obtain spherical aluminum hypophosphite with a particle size of 5.4 microns. The electron microscope photos of this example are shown in image 3 .

[0027] Comparative example (traditional preparation process)

[0028] First, ad...

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Abstract

The invention discloses a preparation method of spherical aluminum hypophosphite. In the method disclosed by the invention, sodium hypophosphite reacts with aluminum sulfate; meanwhile, melamine cyanurate is added as a seed crystal in the earlier stage of reaction, and different dispersants are added to improve the dispersion effect. The spherical aluminum hypophosphite prepared by the method disclosed by the invention has the characteristics of small particle size, regular crystal form and the like, thus the drop of mechanical properties of plastics after the addition of a flame retardant is reduced. Meanwhile, by adopting the melamine cyanurate seed crystal as a synergist in the flame retardant, the flame retardance effect of aluminum hypophosphite after plastic addition is remarkably improved.

Description

technical field [0001] This product relates to a preparation method of a flame retardant, especially a preparation method of spherical aluminum hypophosphite. Background technique [0002] Aluminum hypophosphite is a phosphorus-containing flame retardant, which has the advantages of good thermal stability, low water solubility and good flame retardant effect. When used in engineering plastics such as PA6 and PBT, the heat release rate and the heat generated during combustion are sharply reduced , the amount of char after combustion increases, and the flame retardant performance reaches the UL94 standard V-0 level. [0003] The synthesis of aluminum hypophosphite is relatively mature now. Patent 201210302490.1 discloses a preparation scheme for synthesizing aluminum hypophosphite using sodium hypophosphite and aluminum sulfate, but the aluminum hypophosphite prepared by this experimental scheme has disadvantages such as large particle size and irregular crystal form. have a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/36C09K21/04
Inventor 张旭毕燕杜庆田孙晓丽
Owner JINAN TAIXING FINE CHEM
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