Preparation method of aluminum hypophosphite

A technology of aluminum hypophosphite and sodium hypophosphite, applied in the direction of hypophosphorous acid, phosphorus oxyacid, etc., can solve the problems of environmental and water pollution, high sodium chloride content, affecting flame retardant performance, etc., to achieve less pollution and high purity , the effect of short response time

Inactive Publication Date: 2015-08-26
WUHAN UNIV OF TECH
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  • Claims
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AI Technical Summary

Problems solved by technology

However, the acid-base neutralization method uses hypophosphorous acid as a reactant, and inhalation of hypophosphorous acid vapor or mist is more harmful to the human body, and at the same time has greater pollution to the environment and water bodies.
In addition, when water is used as a solvent to prepare aluminum hypophosphite products, the by-product sodium chloride content is high, which affects its flame retardant performance

Method used

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

Examples

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Comparison scheme
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Embodiment 1

[0019] A method for preparing aluminum hypophosphite, the steps are as follows:

[0020] 1) Add sodium hypophosphite (analytically pure, purity greater than 99wt%) and deionized water into a four-neck flask equipped with an electric stirrer, a condenser, and a thermometer, and heat at 50°C for 1 hour, stir until completely dissolved, and prepare Concentration is the aqueous solution of sodium hypophosphite of 6mol / L;

[0021] 2) dissolving the aluminum chloride powder in ethanol, after the aluminum chloride is dissolved and exothermic, a concentration of 0.5mol / L aluminum chloride ethanol solution can be obtained at room temperature;

[0022] 3) First heat the aqueous solution of sodium hypophosphite obtained in step 1) to 90° C., then slowly add the ethanol solution of aluminum chloride prepared in step 2) into the aqueous solution of sodium hypophosphite through a constant-pressure dropping funnel, while continuously stirring, Control the addition rate at 35-45 drops / min, k...

Embodiment 2

[0024] A method for preparing aluminum hypophosphite, the steps are as follows:

[0025] 1) Add sodium hypophosphite and deionized water into a four-necked flask equipped with an electric stirrer, a condenser, and a thermometer, and heat at 50°C for 0.5h, stir until completely dissolved, and prepare hypophosphorous acid with a concentration of 6mol / L Aqueous solution of sodium;

[0026] 2) Dissolving the aluminum chloride powder in ethanol, after the aluminum chloride is dissolved and exothermic, at room temperature, the ethanol solution of aluminum chloride with a concentration of 1mol / L can be obtained;

[0027] 3) First heat the aqueous solution of sodium hypophosphite obtained in step 1) to 90° C., then slowly add the ethanol solution of aluminum chloride prepared in step 2) into the aqueous solution of sodium hypophosphite through a constant-pressure dropping funnel, while continuously stirring, Control the addition rate at 35-45 drops / minute, keep the reaction temperatu...

Embodiment 3

[0029] A method for preparing aluminum hypophosphite, the steps are as follows:

[0030] 1) Add sodium hypophosphite and deionized water into a four-necked flask equipped with an electric stirrer, a condenser, and a thermometer, and heat at 60°C for 0.5h, stir until completely dissolved, and prepare hypophosphorous acid with a concentration of 2mol / L Aqueous solution of sodium;

[0031] 2) Aluminum chloride powder is dissolved in ethanol, after the aluminum chloride is dissolved and exothermic, a concentration of 0.5mol / L aluminum chloride ethanol solution can be obtained at room temperature;

[0032] 3) First heat the aqueous solution of sodium hypophosphite obtained in step 1) to 90° C., then slowly add the ethanol solution of aluminum chloride prepared in step 2) into the aqueous solution of sodium hypophosphite through a constant-pressure dropping funnel, while continuously stirring, Control the addition rate at 35-45 drops / minute, keep the reaction temperature at about 9...

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Abstract

The invention relates to a preparation method of aluminum hypophosphite. The method comprises the following steps: firstly, preparing a water solution of sodium hypophosphite; secondly, preparing an ethanol solution of aluminum chloride; thirdly, preparing aluminum hypophosphite: firstly heating the water solution of sodium hypophosphite to be 80-90 DEG C, then slowly adding the ethanol solution of aluminum chloride into the water solution of sodium hypophosphite, enabling the molar ratio of sodium hypophosphite to aluminum chloride to be (4-12):1, then performing heating reflux reaction, and treating reaction liquid after the reaction, so as to obtain the aluminum hypophosphite. The method has the advantages that ethyl alcohol serves as the solvent of aluminum chloride, the synthesis technology is simple, the requirement on reaction equipment is low, products obtained hardly contain hazardous substance sodium chloride residue, and the flame retardant property of the aluminum hypophosphite is good.

Description

technical field [0001] The invention belongs to the technical field of flame retardant preparation, and in particular relates to a method for preparing aluminum hypophosphite. Background technique [0002] Aluminum hypophosphite has a high phosphorus content, and has the advantages of good thermal stability, good hydrolytic stability, and high flame retardant effect. Because it does not contain P-O-C bonds of phosphate esters, it has good hydrolytic stability, does not cause polymer decomposition during processing, and does not affect plastic molding compositions. It can be applied to modified plastics such as PP, PA6, and PBT. flame retardant effect. The use of condensed phase flame retardant method can catalyze the carbonization of the body substances, and the synergistic use with other flame retardants can complement each other's advantages and enhance the flame retardant performance. It is a highly efficient synergistic flame retardant. When aluminum hypophosphite is a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/165
Inventor 高山俊戈年号续云昊沈春晖
Owner WUHAN UNIV OF TECH
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