Preparation method for nanometer aluminum hypophosphite

A technology of aluminum hypophosphite and sodium hypophosphite, which is applied in the direction of hypophosphorous acid, nanotechnology, phosphorus oxyacid, etc., to achieve the effect of improving yield and dimensional stability

Inactive Publication Date: 2017-11-10
HUNAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The process methods disclosed in these patent documents have greatly promoted the preparation and process optimization of aluminum hypophosphite, but there a

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 100ml of an aqueous solution containing 10.6g of sodium hypophosphite to 100ml of benzene, add 13g of cetyltrimethylammonium bromide, and stir evenly to prepare a water-in-oil microemulsion, called A liquid; ml of an aqueous solution containing 4.6g of aluminum chloride, add 13g of cetyltrimethylammonium bromide, and stir evenly to prepare a water-in-oil microemulsion, called B liquid; in a water bath at 90°C, put B liquid in Stir at a speed of 30 rpm and slowly drop into liquid A, adjust the pH value of the system between 5-7, and obtain a milky white colloid of aluminum hypophosphite, evaporate the colloid to dryness with a rotary evaporator, and obtain a uniform and stable white Nano aluminum hypophosphite powder.

Embodiment 2

[0028] Add 100ml of an aqueous solution containing 10.6g of sodium hypophosphite to 100ml of toluene, add 13g of cetyltrimethylammonium bromide, and stir well to prepare a water-in-oil microemulsion, called A liquid; add 100ml of Add 13g of cetyltrimethylammonium bromide to an aqueous solution containing 4.6g of aluminum chloride, and stir evenly to prepare a water-in-oil microemulsion, which is called liquid B; Slowly drop into liquid A under the action of stirring, adjust the pH value of the system between 5-7, and obtain a milky white colloid of aluminum hypophosphite, evaporate the colloid to dryness with a rotary evaporator, and obtain uniform and stable white nano-aluminum hypophosphite powder .

Embodiment 3

[0030] Add 200ml of an aqueous solution containing 5.3g of sodium hypophosphite to 200ml of xylene, add 26g of cetyltrimethylammonium bromide, and stir evenly to prepare a water-in-oil microemulsion, called liquid A; in 200ml of xylene Add 200ml of an aqueous solution containing 2.3g of aluminum chloride, add 26g of cetyltrimethylammonium bromide, and stir evenly to prepare a water-in-oil microemulsion, which is called B liquid; in a water bath at 85°C, put B liquid Slowly drop into liquid A under strong stirring, and adjust the pH value of the system between 5-7 to obtain a milky white colloid of aluminum hypophosphite, which is evaporated to dryness with a rotary evaporator to obtain uniform and stable white nano-hypophosphorous acid aluminum powder.

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Abstract

The invention discloses a preparation method for nanometer aluminum hypophosphite, belonging to the technical field of preparation of nanometer materials. The preparation method comprises the following steps: a) adding an aqueous solution of sodium hypophosphite and cetyltrimethylammonium bromide into an organic continuous-phase solvent and carrying out a reaction at 50 to 95 DEG C so as to obtain a water-in-oil reversed-phase microemulsion containing sodium hypophosphite, wherein the microemulsion is named as liquid A; b) adding a water-soluble aluminum salt solution and cetyltrimethylammonium bromide in another organic continuous-phase solvent and carrying out a reaction at 50 to 95 DEG C so as to obtain a water-in-oil reversed-phase microemulsion containing a water-soluble aluminum salt, wherein the microemulsion is named as liquid B; c) mixing the liquid A with the liquid B, adjusting a molar ratio of sodium hypophosphite to the water-soluble aluminum salt at 80 to 95 DEG C and under atmospheric pressure, carrying out heating and refluxing, and then carrying out a reaction in a nanometer microemulsion reactor so as to obtain a nanometer aluminum hypophosphite colloid; and d) carrying out separation, purification and drying on the nanometer aluminum hypophosphite colloid so as to obtain nanometer aluminum hypophosphite powder. According to the invention, the method employs a reversed-phase microemulsion process to prepare uniform and stable nanometer aluminum hypophosphite so as to overcome deficiencies of the conventional methods and processes.

Description

technical field [0001] The invention relates to a method for preparing nano-aluminum hypophosphite, which belongs to the technical field of nano-material preparation. Background technique [0002] Aluminum hypophosphite is widely used in the flame retardant field because of its high phosphorus content, good thermal stability, relatively simple synthesis process and relatively cheap price. It can promote the carbonization of polymers in the combustion process and realize condensed phase flame retardancy. It can also be compounded with other flame retardants to play a synergistic effect and improve the flame retardancy effect. People have conducted various studies on aluminum hypophosphite, mainly including: [0003] (1) A new method and process for the preparation of aluminum hypophosphite. For example, the invention patent application document with publication number CN104163412A discloses the method of reacting sodium hypophosphite and soluble aluminum salt, separating al...

Claims

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Application Information

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IPC IPC(8): C01B25/165B82Y40/00
CPCB82Y40/00C01B25/165
Inventor 魏珊珊赵永真尤瑶瑶袁文聪刘策陈宪宏
Owner HUNAN UNIV OF TECH
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