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Preparation method of modified aluminum hypophosphite

A technology of aluminum hypophosphite and sodium hypophosphite, applied in dyeing physical treatment, dyeing low-molecular organic compound treatment, dyeing high-molecular organic compound treatment, etc., can solve the problems of wide particle size distribution, poor monodispersity, serious agglomeration, etc. , to achieve the effect of excellent lipophilic performance, small particle size and narrow particle size distribution

Inactive Publication Date: 2016-09-21
SHANDONG CHUANJUN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional liquid-phase synthesis is one of the main methods for preparing ultrafine powders, but there are also problems such as wide particle size distribution, difficulty in controlling, severe agglomeration, and poor monodispersity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Dissolve 318g sodium hypophosphite in water, stir at high speed to dissolve, dilute to 600ml, add 3.2g phosphate; dissolve 128g aluminum chloride and 3.8g polyethylene glycol in water, dilute to 400ml; The aluminum chloride solution is slowly added to the sodium hypophosphite solution in a mist form, and it takes 2 hours to complete the addition. During the process, the stirring speed is 1500r / min. The turbid liquid; put the above turbid liquid into a centrifuge, centrifuge for 50 minutes, wash with water twice, and dry at 105°C to obtain the modified aluminum hypophosphite; the yield is 98.1%, D50 is 6.3 μm, and the residual rate of 325 mesh sieve is 0.13%.

Embodiment 2

[0032] Dissolve 280g sodium hypophosphite in water, stir at high speed to dissolve, dilute to 650ml, add 3.4g phosphoric acid ester; dissolve 105g aluminum chloride and 4.2g polyethylene glycol in water, dilute to 450ml; The aluminum chloride solution is slowly added to the sodium hypophosphite solution in a mist form, and it takes 2.5 hours to complete the addition. During the process, the stirring speed is 1800r / min. The turbid liquid; put the above turbid liquid into a centrifuge, centrifuge for 60 minutes, wash with water twice, and dry at 160°C to obtain the modified aluminum hypophosphite; the yield is 98.5%, the D50 is 9 μm, and the 325 mesh sieve rate is 0.18 %.

Embodiment 3

[0034] Dissolve 360g of sodium hypophosphite in water, stir at high speed to dissolve, dilute to 600ml, add 4.7g of phosphoric acid ester; dissolve 145.7g of aluminum chloride and 4.4g of polyethylene glycol in water, dilute to 500ml; at a temperature of 26°C, Slowly add the aluminum chloride solution into the sodium hypophosphite solution in the form of mist, and finish adding in 2 hours. During the process, the stirring speed is 1600r / min. The turbid solution of aluminum; put the above turbid solution into a centrifuge, centrifuge for 40 minutes, wash with water three times, and dry at 180°C to obtain the modified aluminum hypophosphite; the yield is 98.3%, the D50 is 8 μm, and the residual rate of 325 mesh sieve is 0.13%.

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Abstract

The invention belongs to the technical field of preparation of a flame retardant, and particularly relates to a preparation method of modified aluminium hypophosphite. The preparation method comprises the following steps: dissolving sodium hypophosphite into water to prepare sodium hypophosphite solution, adding phosphate, and stirring at high speed and dissolving; dissolving aluminum chloride and polyethylene glycol into water to prepare aluminum chloride solution; stirring at 10-30 DEG C, normal pressure and high speed, adding the aluminum chloride solution into the sodium hypophosphite solution, slowly stirring and reacting to obtain turbid solution containing aluminum hypophosphite; pumping the turbid solution into a centrifugal machine for centrifuging, washing with water, and drying to obtain the modified aluminium hypophosphite. The prepared modified aluminium hypophosphite can be excellently dispersed into a high-molecular material, the mechanical performance and flame-retardant property of the high-molecular material can be obviously improved, and the electrical property of resin can be maintained; the preparation is simple in technology, temperature rise and regulation of pH value of the reaction solution are not needed, the yield can achieve up to 98.0%, and the modified aluminium hypophosphite is pollution-free and environmental friendly.

Description

technical field [0001] The invention belongs to the technical field of flame retardant preparation, and in particular relates to a preparation method of modified aluminum hypophosphite. Background technique [0002] Aluminum hypophosphite flame retardant has high phosphorus content, good thermal stability, high flame retardant efficiency, does not cause polymer decomposition during processing, and does not volatilize under normal conditions, so that its applied products have high thermal stability. However, the particle size of the aluminum hypophosphite prepared by the current process is between 30 and 50 microns, the particles are relatively large, and they are easy to aggregate and have poor dispersion. Grinding to ultra-fine powder, dust is easy to be generated in the process, which poses a threat to safe production. On the other hand, aluminum hypophosphite is an inorganic salt with charges on the surface, hydrophilic and oleophobic, and it is difficult to disperse uni...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09C1/40C09C3/08C09C3/10C09C3/04C08K9/04C08K3/32
Inventor 杨金晓刘琪杨忠军
Owner SHANDONG CHUANJUN CHEM
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