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Method for preparing microcapsulated superfine red phosphorus

A technology of microencapsulation and red phosphorus, applied in chemical instruments and methods, inorganic chemistry, phosphorus compounds, etc., can solve the problem of large phosphine release, weak surface adhesion of red phosphorus, and combination of coating layer and red phosphorus It can reduce the amount of PH3, stabilize the powder, and improve the strength.

Inactive Publication Date: 2006-05-24
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The above-mentioned organic coating method is due to the polarity difference between polymer or resin and red phosphorus or hydroxide, and their adhesion on the surface of red phosphorus is weak, and the coating layer is not tightly combined with red phosphorus after curing, and the amount of phosphine released Still big, still has many problems in application

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  • Method for preparing microcapsulated superfine red phosphorus

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preparation example Construction

[0024] In conjunction with accompanying drawing, the preparation method of microencapsulated ultrafine red phosphorus of the present invention comprises the following steps:

[0025] 1.1 Boil 2-200μm ultra-fine red phosphorus with sulfuric acid solution, filter, and wash with water, then boil with sodium cyanide and sodium hydroxide solution, filter, wash with water, remove impurities in the raw material, dry and seal for storage;

[0026] 1.2 Stir and dissolve the metal compound, precipitate with ammonia water, dilute with water after centrifugal precipitation, raise the temperature, add aluminum nitrate, sulfuric acid solution or hydrochloric acid solution dropwise, and obtain the metal hydroxide sol;

[0027] 1.3 Mix acrylamide monomer, N,N'-methylenebisacrylamide network agent and ammonium persulfate initiator, and heat up to react to form a polymer network gel;

[0028] 1.4 Add the polymer network gel to the sol of the metal hydroxide synthesized in step 1.2, and heat up ...

Embodiment 1

[0031] Embodiment 1: the preparation method of microencapsulated ultrafine red phosphorus of the present invention, comprises the following steps:

[0032] The first step, weigh 10.0g ultrafine red phosphorus (average particle size 14μm), boil with 30ml 5% sulfuric acid solution for 5-6h, filter, wash 3-4 times with 50ml deionized water, and then wash with 30ml 5% sodium cyanide Boil with 30ml of 1.5% sodium hydroxide solution for 1-2 hours, filter, wash with 50ml of deionized water for 3-4 times to remove trace impurities of iron and copper in the raw material, dry in vacuum at 70-80°C for 24-30 hours, cool and store in In a sealed and dry jar, 9.9 g of purified red phosphorus was obtained.

[0033] In the second step, weigh 4.5g of Al(NO 3 ) 3 9H 2 O, add 30ml of water and stir to dissolve, precipitate with ammonia water and adjust the pH to 8-9, after centrifugal precipitation, wash with 100ml of deionized water for 3-4 times, control the temperature at 70°C and drop int...

Embodiment 2

[0044] Embodiment 2: the preparation method of microencapsulated ultrafine red phosphorus of the present invention, comprises the following steps:

[0045] The first step, weigh 10.0g ultrafine red phosphorus (average particle size 5μm), boil with 30ml 5% sulfuric acid solution for 5-6h, filter, wash 3-4 times with 50ml deionized water, and then wash with 30ml 5% sodium cyanide Boil with 30ml of 1.5% sodium hydroxide solution for 1-2 hours, filter, wash with 50ml of deionized water for 3-4 times to remove trace iron and copper impurities in raw materials, vacuum dry at 70-80°C for 24-30 hours, cool and store In a sealed and dry jar, 9.8 g of purified red phosphorus was obtained.

[0046] The second step, weigh 1.5g AlCl 3 , add 30ml of water and stir to dissolve, precipitate with ammonia water and adjust the pH to 8-9, after centrifugation, add 100ml of deionized water to the precipitate to dilute, control the temperature at 75 ° C with 10% aluminum nitrate solution dropwise ...

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Abstract

The invention discloses a method for preparing micro-capsulized superfine red phosphorus, boiling the superfine red phosphorus with vitriol, sodium cyanide solution and sodium hydroxide solution, separately, filtering, eliminating impurities, and drying, and storing by sealing; blending and dissolve metal compound, depositing with ammonia, centrifuging and adding water to dilute, raising temperature, dropping in aluminum nitrate, vitriol or HCl and making metal hydroxide sol; mixing propylene acylamide monomers and N, Ní»-methylene dipropylene acylamide with ammonium persulphate, raising temperature and reacting to form high molecular network gel; adding the high molecular network gel into the metal hydroxide sol, raising the temperature and reacting to form high molecular network gel of metal hydroxide, mixing the high molecular network gel of metal hydroxide with the processed superfine red phosphorus, blending and placing still so that the sol takes the red phosphorus as the center to make surface absorption to form gel and coating a layer of colloid membrane on the red phosphorus surface, so as to obtain the micro-capsulized superfine red phosphorus. The advantages of the invention: it improves the stability, invariability and surface activity of the red phosphorus, improving processing property.

Description

a technical field [0001] The invention relates to a microencapsulation treatment technology of ultrafine red phosphorus, in particular to a preparation method of microencapsulated ultrafine red phosphorus. Two background technology [0002] Red phosphorus has been widely used in industrial and agricultural production and national defense industry. Because the smoke produced by its combustion in the air has good performance in shielding visible light, it is used in the military industry to prepare instant smoke fuming agents. Due to the advantages of high flame retardancy, non-corrosion, easy dispersion and low price, red phosphorus series flame retardants are gradually expanding their application fields in halogen-free flame-retardant engineering plastics. However, the stability and safety of red phosphorus, especially ultra-fine red phosphorus, are more prominent in the process of preparation, storage and production, because of its low ignition point, easy spontaneous combu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/023
Inventor 汪信陈海群陆路德杨绪杰朱俊武刘孝恒赵春宝韩巧凤卑凤利江晓红
Owner NANJING UNIV OF SCI & TECH
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