Preparation method of low-viscosity microcapsule-wrapped APP (ammonium polyphosphate)

An ammonium polyphosphate and microcapsule technology, applied in the direction of dyeing polymer organic compounds, fibrous fillers, etc., can solve the problems of poor flame retardant durability, thorn-like powder, and poor flowability, and achieve excellent Effects of flowability and compatibility, average particle size, excellent electrical properties

Active Publication Date: 2015-06-17
PRESAFER QINGYUAN PHOSPHOR CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to its hygroscopicity, it is not conducive to long-term storage, and also reduces its electrochemical performance, which limits its application in the electrical industry.
[0005] (2) Poor compatibility and dispersion with the substrate
As a result of mechanical dispersion, APP powder is easy to form agglomerates in the local part of the material, which not only reduces the material properties, but also because of the lack of affinity between them, the flame retardant is easy to migrate from the inside of the material to the surface, causing "white frost" on the surface. The flame retardant performance gradually decreases
[0006] (3) The flame retardant durability is not good
[0007] (4) The thermal stability of APP is poor
Compared with unwrapped APP, the water solubility of the wrapped APP is significantly reduced and the thermal stability is improved, but this method still has shortcomings. The cross-linking density of the capsule material is affected by the ratio of melamine / phenol to formaldehyde, the reaction temperature And the influence of the pH value of the solution is large and difficult to control, and the reproducibility of the product is not good
[0010] In addition to the shortcomings mentioned above, the above patents ignore the following point: many prepolymers in the market can wrap APP, and the water solubility can also be very low, but in practical applications, they face the following Problems: 1. When the amount of ammonium polyphosphate added is high, the viscosity of the solvent system is relatively high, which cannot be dispersed and cannot be processed and used; 2. The powder is thorny, has poor fluidity and is not compact; and this problem is caused The most important reason is that when wrapping, due to the continuous curing of the melamine formaldehyde resin prepolymer during the reaction process, even if the powder has formed a wrapping layer, there are still some active groups exposed to continue the crosslinking reaction , causing the coating layer to have many branched chains, the surface is uneven, and the gap between the powders is increased, and the powders are not dense, which in turn leads to the reason that the viscosity is relatively high in the actual application process.

Method used

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  • Preparation method of low-viscosity microcapsule-wrapped APP (ammonium polyphosphate)
  • Preparation method of low-viscosity microcapsule-wrapped APP (ammonium polyphosphate)
  • Preparation method of low-viscosity microcapsule-wrapped APP (ammonium polyphosphate)

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[0026] A method for preparing ammonium polyphosphate wrapped in low-viscosity microcapsules, comprising the following steps: in a reaction kettle, dispersing melamine-formaldehyde resin prepolymer and ammonium polyphosphate in a solvent, adding a curing agent solution dropwise, after the dropwise addition, Reflux reaction for 0.5~5h, then cool down to 40~50°C, then add end-capping agent dropwise, after dropwise addition, keep warm for 0.5~3h, cool to room temperature, then filter, wash, drain, use rake dryer, Dry under reduced pressure for 6-24 hours to obtain ammonium polyphosphate powder wrapped in microcapsules.

[0027] The mass ratio of ammonium polyphosphate, melamine formaldehyde resin prepolymer and solvent is 1:0.05~0.20:1.5~3.0.

[0028] The curing agent is at least one of ammonium chloride, diammonium hydrogen phosphate, ammonium hydrogen phosphate, sodium dihydrogen phosphate, potassium dihydrogen phosphate acid salt, citric acid, and acetic acid.

[0029] The cap...

Embodiment 1

[0035] In a 200L reactor with a stirring paddle and a reflux device, disperse 20kg of melamine-formaldehyde resin prepolymer CS303 and 200kg of ammonium polyphosphate in a mixed solvent of 200kg of water and 100kg of acetone, and add 0.1kg of curing agent dropwise Ammonium chloride (made into 20wt% aqueous solution), after the dropwise addition, seal the reactor well, raise the temperature to reflux temperature, keep it warm for 3h, then cool down to 50°C, add 0.1kg of methanol dropwise, after the dropwise addition, keep it warm for 1h, and react Finished, cooled to room temperature, then centrifuged, washed with a solvent, dried, and aged and dried at 80°C for 6 hours under reduced pressure using a rake dryer to obtain ammonium polyphosphate powder wrapped in microcapsules.

Embodiment 2

[0037] In a 200L reactor with a stirring paddle and a reflux device, 10kg of melamine formaldehyde resin prepolymer 5830 and 200kg of ammonium polyphosphate were dispersed in 350kg of DMF solvent, and 0.2kg of curing agent diammonium hydrogen phosphate ( 20wt% aqueous solution), after the dropwise addition, seal the reactor well, raise the temperature to reflux temperature, keep it warm for 2h, then cool down to 60°C, add 0.1kg of ethanol dropwise, after the dropwise addition, keep warm for 1.5h, the reaction is over, cool to room temperature, then centrifuged, washed with a solvent, dried, and aged and dried at 120° C. for 6 hours under reduced pressure using a rake dryer to obtain ammonium polyphosphate powder wrapped in microcapsules.

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Abstract

The invention discloses a method for preparing ammonium polyphosphate wrapped in low-viscosity microcapsules. After the addition, reflux reaction for 0.5~5h, then lower the temperature to 40~50°C, then add the end-capping agent dropwise, after the dropwise addition, keep the temperature for 0.5~3h reaction, cool to room temperature, then filter, wash with solvent, drain, and use Rake dryer, drying under reduced pressure for 6~24h to obtain ammonium polyphosphate powder wrapped in microcapsules. Compared with the uncoated ammonium polyphosphate, the microcapsule-coated ammonium polyphosphate prepared by the present invention has low viscosity, excellent fluidity and compatibility, low water solubility, high temperature immersion resistance, precipitation resistance, excellent electrical properties, etc. features. It can be used in polymer materials such as polyolefins, and can also be used in fabrics, epoxies and coatings.

Description

technical field [0001] The invention relates to a method for preparing low-viscosity microcapsule-wrapped ammonium polyphosphate. Background technique [0002] APP is an excellent flame retardant. It has high phosphorus content and nitrogen content, and there is a P-N synergistic effect between them, so it has high flame retardant performance, and because it can be compounded with many other flame retardants to improve its flame retardancy and performance Sex, little smoke, low toxicity (LD50>10g / kg), so some people call it "environmentally friendly flame retardant". [0003] However, due to the characteristics of its own chemical structure, it has the following inherent defects. [0004] (1) High hygroscopicity. There are oxygen bonds in its chemical structure, and the oxygen bonds are often arranged on the outer surface, making it easy to absorb water molecules. Due to its hygroscopicity, it is not conducive to long-term storage, and its electrochemical performance ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09C1/00C09C3/10
Inventor 李章武周侃
Owner PRESAFER QINGYUAN PHOSPHOR CHEM
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