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

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

Active Publication Date: 2014-01-01
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,

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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preparation example Construction

[0026] A method for preparing low-viscosity microcapsule-encapsulated ammonium polyphosphate, 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, and after dropping, Reflux reaction for 0.5~5h, then cool down to 40~50℃, then add end-capping agent dropwise, after the dropwise addition, keep the reaction for 0.5~3h, cool to room temperature, then filter, wash, drain, use rake dryer, in Dry under reduced pressure for 6-24 hours to obtain ammonium polyphosphate powder encapsulated 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.

[00...

Embodiment 1

[0035] In a 200L reactor with a stirring paddle and a reflux device, 20kg of melamine formaldehyde resin prepolymer CS303 and 200kg of ammonium polyphosphate were dispersed in a mixed solvent of 200kg of water and 100kg of acetone, and 0.1kg of curing agent was added dropwise. Ammonium chloride (made into a 20wt% aqueous solution), after the dropwise addition, seal the reaction kettle, raise the temperature to the reflux temperature, keep the temperature for 3 hours, then lower the temperature to 50°C, add 0.1kg methanol dropwise, complete the dropwise addition, keep the temperature for 1 hour, and react After finishing, it was cooled to room temperature, then centrifuged, washed with solvent, dried, matured and dried under reduced pressure at 80° C. for 6 hours using a rake dryer to obtain ammonium polyphosphate powder encapsulated 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 was completed, the reaction kettle was sealed, heated to the reflux temperature, kept for 2 hours, then cooled to 60°C, 0.1 kg of ethanol was added dropwise, the dropwise addition was completed, the temperature was kept for 1.5 hours, the reaction was completed, and the cooling After reaching room temperature, centrifuging, washing with solvent, drying, using a rake dryer, curing and drying under reduced pressure at 120° C. for 6 hours to obtain ammonium polyphosphate powder encapsulated in microcapsules.

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Abstract

The invention discloses a preparation method of low-viscosity microcapsule-wrapped APP. The method comprises the steps as follows: in a reaction kettle, a melamine formaldehyde resin pre-polymer and APP are dispersed in a solvent; a curing agent solution is dripped; after dripping, a backflow reaction is performed for 0.5-5 h; the temperature is decreased to 40-50 DEG C; an end-sealing agent is dripped; after dripping, a heat preservation reaction is performed for 0.5-3 h; the mixture is cooled to a room temperature; then the mixture is filtered, washed with a solved and pumped; a rake type drier is used; and the mixture is dried for 6-24 h under a pressure reduction condition, so that microcapsule-wrapped APP powder is obtained. Compared with un-wrapped APP, the microcapsule-wrapped polyphosphate powder has the characteristics of low viscosity and water solubility, excellent flowing property and compatibility, high-temperature soaking resistance, precipitation resistance, excellent electrical property and the like. The APP can be applied to high polymer materials such as polyolefin and the like and can also be applied to fabrics, epoxy 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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IPC IPC(8): C09C1/00C09C3/10
Inventor 李章武周侃
Owner PRESAFER QINGYUAN PHOSPHOR CHEM
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