Ammonium monoacid phosphate polyurethane flame-retardant microcapsules

A diammonium hydrogen phosphate and microcapsule technology, which is applied in the field of microcapsule synthesis, can solve problems such as migration, failure, and functional weakening of water-based coatings, and achieve the effect of simple method, easy control, and excellent thermal stability

Inactive Publication Date: 2015-04-29
重庆市大足区季家镇卫生院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the good water solubility of diammonium hydrogen phosphate, it often migrates, decomposes and fails due to dissolution in water, which weakens its functionality in water-based coatings

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0022] A method for synthesizing diammonium hydrogen phosphate polyurethane flame-retardant microcapsules, comprising the steps of:

[0023] Diammonium hydrogen phosphate is dissolved in a small amount of deionized water, and then mixed with the hydrophilic monomer to obtain an aqueous solution of the capsule core substance and the hydrophilic monomer;

[0024] Add a solvent and an emulsifier to the above aqueous solution, and disperse evenly to obtain a stable W / O emulsion;

[0025] Uniformly disperse the catalyst and oil-soluble monomer in the toluene solution;

[0026] Slowly heat up the W / O emulsion, then slowly drop the oil-soluble monomer solution into the W / O emulsion, keep stirring, and start the interfacial polymerization reaction;

[0027] Maintain the reaction, cool down and discharge the material, then centrifuge, wash the sedimentation layer with deionized water three times, filter under reduced pressure, and dry in vacuum at constant temperature to obtain microc...

Embodiment 1

[0029] Diammonium hydrogen phosphate is dissolved in deionized water according to the volume ratio of 1:1, and then mixed evenly with 10% hydrophilic monomer to obtain an aqueous solution of capsule core material and hydrophilic monomer; add 3% solvent to the above aqueous solution and 6% emulsifier, dispersed for 10 minutes to obtain a stable W / O emulsion; uniformly disperse the catalyst and oil-soluble monomer in the toluene solution; slowly heat the W / O emulsion to 50 ° C, and then the oil-soluble The monomer solution is slowly added dropwise into the W / O emulsion, and the drop is completed within 0.5h. Keep stirring and carry out the interfacial polymerization reaction for 1h; maintain the reaction, cool down to 20°C and discharge, centrifuge at 3000r / min for 1min, and use the sedimentation layer Rinse with deionized water three times, then filter under reduced pressure, and vacuum dry at a constant temperature of 35° C. for 20 hours to obtain microcapsule particles.

Embodiment 2

[0031] Diammonium hydrogen phosphate is dissolved in deionized water at a volume ratio of 1:1, and then mixed evenly with 12% hydrophilic monomer to obtain an aqueous solution of capsule core material and hydrophilic monomer; add 4% solvent to the above aqueous solution and 8% emulsifier, dispersed for 20 minutes to obtain a stable W / O emulsion; uniformly disperse the catalyst and oil-soluble monomer in the toluene solution; slowly heat the W / O emulsion to 55 ° C, and then the oil-soluble The monomer solution is slowly added dropwise into the W / O emulsion, and the drop is completed within 0.8 hours. Keep stirring and carry out the interfacial polymerization reaction for 1.5 hours; maintain the reaction, cool down to 30°C and discharge, and centrifuge at 3200r / min for 2 minutes, and the sedimentation layer Rinse with deionized water three times, then filter under reduced pressure, and vacuum dry at a constant temperature of 38° C. for 22 hours to obtain microcapsule particles. ...

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Abstract

The invention relates to a synthesis method of ammonium monoacid phosphate polyurethane flame-retardant microcapsules, which comprises the following steps: dissolving ammonium monoacid phosphate in a small amount of deionized water, and uniformly mixing with a hydrophilic monomer to obtain a capsule core substance-hydrophilic monomer water solution; adding a solvent and an emulsifier into the water solution, and dispersing uniformly to obtain a stable W/O emulsion; uniformly dispersing a catalyst and an oil-soluble monomer in a toluene solution; slowly heating the W/O emulsion, slowly and dropwisely adding the oil-soluble monomer solution into the W/O emulsion, and starting performing interfacial polymerization reaction while keeping stirring; and keeping the reaction, cooling, discharging, carrying out centrifugal separation, flushing the settlement layer with deionized water three times, carrying out vacuum filtration under reduced pressure, and carrying out constant-temperature vacuum drying to obtain microcapsule particles. The method is simple and controllable, and the synthesized ammonium monoacid phosphate polyurethane flame-retardant microcapsules have excellent heat stability and can solve the problem of high water solubility, migration and loss of effect when the ammonium monoacid phosphate is used as a fireproof flame retardant.

Description

technical field [0001] The invention relates to a microcapsule synthesis technology, in particular to a diammonium hydrogen phosphate polyurethane flame-retardant microcapsule. Background technique [0002] A microcapsule is a micron-sized container or package composed of a polymer wall shell and a solid, liquid or gaseous core substance. Artificial microencapsulation technology has been further developed since 1953 when NCR Corporation of the United States applied for the patent of microcapsules for carbonless copy paper, and was further developed by the pharmaceutical industry to coat active pharmaceutical ingredients for controlled release. In the past 10 years, this technology has achieved a wide range of commercial applications in the pharmaceutical, agricultural, food, cosmetic and textile industries. The main goal of microencapsulation technology is to protect, control the release or improve compatibility of the core material. Microcapsules can combine the advantage...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K21/14C09K21/04B01J13/16
Inventor 杨秀川黎时昌
Owner 重庆市大足区季家镇卫生院
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