Preparation method of microcapsule aluminum hypophosphite flame retardant

A technology of aluminum hypophosphite and microcapsules is applied in the field of materials to achieve the effects of improved water resistance, improved safety and low cost

Active Publication Date: 2016-04-06
JINAN TAIXING FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a kind of preparation method of microcapsule aluminum hypophosphite flame retardant in order to overcome existing inorganic aluminum hypophosphite water solubility and flammability etc. Improve its application performance in water-based flame retardant systems and expand its application range

Method used

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  • Preparation method of microcapsule aluminum hypophosphite flame retardant
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  • Preparation method of microcapsule aluminum hypophosphite flame retardant

Examples

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Embodiment 1

[0028] A preparation method of microcapsule aluminum hypophosphite flame retardant, the steps are as follows:

[0029] Add melamine, 37% formaldehyde solution and water into the reaction kettle with a mass ratio of 1:2:10, adjust the pH in the kettle to 8 with 1% aqueous sodium hydroxide solution, and react for 25 minutes at a temperature of 50°C , adding polyethylene glycol with 0.1 times the mass of melamine, and then reacting for 80 minutes to end the reaction to obtain a modified melamine resin prepolymer solution;

[0030] Add inorganic aluminum hypophosphite and water into the reaction kettle at a mass ratio of 1:8 at room temperature, then add 0.3% of aluminum hypophosphite quality surfactant sodium dodecylbenzene sulfonate, and fully stir for 25 minutes to make aluminum hypophosphite Disperse evenly; then, raise the temperature to 60°C, slowly add the modified melamine resin prepolymer solution in the first step, which is 6 times the mass of aluminum hypophosphite, int...

Embodiment 2

[0031] A preparation method of microcapsule aluminum hypophosphite flame retardant, the steps are as follows:

[0032] Add melamine, 37% formaldehyde solution and water into the reaction kettle at a mass ratio of 1:4:8, adjust the pH inside the kettle to 9 with triethylamine, react at 80°C for 10 minutes, add 0.2 times The polyvinyl alcohol of melamine quality, finishes reaction after reacting again 40min, obtains modified melamine resin prepolymer solution;

[0033] Add inorganic aluminum hypophosphite and water into the reaction kettle at a mass ratio of 1:6 at room temperature, then add 0.5% aluminum hypophosphite quality surfactant hexadecyltrimethylammonium bromide, fully stir for 20min, and make the secondary The aluminum phosphate is dispersed evenly; then, the temperature is raised to 90°C, and the modified melamine resin prepolymer solution in the first step, which is 4 times the mass of aluminum hypophosphite, is slowly added to the reaction kettle, and the pH is adj...

Embodiment 3

[0035] A preparation method of microcapsule aluminum hypophosphite flame retardant, the steps are as follows:

[0036] Add melamine, 37% formaldehyde solution and water into the reaction kettle with a mass ratio of 1:1:11, adjust the pH in the kettle to 10 with triethanolamine, and react for 15 minutes at a temperature of 70°C, then add 0.3 times of melamine quality urea, and then finish the reaction after 40 minutes of reaction to obtain a modified melamine resin prepolymer solution;

[0037] Add inorganic aluminum hypophosphite and water into the reaction kettle at a mass ratio of 1:4 at room temperature, then add 1% aluminum hypophosphite quality surfactant sodium lauryl sulfate, and stir thoroughly for 30 minutes to disperse aluminum hypophosphite evenly Then, the temperature was raised to 75°C, and the modified melamine resin prepolymer solution in the first step, which was 2 times the mass of aluminum hypophosphite, was slowly added to the reactor, and the pH was adjuste...

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Abstract

The present invention relates to a preparation method of a microcapsule aluminum hypophosphite flame retardant. The method comprises the steps of: first reacting melamine, a formaldehyde solution and a resin modifier under reaction conditions of pH of 8-10 and a temperature of 50-80 DEG C for 0.5-2 h to prepare a melamine resin prepolymer; then slowly adding the prepolymer to water with aluminum phosphate dispersed therein, reacting at 65-95 DEG C for 1-5 h, and treating to obtain the microcapsule coated inorganic aluminum phosphate flame retardant. The obtained microcapsule inorganic aluminum hypophosphite flame retardant has greatly improved water resistance, boiling residual rate of 92% to 97% and average particle diameter of 10-35 mum, solves the disadvantage of flammability of inorganic aluminum hypophosphite, and greatly improves the safety of the production and application process.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a preparation method of a microcapsule aluminum hypophosphite flame retardant. Background technique [0002] Inorganic aluminum hypophosphite (Al(H 2 PO 2 ) 3 ) is a new type of halogen-free phosphorus-based flame retardant, which has good thermal stability and high phosphorus content, and its application in PBT, PET, and PA6 has a good flame-retardant effect. However, its water-soluble and flammable characteristics limit its application in certain fields. Tan Yilun et al., microencapsulated aluminum hypophosphite flame retardant glass fiber reinforced PA6 (Synthetic Resins and Plastics 2014, 31(3): 21) showed that the use of microencapsulation technology to modify aluminum hypophosphite (AlHP) can improve the flame retardant Fuel efficiency, thermal stability and compatibility with PA6. The preparation method of T-AlHP is: using ethanol as solvent, AlHP as cap...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/18B01J13/02C09K21/04
CPCB01J13/02B01J13/18C09K21/04
Inventor 刘彦余王长旭孙晓丽肖学文张雅民
Owner JINAN TAIXING FINE CHEM
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