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Nucleotide-based flame retardant microsphere and preparation method and application thereof

A nucleotide and nucleotide-based technology, applied in the field of bio-based flame retardants and their preparation, achieves the effects of wide application range, simple preparation operation and good flame retardant effect

Active Publication Date: 2016-05-11
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no research report on the preparation and application of nucleotide-based flame-retardant microspheres in the world.

Method used

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  • Nucleotide-based flame retardant microsphere and preparation method and application thereof
  • Nucleotide-based flame retardant microsphere and preparation method and application thereof
  • Nucleotide-based flame retardant microsphere and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Synthesis of Nucleotide-Based Flame Retardant Microspheres

[0036] Weigh 0.1mol (12.61g) of melamine and add it to a 250ml four-necked flask, add 150ml of deionized water, adjust the pH of the solution to 11 with sodium hydroxide, heat to 30°C, add 0.3mol (24.34g) of 37% formaldehyde solution ), stirred and reacted for 8h to obtain a clear and transparent prepolymer liquid.

[0037] Weigh 0.05mol (18.16g) of guanylic acid, add it into a 500ml four-necked bottle with a mechanical stirrer, a condenser tube, and a constant pressure dropping funnel, add 100ml of deionized water, and a dispersant polymer with 0.5% guanylic acid quality. Vinyl alcohol (0.09g), heated up to 30°C, stirred for 3h to obtain a homogeneous solution. Then, the previously obtained pre-polymerization solution was added dropwise to the solution, and the drop was completed after 4 hours, and then the pH of the solution was adjusted to 6 with hydrochloric acid, stirred and reacted at 30°C for 6 hours, ...

Embodiment 2

[0039] Synthesis of Nucleotide-Based Flame Retardant Microspheres

[0040] Weigh 0.08mol (10.09g) of melamine into a 250ml four-neck flask, add 120ml of deionized water, adjust the pH of the solution to 10 with sodium hydroxide, heat to 50°C, add 0.24mol (19.47g) of formaldehyde solution, and stir After 4 hours of reaction, a clear and transparent prepolymer solution was obtained.

[0041] Weigh guanylic acid 0.08mol (29.06g), join with mechanical stirring, condenser tube, in the 500ml four-necked bottle of constant pressure dropping funnel, add deionized water 120ml, the dispersant polymer of 0.3% guanylic acid mass Vinyl alcohol (0.09g), heated to 50°C, stirred for 1.5h to obtain a uniform solution. Then, the previously obtained prepolymerization solution was added dropwise to the solution for 2.5 hours, and then the pH of the solution was adjusted to 5 with hydrochloric acid, stirred and reacted for 6 hours at 50°C, separated, washed and dried to obtain flame-retardant mic...

Embodiment 3

[0043] Synthesis of Nucleotide-Based Flame Retardant Microspheres

[0044] Weigh 0.1mol (12.61g) of melamine into a 250ml four-neck flask, add 150ml of deionized water, adjust the pH of the solution to 13 with triethylamine, heat to 60°C, add 0.5mol of glyoxal solution, and stir for 4 hours , to obtain a clear and transparent pre-polymerization solution.

[0045] Weigh 0.2mol (72.64g) of guanylic acid, add it to a 500ml four-necked bottle with mechanical stirring, condenser, and constant pressure dropping funnel, add 200ml of deionized water, and 0.1% guanylic acid mass as a dispersant polyethylene Alcohol (0.07g), heated up to 60°C, stirred for 1h to obtain a homogeneous solution. Then, the previously obtained prepolymerization solution was added dropwise to the solution for 1 hour, and then the pH of the solution was adjusted to 4 with acetic acid, stirred and reacted for 5 hours at 60°C, separated, washed, and dried to obtain flame-retardant microspheres. Immerse the flam...

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Abstract

The present invention discloses a nucleotide-based flame retardant microsphere and a preparation method and application thereof. The nucleotide-based flame retardant microsphere has a structural formula as shown in formula (1). According to the method, the PH value of melamine and an aldehyde-group-containing compound is adjusted to 8 to 13, the melamine and the aldehyde-group-containing compound are reacted to obtain a hydroxyl-containing prepolymer solution; nucleotide is dissolved in deionized water, dispersant polyvinyl alcohol is added, and a nucleotide solution is obtained by heating to 30-90 DEG C and stirring for 1-5h; the prepolymer solution is added dropwise into the nucleotide solution, the pH is adjusted to 1-6 for reaction at 30-90 DEG C for 1-8h, and a flame retardant microsphere is obtained by separation; and finally, the flame retardant microsphere is immersed in a solution of a silane coupling agent, and active groups on microsphere surface are functionally treated. The nucleotide-based flame retardant microsphere is derived from biological raw materials, consumption of non-renewable resources such as petrochemicals can be reduced, the nucleotide-based flame retardant microsphere belongs to a non-halogen system, secondary hazards in the process of combustion of the material can be reduced, and the nucleotide-based flame retardant microsphere belongs to an environment-friendly green flame retardant.

Description

technical field [0001] The invention relates to a bio-based flame retardant and a preparation method thereof, in particular to a nucleotide-based flame-retardant microsphere, a preparation method and application thereof, especially an application in flame-retardant polymer materials. Background technique [0002] The application of polymer materials is becoming more and more extensive, and it has become one of the indispensable materials that are closely related to people's material life. However, due to their own structure, most polymer materials are flammable, so while bringing convenience to people's lives, they also hide fire safety hazards. Endowing materials with flame retardant properties is an important means of preventing fire accidents in the world. It can avoid the occurrence of fire or at least play a role in retarding combustion, delaying fire spread, and gaining time for escape and rescue. It is of great significance to the protection of human life and property...

Claims

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Application Information

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IPC IPC(8): C08K9/06C08K5/521C08L23/12C08L23/06C08L25/06C08L75/04C08L23/08C08L67/04
CPCC08K5/521C08K9/06C08L2201/02C08L67/04C08L23/12C08L23/0853C08L23/06C08L25/06C08L75/04
Inventor 李娟王志敬
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI