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A high-efficiency flame-retardant nano-synergist and its preparation method and application

A nano-synergist and high-efficiency technology, applied in the field of polymer materials, can solve the problems of easy migration, affecting polymer materials, large addition amount, etc., and achieve the effects of good flame retardant performance, improved flame retardant performance, and good dispersibility.

Inactive Publication Date: 2020-04-07
SOUTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the popular flame retardant research is organic P-N intumescent flame retardants and inorganic hydrotalcite (LDH) flame retardants. Among them, organic P-N intumescent flame retardants are favored by people for their low toxicity and halogen-free advantages. , but the P-N intumescent flame retardant (IFR) has poor weather resistance and is easy to migrate. The large addition amount leads to low flame retardant efficiency, especially the large addition amount will reduce the mechanical properties of the material and affect the use of polymer materials.
Inorganic hydrotalcite (LDH) flame retardants, such as aluminum hydroxide, magnesium hydroxide, etc., have the characteristics of high flame retardant efficiency, low smoke, low toxicity, low corrosion and low price, but due to their large addition amount, Need to add nearly 50% to show a good flame retardant effect, and too much addition will often cause the mechanical properties of polymer materials to be seriously affected
A large number of studies have shown that a small amount of nano-flame retardant synergistic IFR can greatly improve the flame-retardant efficiency, but the problems of nano-particle agglomeration and low catalyst efficiency have not been well resolved. In summary, the development has high Synergists with dispersibility and high catalytic efficiency are the main challenges in the development of IFR synergistic flame retardants

Method used

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  • A high-efficiency flame-retardant nano-synergist and its preparation method and application
  • A high-efficiency flame-retardant nano-synergist and its preparation method and application
  • A high-efficiency flame-retardant nano-synergist and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Preparation of highly efficient flame retardant nano-synergist (FeP-APP3-Chitosan)

[0030] (1) Dissolve 3g of ethephon in 500mL of ice water, then add 0.22mol of diethylenetriamine, 0.3g of potassium iodide, and 160mL of an aqueous solution containing 0.64g of NaOH to obtain a reaction solution, and react the reaction solution at 15°C for 100h , evaporated and crystallized after standing overnight, and the crystallized product was recrystallized twice with ethanol, and dried in vacuum at 30°C for 4 hours to obtain organic phosphonic acid: H 3 o 3 P(CH 2 ) 2 NH(CH 2 ) 2 NH(CH 2 ) 2 NH 2 (abbreviation (AE) 3 P);

[0031] (2) 4.2g (AE) 3 P and 3.96gFeCl 2 4H 2 O was dissolved in 100mL water together, and then reacted at 70°C for 4h to obtain an intermediate, which was washed with distilled water and dried in vacuum at 50°C for 4h to obtain a nanoscale organometallic phosphonate: Fe[O 3 P(CH 2 ) 2 NH(CH 2 ) 2 NH(CH 2 ) 2 NH 2 ] 2 (referred to as FeP); ...

Embodiment 2

[0034] Preparation of highly efficient flame retardant nano-synergist (FeP-APP3-Melamine)

[0035] (1) Mix 0.2mol formamide, 0.22mol phosphorous acid and 20mL hydrochloric acid with a mass fraction of 36%, and heat to 110°C, then add 18.65mL of formaldehyde solution with a mass fraction of 37%, and the addition is complete Finally, reflux at 110°C for 1 hour, cool down, and stand overnight, then recrystallize with acetone, wash with acetone and dry under vacuum at 50°C to obtain organic phosphonic acid;

[0036] Step (2) and step (3) refer to step (2) and step (3) in embodiment 1, difference is that chitosan is replaced by melamine.

Embodiment 3

[0038] Preparation of highly efficient flame retardant nano-synergist (ZrP-APP3-Chitosan)

[0039] (1) After dissolving 2.89g ethephon in 500mL ice water, add 0.24mol triethylenetetramine, 0.3g potassium iodide, and 160mL aqueous solution containing 0.48g NaOH to obtain a reaction solution, and react the reaction solution at 18°C After standing overnight for 110 hours, it was evaporated and crystallized, and the crystallized product was recrystallized twice with ethanol, and dried in vacuum at 40°C for 6 hours to obtain organic phosphonic acid: H 2 o 3 P(CH 2 ) 2 NH(CH 2 ) 2 NH(CH 2 ) 2 NH(CH 2 ) 2 NH 2 (abbreviation (AE) 4 P);

[0040] (2) 4.2g (AE) 4 P and 4.2g ZrOCl 2 ·8H 2 Dissolve O together in 100 mL of water, and then react at 85°C for 12h to obtain an intermediate, which is washed with distilled water and then vacuum-dried at 60°C for 6h to obtain a nanoscale organometallic phosphonate: Zr[ o 3 P(CH 2 ) 2 NH(CH 2 ) 2 NH(CH 2 ) 2 NH(CH 2 ) 2 NH ...

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Abstract

The invention relates to an efficient flame-retardant nano synergist and a preparation method and application thereof, and belongs to the technical field of high polymer materials. According to the method, ammonium ion exchange reaction is carried out by amino and ammonium polyphosphate on nano organic metal phosphonate or chemical bonding is carried out by hydrogen-bond interaction between the amino and the ammonium polyphosphate, thus, the nano organic metal phosphonate is dispersed in an ammonium polyphosphate polyanion solution in a stripping manner, and a synergist with good dispersity and catalytic property is formed by self-assembling through electrostatic interaction of a polycationic polymer and ammonium polyphosphate. Compared with an existing silane coupling agent, the ammoniumpolyphosphate not only can greatly improve dispersibility of the nano organic metal phosphonate, but also has good flame retardance property, it can be ensured that the nano synergist has good dispersity in a polymer material through the electrostatic interaction of the ammonium polyphosphate and the polycationic polymer in the later period, and the flame retardance property of the flame-retardantpolymer prepared finally is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a high-efficiency flame-retardant nano synergist and its preparation method and application. Background technique [0002] Polymer materials are widely used in machinery, electronics, construction and other fields due to their excellent comprehensive properties, but at the same time their flammable characteristics also pose a threat to people's lives and property, and flame retardants can effectively reduce the The flammability of the polymer prevents the rapid spread of the fire and reduces the burning speed of the polymer. Therefore, the development of flame-retardant polymers has become a trend. At present, the popular flame retardant research is organic P-N intumescent flame retardants and inorganic hydrotalcite (LDH) flame retardants. Among them, organic P-N intumescent flame retardants are favored by people for their low toxicity and halogen-free advan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/5317C08K5/3492C08K3/32C08L23/12
CPCC08K3/32C08K5/34922C08K5/5317C08K2003/323C08L23/12
Inventor 刘昌华刘炜烽罗列红
Owner SOUTHWEST UNIV