A hydrophobic sio 2 Coated halogen-free intumescent flame retardant and its preparation method and application

An intumescent flame retardant and hydrophobic modifier technology, applied in the field of flame retardants, can solve the problems of increasing the difficulty of waste liquid separation and treatment, and achieve the effects of avoiding dissolution loss, strong operability, and improving compatibility

Active Publication Date: 2020-09-29
WUHAN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN101760049B discloses a preparation method of core-shell silica-coated ammonium polyphosphate, dispersing ammonium polyphosphate in an aqueous solution with a mass percentage of ethanol of 10-30%, adjusting the pH value, and then adding silicic acid dropwise Ester / ethanol solution, after fully reacting, add titanate coupling agent and borate coupling agent to the slurry for surface treatment to obtain silicon dioxide-coated ammonium polyphosphate, the ethanol aqueous solution used in this patent The proportion is very high, accounting for about 70-90%, and it takes a long time for the hydrolysis of ethyl orthosilicate. Ammonium polyphosphate always exists in the reaction system, and there will be a lot of dissolved in water, which will cause losses, and increase the difficulty of waste liquid separation and treatment.
In addition, the patent states that if the ethanol concentration is too high, coating will not occur, indicating that the patent cannot solve the problem of loss of ammonium polyphosphate due to dissolution in water by adjusting the amount of water

Method used

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  • A hydrophobic sio <sub>2</sub> Coated halogen-free intumescent flame retardant and its preparation method and application
  • A hydrophobic sio <sub>2</sub> Coated halogen-free intumescent flame retardant and its preparation method and application
  • A hydrophobic sio <sub>2</sub> Coated halogen-free intumescent flame retardant and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1) Add 5mL of cationic polyelectrolyte polydiallyldimethylammonium chloride aqueous solution with a mass concentration of 2% and 95mL of absolute ethanol into the three-necked bottle and stir evenly, then disperse 15g of the halogen-free expansion flame retardant ammonium polyphosphate Pretreatment was performed in the above solution, and after stirring at room temperature for 6 minutes, solid-liquid separation was carried out to obtain a halogen-free intumescent flame retardant ammonium polyphosphate with positive charges on the surface.

[0038] 2) Add 100mL absolute ethanol, 2.0mL ultrapure water, 3.0mL NH 3 ·H 2 O, after stirring for 2min, directly add 3.0mL orthosilicate ethyl ester, and after magnetic stirring reaction for 4.0h, the nano-SiO with negative charge on the surface is obtained. 2 Collagen solution.

[0039] 3) The positively charged halogen-free intumescent flame retardant prepared in step 1) is directly added to the negatively charged nano-SiO in st...

Embodiment 2

[0042] 1) Add 3mL of cationic polyelectrolyte polydiallyldimethylammonium chloride aqueous solution with a mass concentration of 4% and 97mL of absolute ethanol into the there-necked bottle and stir evenly, then disperse 20g of halogen-free intumescent flame retardant melamine in the above-mentioned Pretreatment is carried out in the solution, and after stirring at room temperature for 8 minutes, solid-liquid separation is carried out to obtain the positively charged halogen-free intumescent flame retardant melamine on the surface.

[0043] 2) Add 100mL absolute ethanol, 2.8mL ultrapure water, 4.0mL NH 3 ·H 2 O, after stirring for 4min, directly add 4.5mL orthosilicate ethyl ester, and after magnetic stirring for 5.5h, the nano-SiO with negative charge on the surface is obtained. 2 Collagen solution.

[0044] 3) The positively charged halogen-free intumescent flame retardant melamine prepared in step 1) is directly added to the negatively charged nano-SiO in step 2). 2 Coll...

Embodiment 3

[0047] 1) Add 2.5mL of cationic polyelectrolyte polydiallyldimethylammonium chloride aqueous solution with a mass concentration of 6% and 97.5mL of absolute ethanol into the there-necked bottle and stir evenly, then mix the halogen-free expansion flame retardant melamine phosphate 25 g was dispersed in the above solution for pretreatment, and after stirring at room temperature for 10 minutes, solid-liquid separation was carried out to obtain a halogen-free intumescent flame retardant melamine phosphate with a positive charge on the surface.

[0048] 2) Add 100mL absolute ethanol, 1.0mL ultrapure water, 5.0mL NH 3 ·H 2 O, after stirring for 5min, directly add 5.5mL orthosilicate ethyl ester, and after magnetic stirring for 7.5h, the nano-SiO with negative charge on the surface is obtained. 2 Collagen solution.

[0049] 3) Add the positively charged halogen-free intumescent flame retardant melamine phosphate prepared in step 1) directly to the negatively charged nano-SiO in st...

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Abstract

The invention discloses a hydrophobic SiO 2 Coated halogen-free intumescent flame retardant and its preparation method and application. The preparation method comprises: (1) obtaining a halogen-free intumescent flame retardant with a positive charge on the surface; (2) obtaining a nano-SiO with a negative charge on the surface 2 Collagen solution; (3) to obtain SiO 2 Coated halogen-free intumescent flame retardant; (4) obtain hydrophobic SiO 2 Encapsulated halogen-free intumescent flame retardant. The invention provides a simple preparation method of a hydrophobic halogen-free intumescent flame retardant, which can be carried out step by step, has strong operability, is beneficial to industrial production, and can effectively avoid the reaction of the halogen-free intumescent flame retardant in water-containing Existing in the system for a long time causes the problem of flame retardant dissolution loss.

Description

technical field [0001] The invention belongs to the technical field of flame retardants, and more specifically relates to a hydrophobic SiO 2 Coated halogen-free intumescent flame retardant and its preparation method and application. Background technique [0002] Typical representatives of intumescent halogen-free flame retardants are ammonium polyphosphate, melamine phosphate, melamine, etc., which have excellent properties such as low smoke, low toxicity, and high-efficiency flame retardancy, and are widely used in polymer resin materials. However, these expandable halogen-free flame retardants are all inorganic materials, which have poor compatibility with polymer resin materials. In addition, ammonium polyphosphate, melamine phosphate, and melamine have different degrees of solubility in water, are easy to hydrolyze, and have moisture absorption and migration. Penetration and other disadvantages greatly reduce its application field. [0003] Common modification methods...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K13/06C08K9/10C08K9/06C08K9/04C08K3/32C08L101/00
CPCC08K3/32C08K9/06C08K9/08C08K9/10C08K13/06C08K2003/323C08L101/00C08L2201/02C08L2201/22
Inventor 王春蕾胡黎明王洋闫俊涛范国枝秦振华李建芬张顺喜
Owner WUHAN POLYTECHNIC UNIVERSITY
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