P-N-Si flame-retardant nanogel and preparation method and application thereof

A nanogel, p-n-si technology, applied in the manufacture of fire-resistant and flame-retardant filaments, artificial filaments made of viscose, etc., can solve the problems of unfriendly environment, releasing a large amount of poisonous gas and smoke, environmental hazards, etc. Achieve the effects of rich benzene rings and carbon chains, improved flame retardancy, and high carbon residue

Active Publication Date: 2018-09-28
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Halogen organic compound flame retardants, such as Lenging (Austria), Polynosic (Japan), HFG (Japan), these fibers containing halogen organic compound flame retardants, although the flame retardant effect is good, but they are not friendly to the environment or burn Release a large amount of poisonous gas and smoke, causing harm to the environment

Method used

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  • P-N-Si flame-retardant nanogel and preparation method and application thereof
  • P-N-Si flame-retardant nanogel and preparation method and application thereof
  • P-N-Si flame-retardant nanogel and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] (1) Weigh 2.76g of 0.02mol 3,4-dihydroxybenzaldehyde and dissolve it in 30ml of methanol, put 1mg of zinc acetate as a catalyst, weigh 0.01mol of 1,3-bis(3-aminopropyl)-1, 2.48g of 1,3,3-tetramethyldisiloxane, dissolved in 15ml of methanol, put into a 100ml constant pressure separatory funnel, and slowly added dropwise to the solution containing 3,4-dihydroxybenzene within 1 hour In a three-necked flask of formaldehyde, magnetically stirred, heated to 70°C in a water bath, and reacted for 10 hours, the reactant was precipitated with a mixture of ice and water, and vacuum-dried at 50°C for 12 hours, and the obtained intermediate product (I) was brown-black powder.

[0046] (2) Weigh 0.01mol intermediate product (I) 4.88g and 0.02mol 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide 4.32g, with 60ml absolute ethanol as solvent, The oil bath was heated to 70°C and reacted for 12 hours. The reacted product was precipitated with a mixture of ice and water, and dried in vacu...

Embodiment 2

[0056] (1) Dissolve 0.02mol 2.44g p-hydroxybenzaldehyde in 30ml methanol, put 1mg zinc acetate as catalyst, weigh 0.01mol 1,3-bis(3-aminoethyl)tetramethyldisiloxane 2.20g, dissolved in 15ml of methanol, put into a 100ml constant pressure separatory funnel, slowly added dropwise to the three-necked flask containing p-hydroxybenzaldehyde within 1 hour, stirred magnetically, heated the water bath to 70°C, and reacted After 10 hours, the reactant was precipitated with a mixture of ice and water, and dried under vacuum at 50° C. for 12 hours, and the obtained intermediate product (I) was brownish yellow powder.

[0057] (2) Weigh 0.01mol intermediate product (I) 4.28g and 0.02mol 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide 4.32g, with 50ml absolute ethanol as solvent, The oil bath was heated to 70°C and reacted for 12 hours. The reacted product was precipitated with a mixture of ice and water, and dried in vacuum at 60°C for 12 hours. The obtained intermediate product (II) w...

Embodiment 3

[0068] (1) Weigh 0.02mol 2.44g o-hydroxybenzaldehyde and dissolve it in 30ml methanol, put 1mg zinc acetate as catalyst, weigh 0.01mol 1,3-bis(3-aminopropyl)tetramethyldisiloxane 2.48g, the reaction conditions are the same as in Example 1, and the intermediate product (I) obtained is a bright yellow powder.

[0069] (2) Weigh 4.56 g of 0.01 mol of intermediate product (I) and 2.76 g of 0.02 mol of diethyl phosphate, the reaction conditions are the same as in Example 1, and the obtained intermediate product (II) is gray powder.

[0070] (3) Weigh 0.0005mol intermediate product (II) 0.382g and 0.005mol methacryloyl chloride 0.52g (0.48ml), dissolve in 15ml tetrahydrofuran, 0.005mol triethylamine 0.5g (0.7ml) is a binding agent, react The conditions were the same as in Example 1, and the obtained intermediate product (III) was a white powder.

[0071] (4) With 20ml dimethyl sulfoxide as a solvent and 0.01g ammonium persulfate as an initiator, 0.5g of the intermediate product (II...

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Abstract

The invention relates to a P-N-Si flame-retardant nanogel and a preparation method and the application thereof. The P-N-Si flame-retardant nanogel adopts a structural formula as follows: FORMULA. Thepreparation method comprises the following steps: preparing an intermediate I, preparing an intermediate II, preparing an intermediate III, and preparing the P-N-Si flame-retardant nanogel. The P-N-Siflame-retardant nanogel is applied to the preparation of flame-retardant viscose fiber, lyocell fiber or other regenerated cellulose fiber. The flame-retardant nanogel is a halogen-free environment-friendly flame retardant which does not release formaldehyde, and incombustible gas decomposed by heat can enable a system to foam to produce a blow-out effect; the nanogel is in a form of nano-sized microparticles, the addition amount thereof into a spinning stock solution is reduced to 8-16%, and the technological cost can be effectively reduced.

Description

technical field [0001] The invention belongs to the field of flame retardants and their preparation and application, in particular to a P-N-Si flame-retardant nano gel and its preparation method and application. Background technique [0002] Flame retardants are a class of additives that can effectively prevent materials from burning or inhibit flame propagation. At present, there are many flame retardants used for flame-retardant viscose cellulose at home and abroad. According to the classification of elements, they are mainly divided into halogen-based, phosphorus-based, and nitrogen-based. , silicon series and the mixed system of several series. Halogen organic compound flame retardants, such as Lenging (Austria), Polynosic (Japan), HFG (Japan), these fibers containing halogen organic compound flame retardants, although the flame retardant effect is good, but they are not friendly to the environment or burn Release a large amount of poisonous gas and smoke, causing harm ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F130/08D01F1/07D01F2/08
CPCC08F130/08D01F1/07D01F2/08
Inventor 吴德群明景范硕朱建华李娜李发学王学利俞建勇
Owner DONGHUA UNIV
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