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Preparation method of novel phosphorus-nitrogen flame retardant

A flame retardant and a new type of technology, applied in the field of flame retardants, can solve the problems of poor compatibility of phosphorene nanosheets, low addition amount, high flame retardant efficiency, etc. The effect of efficiency

Pending Publication Date: 2022-04-19
GUANGDONG HERUN PRECISION METAL MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a novel phosphorus-nitrogen flame retardant preparation method aimed at the deficiencies of the prior art, which not only overcomes the problems of phosphorene nanosheet oxidation and poor compatibility, but also has the advantages of low addition amount, high resistance Advantages of fuel efficiency

Method used

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  • Preparation method of novel phosphorus-nitrogen flame retardant
  • Preparation method of novel phosphorus-nitrogen flame retardant
  • Preparation method of novel phosphorus-nitrogen flame retardant

Examples

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Effect test

Embodiment 1

[0031] A preparation method of a novel phosphorus-nitrogen flame retardant, comprising the following steps:

[0032] (1) Under the protection of nitrogen, 1.0g black phosphorus crystals and 20.0g urea were added in the ball mill jar, and then ball milled at a speed of 500r / min for 8 hours; after the ball mill finished, transfer the ball mill product to In a centrifuge tube, centrifuge at 1000r / min for 15 minutes to collect the upper layer suspension; centrifuge the upper layer suspension at 8000r / min for 30 minutes, collect the lower layer precipitate and dry it in vacuum at 140°C for 4 hours to obtain the amino graft Branched phosphorene nanosheets;

[0033] (2) Get 2.0g of melamine and add 30ml of deionized water, mechanically stir, and the rotating speed is 300r / min; then dropwise add 8.6ml (37%) of formaldehyde solution, and use the newly configured Na 2 CO 3 (10%) solution adjusts pH to 9, heats up to 80 DEG C, continues to stir for 30 minutes, obtains melamine-formalde...

Embodiment 2

[0036] A preparation method of a novel phosphorus-nitrogen flame retardant, comprising the following steps:

[0037] (1) Under the protection of nitrogen, 1.5g black phosphorus crystals and 40.0g urea were added to the ball mill jar, then ball milled at a speed of 600r / min for 12 hours; after the ball mill finished, transfer the ball mill product to In a centrifuge tube, centrifuge at 1500r / min for 20 minutes to collect the upper layer suspension; centrifuge the upper layer suspension at 6000r / min for 20 minutes, collect the lower layer precipitate and dry it in vacuum at 120°C for 5 hours to obtain the amino graft Branched phosphorene nanosheets;

[0038] (2) Get 4.0g of melamine and add 50ml of deionized water, mechanically stir, and the rotating speed is 400r / min; 2 CO 3 (10%) solution adjusts pH to 8, heats up to 60 ℃, continues to stir for 60 minutes, obtains melamine-formaldehyde prepolymer;

[0039] (3) Get 1.5g amino-grafted phosphorene nanosheets, add it to 20.0g m...

Embodiment 3

[0041] A preparation method of a novel phosphorus-nitrogen flame retardant, comprising the following steps:

[0042](1) Under the protection of nitrogen, 2.0g black phosphorus crystals and 60.0g urea were added in the ball mill jar, and then ball milled at a speed of 800r / min for 16 hours; after the ball mill finished, the ball mill product was transferred to In a centrifuge tube, centrifuge at 2000r / min for 10 minutes to collect the upper layer suspension; centrifuge the upper layer suspension at 5000r / min for 30 minutes, collect the lower layer precipitate and dry it in vacuum at 100°C for 8 hours to obtain the amino graft Branched phosphorene nanosheets;

[0043] (2) Take 5.0g of melamine and add 40ml of deionized water, stir mechanically at a speed of 300r / min; then add 17.9ml (37%) of formaldehyde solution dropwise, and use newly configured NaHCO 3 (10%) solution adjusts pH to 8, heats up to 50 ℃, continues to stir for 40 minutes, obtains melamine-formaldehyde prepolymer...

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Abstract

The invention relates to the technical field of flame retardants, in particular to a preparation method of a novel phosphorus-nitrogen flame retardant, which comprises the following steps: step 1, mixing and ball-milling black phosphorus crystals and amine substances in an inert atmosphere; 2, transferring a ball-milled product obtained in the step 1 into a centrifugal tube by using a polar solvent, carrying out centrifugal treatment, then collecting an upper-layer suspension, continuously centrifuging, collecting a lower-layer precipitate, and drying, so as to obtain an amino-grafted phosphorene nanosheet; 3, melamine is dissolved in deionized water, a formaldehyde solution is slowly added under the heating condition, the pH is adjusted to be alkaline, a reaction is conducted, and a melamine-formaldehyde prepolymer is obtained; and 4, adding the amino-grafted phosphorene nanosheet prepared in the step 2 into the melamine-formaldehyde prepolymer prepared in the step 3, mixing, dispersing, filtering, and drying in vacuum to obtain the novel phosphorus-nitrogen flame retardant.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a preparation method of a novel phosphorus-nitrogen flame retardant. Background technique [0002] Polymer materials have the advantages of good chemical resistance, easy processing and molding, and low cost, and are widely used in various fields of people's lives. However, since most polymer materials contain C, H, O and other elements, they are extremely flammable, and a large amount of toxic and harmful gases will be produced during the combustion process, which poses a huge safety hazard to the life and property safety of the society and people. . In order to improve the flammability of high molecular polymers, many scholars and research institutes at home and abroad have carried out in-depth research on polymer flame retardant technology. From halogen flame retardants to halogen-free flame retardants, new flame retardant materials are constantly emerging. The deve...

Claims

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Application Information

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IPC IPC(8): C08L61/28C08K9/04C08K3/02C08L63/00C08G12/32
CPCC08L61/28C08G12/32C08K9/04C08K3/02C08L63/00C08K2003/026C08L2201/02C08K2201/011
Inventor 刘声金
Owner GUANGDONG HERUN PRECISION METAL MATERIALS CO LTD
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