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Bio-based reactive flame retardant, flame-retardant waterborne polyurethane emulsion and preparation methods of bio-based reactive flame retardant and flame-retardant waterborne polyurethane emulsion

A reactive flame retardant, water-based polyurethane technology, applied in the field of flame retardant materials, can solve the problems of complex preparation process, poor compatibility between bio-based flame retardants and substrates, etc.

Active Publication Date: 2021-09-07
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the problems of poor compatibility between bio-based flame retardants and substrates, complex preparation process and further improvement of flame retardancy in the prior art, the present invention provides a bio-based reactive flame retardant, flame-retardant water-based polyurethane emulsion and its preparation method

Method used

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  • Bio-based reactive flame retardant, flame-retardant waterborne polyurethane emulsion and preparation methods of bio-based reactive flame retardant and flame-retardant waterborne polyurethane emulsion
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  • Bio-based reactive flame retardant, flame-retardant waterborne polyurethane emulsion and preparation methods of bio-based reactive flame retardant and flame-retardant waterborne polyurethane emulsion

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] 1. Preparation of bio-based reactive flame retardant (PAMAD-1):

[0046] Add 0.55g of dimethylolpropionic acid (DMPA), 7.95g of phytic acid (PA) and 3.1g of melamine (MA) into 60mL of deionized water respectively to obtain 2,2-dimethylolpropionic acid dispersion, phytic acid Dispersions and dispersions of nitrogenous compounds;

[0047] At a stirring speed of 100r / min and 75°C, add the 2,2-dimethylolpropionic acid dispersion liquid dropwise to the melamine dispersion liquid, react for 4 hours, and then slowly add the phytic acid dispersion liquid dropwise into the reaction system , after all the dropwise addition, continue to react for 5h, filter with suction, wash, dry with a blast oven to remove most of the water, and then dry with a vacuum oven to obtain a bio-based reactive flame retardant PAMAD-1 with a yield of 74.7% , The char formation rate is 12.37% (at a temperature of 480°C).

[0048] Yield / %=m 产物 / (m DMPA +m PA +m MA )*100

[0049] 2. Preparation of f...

Embodiment 2

[0052] 1. Preparation of bio-based reactive flame retardant (PAMAD-2):

[0053] Add 1.6g dimethylolpropionic acid (DMPA), 7.54g phytic acid (PA) and 10.1g melamine (MA) into 60mL deionized water respectively to obtain 2,2-dimethylolpropionic acid dispersion, phytic acid Dispersions and dispersions of nitrogenous compounds;

[0054] At a stirring speed of 100r / min and 85°C, add the 2,2-dimethylolpropionic acid dispersion liquid dropwise to the melamine dispersion liquid, react for 2 hours, and then slowly add the phytic acid dispersion liquid dropwise into the reaction system , after all the dropwise addition, continue to react for 3h, filter with suction, wash, remove most of the water by drying in a blast oven, and then dry in a vacuum oven to obtain a bio-based reactive flame retardant PAMAD-2, with a yield of 81.27% , The char formation rate is 17.11% (at a temperature of 480°C).

[0055] 2. Preparation of flame retardant water-based polyurethane emulsion PWPU-2:

[0056...

Embodiment 3

[0058] 1. Preparation of bio-based reactive flame retardant (PAMAD-3):

[0059] Add 2.6g dimethylolpropionic acid (DMPA), 7.54g phytic acid (PA) and 7.06g melamine (MA) into 60mL deionized water respectively to obtain 2,2-dimethylolpropionic acid dispersion, phytic acid Dispersions and dispersions of nitrogenous compounds;

[0060] At a stirring speed of 100r / min and at 80°C, add the 2,2-dimethylol propionic acid dispersion liquid dropwise to the melamine dispersion liquid, react for 3 hours, and then slowly add the phytic acid dispersion liquid dropwise into the reaction system , after all the dropwise addition, continue to react for 4h, filter with suction, wash, remove most of the water by drying in a blast oven, and then dry in a vacuum oven to obtain a bio-based reactive flame retardant PAMAD-3 with a yield of 80.7% , The char formation rate is 16.77%.

[0061] 2. Preparation of flame retardant water-based polyurethane emulsion PWPU-3:

[0062] Weigh 56.2g of polypropy...

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Abstract

The invention relates to the technical field of flame-retardant materials, and particularly discloses a bio-based reactive flame retardant, a flame-retardant waterborne polyurethane emulsion and preparation methods of the bio-based reactive flame retardant and the flame-retardant waterborne polyurethane emulsion. The bio-based reactive flame retardant is prepared from 2,2-dimethylolpropionic acid, phytic acid and a nitrogen-containing compound in a molar ratio of (0.3-2):1:(2-8) through reaction, and the bio-based reactive flame retardant is good in storage stability, high in char forming rate and stable in flame retardant property. The bio-based reactive flame retardant is used as a hard-segment flame-retardant chain extender to chemically modify aqueous polyurethane, the aqueous polyurethane can have good flame resistance and heat resistance, the bio-based flame-retardant polyurethane material with characteristics of excellent mechanical property and excellent flame resistance can be obtained, the limit oxygen index can achieve 29.5%, the UL-94 combustion grade can achieve the v-0 grade, the carbon residue rate can achieve 15%, and the tensile strength can achieve 13 MPa or more; and the raw material source and the preparation process are green and environment-friendly, meet the development trend of carbon neutralization and the requirements of continuous development, and have relatively high popularization and application values.

Description

technical field [0001] The invention relates to the technical field of flame retardant materials, in particular to a bio-based reactive flame retardant, a flame retardant water-based polyurethane emulsion and a preparation method. Background technique [0002] With the enhancement of people's awareness of environmental protection, green and environmentally friendly bio-based flame retardants have received extensive attention. The use of bio-based materials that exist in nature as flame retardants meets the requirements of the green environmental protection strategy and is also an inevitable way to achieve sustainable development of materials. At present, materials commonly used as bio-based flame retardants include starch, chitosan, cellulose and hemicellulose, cyclodextrin, phytic acid, etc. However, natural bio-based materials have poor heat resistance and low flame retardant efficiency. Many disadvantages hinder its application in the field of flame retardants. [0003]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/117C07D251/56C07C51/41C07C59/10C08G18/38
CPCC07F9/117C07D251/56C07C51/412C08G18/3889C07C59/10
Inventor 顾丽敏史亚楠葛艳蕊薛颖超
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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