A kind of preparation method of phosphorus-nitrogen flame retardant waterborne polyurethane

A water-based polyurethane and flame retardant technology, applied in the field of functional materials, can solve the problems of decreased mechanical properties of flame retardant substrates, unfavorable dispersion by the flame retardant substrate, poor compatibility of polymers, etc., and achieves improved flame retardant properties. Effect, good flame retardant performance, good compatibility

Active Publication Date: 2021-05-28
ZHONGYUAN ENGINEERING COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Nitrogen-based flame retardants have the advantages of colorless, low toxicity, and low smoke. They do not produce corrosive gases during combustion and are inexpensive. The compatibility of materials is not good, which is not conducive to the dispersion in the flame retardant substrate, resulting in the decline of the mechanical properties of the flame retardant substrate
Silicon-containing flame retardants not only have good flame retardant effects due to their own characteristics, but also improve the mechanical properties of flame retardant substrates during use. However, the high cost greatly limits their further applications.

Method used

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  • A kind of preparation method of phosphorus-nitrogen flame retardant waterborne polyurethane
  • A kind of preparation method of phosphorus-nitrogen flame retardant waterborne polyurethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027]The method of preparing the phosphorus-nitrogen flame retardant polyurethane of the present embodiment is as follows:

[0028]S1, with a mass fraction, 13 segment tetrazaiol and 89 parts of trichlorogene phosphorus were added to a three flask, and the reflux was stirred, and at 60 ° C for 1 h, then the reaction was reacted at 105 ° C to no HCl release. The white solid product was cooled and filtered, washed with dichloromethane, then washed with anhydrous ethanol, and filtered into a 60 ° C vacuum oven dry to constant weight, and the intermediate PDD was obtained.

[0029]S2, according to the number of parts, 9 parts of S1 made of PDD, 7.2 parts of piperazine ethanol, 5.8 parts of triethylamine and 150 parts of acetonitrile, warmed to 55 ° C, reaction 8 h, magnetic stir, condensed back, then The filtration was filtered, then washed with N, N-dimethylformamide (DMF), acetone and diethyl ether were washed multiple times, and finally was dried in an oven to prepare a solid small molecu...

Embodiment 2

[0035]The method of preparing the phosphorus-nitrogen flame retardant polyurethane of the present embodiment is as follows:

[0036]S1, with a mass fraction, 13 segment tetrazaiol and 89 parts of trichlorogene phosphorus were added to a three flask, and the reflux was stirred, and at 60 ° C for 1 h, then the reaction was reacted at 105 ° C to no HCl release. The white solid product was cooled and filtered, washed with dichloromethane, then washed with anhydrous ethanol, and filtered into a 60 ° C vacuum oven dry to constant weight, and the intermediate PDD was obtained.

[0037]S2, according to the number of mass parts, 7.2 servidine ethanol, 5.8 parts of triethylamine, and 150 parts of acetonitrile, a temperature of 55 ° C, and the reaction is stirred at a temperature of 55 ° C, and the magnetic stirring is heated. The filtration was then filtered, then washed with N, N-dimethylformamide (DMF), acetone and diethyl ether were washed multiple times, and finally was dried in an oven to prep...

Embodiment 3

[0043]The method of preparing the phosphorus-nitrogen flame retardant polyurethane of the present embodiment is as follows:

[0044]S1, with a mass fraction, 39 piezulidaniol and 267 parts of trichlorophosphorus were added to a three flask, and the mixture was stirred and stirred at 60 ° C for 2 h, and then the reaction was reacted at 105 ° C to no HCl release. The white solid product was cooled and filtered, washed with dichloromethane, then washed with anhydrous ethanol, and filtered into a 60 ° C vacuum oven dry to constant weight, and the intermediate PDD was obtained.

[0045]S2, according to the number of parts, 27 parts of step 1, PDD, 21.6 parts of piperazine ethanol, 17.4 parts of triethylamine and 450 servants of acetonitrile, warmed to 55 ° C, reaction 10 h, magnetic stirring, condensed reflux, The filtration was then filtered, then washed with N, N-dimethylformamide (DMF), acetone and diethyl ether were washed multiple times, and finally was dried in an oven to prepare a solid...

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Abstract

The invention relates to a preparation method of phosphorus-nitrogen flame-retardant water-based polyurethane, comprising: reacting the product prepared after phosphorus oxychloride and pentaerythritol, and then reacting with piperazine ethanol and triethylamine to prepare a solid small molecular phosphorus -Nitrogen flame retardant; add polyether polyol, isophorone diisocyanate, and catalyst into the there-necked flask, heat, heat and stir for a period of time, then add the prepared phosphorus-nitrogen flame retardant, and continue to heat and stir for a period of time at a certain temperature time, then continuously add 2,2-dimethylolpropionic acid and 1,4-butanediol to react, then cool down to 60°C, add triethylamine to neutralize, continue stirring for 30 minutes, then add a certain amount of distilled water, and stir quickly 30min, the reaction is over. The invention prepares a reactive flame-retardant water-based polyurethane, which has good flame-retardant effect, simple synthesis method, low cost, good practicability and economy, and good market prospect.

Description

Technical field[0001]The present invention relates to a method of preparing a phosphorus-nitrogen flame retardant aqueous polyurethane having a good thermal stability, high flame retardancy, and belongs to the field of functional materials.Background technique[0002]Waterborne polyurethane is an advantage that is non-toxic, odorless, non-polluting, non-influential health, non-pollution, and does not affect human health than solvent polyurethane materials. At present, the polyurethane resin has gradually substituted solvent-type polyurethane and has become the development direction of the polyurethane industry. Waterborne polyurethane is used very widely, mainly used primarily in coatings, binders, fiber surface treatment agents, and fabric coatings. However, since the polyurethane material is very easy to combust, flame retardant treatment is performed prior to use.[0003]Improve the flame retardancy of the material, which can be introduced or added to an element having a flame retard...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/66C08G18/38C08G18/08C08G18/10C08G18/32C08G18/34C08G18/48
CPCC08G18/0823C08G18/10C08G18/3206C08G18/348C08G18/48C08G18/6692C08G18/3889
Inventor 喻国敏宋梦焦书燕贾旭李英华马明星李慧王红芳张留学
Owner ZHONGYUAN ENGINEERING COLLEGE
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