CN110078886A - A kind of preparation method of phosphorus-nitrogen extinguishing waterborn polyurethane - Google Patents
A kind of preparation method of phosphorus-nitrogen extinguishing waterborn polyurethane Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/0804—Manufacture of polymers containing ionic or ionogenic groups
- C08G18/0819—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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Abstract
The present invention relates to a kind of phosphorus-nitrogen extinguishing waterborn polyurethane preparation methods, comprising: the product that will be prepared after phosphorus oxychloride and pentaerythrite reaction, then reacted with piperazine ethanol, triethylamine, prepare a kind of solid small molecule phosphorus-nitrogen combustion inhibitor；There-necked flask is added in polyether polyol, isophorone diisocyanate, catalyst, heating and thermal insulation stirring a period of time, then phosphorus-the nitrogen combustion inhibitor prepared is added, continues insulated and stirred for a period of time at a certain temperature, is then continuously added 2 again, 2- dihydromethyl propionic acid, 1,60 DEG C are cooled to after the reaction of 4- butanediol, triethylamine is added and neutralizes, a certain amount of distilled water is added after persistently stirring 30min, quickly stirring 30min, reaction terminate.The present invention has prepared a kind of extinguishing waterborn polyurethane of response type, and good flame retardation effect, synthetic method is simple, cost is relatively low, there is good practicability and economy, has good market prospects.
Description
Technical field
The present invention relates to a kind of phosphorus-nitrogen extinguishing waterborn polyurethane preparation method, have that thermal stability is good, anti-flammability is high
Feature belongs to field of functional materials.
Background technique
Aqueous polyurethane is one kind using water as medium polyurethane material, compared with solvent polyurethane, with nontoxic, tasteless,
No pollution to the environment, the advantages that not influencing the health of people.Currently, polyurethane resin aqueousization gradually replaces solvent type
Polyurethane becomes the developing direction of polyurethane industries among others.Aqueous polyurethane is very widely used, be mainly used at present coating,
Adhesive, fiber surface treatment agent and fabric coating etc..But since polyurethane material is very easy to burning, make
With preceding carrying out flame retardant treatment.
The flame retardant property for improving material, can wherein introduce or be added some elements with flame retardant effect or its chemical combination
Object.Common fire retardant can be divided into inorganic fire retardants and organic fire-retardant two major classes.Inorganic fire retardants, such as magnesium hydroxide, hydrogen-oxygen
Change aluminium etc., has many advantages, such as that thermal stability is good, non-volatile, effect is lasting, cheap.But they are deposited in use
Loading it is big, with substrate binding force is small, poor compatibility the disadvantages of, can processing to material and mechanical property cause unfavorable shadow
It rings.Halogenated flame retardant in organic fire-retardant is because its efficient flame retardant effect is using than wide, and still, halogenated flame retardant is firing
A large amount of poison gas can be released during burning, bring more serious secondary injury.Fire retardant mostly uses halogen-free flameproof at present
Agent is primarily referred to as the compound containing ignition-proof elements such as phosphorus, nitrogen, silicon.Nitrogenated flame retardant has many advantages, such as colourless, less toxic, low cigarette,
Corrosive gas and cheap is not generated in combustion process, still, flame retardant effect is bad when this based flame retardant is used alone, and
It is bad with the compatibility of some high polymers, it is unfavorable for by the dispersion in ignition resistant substrate, under the mechanical performance for causing ignition resistant substrate
Drop.Silicone-containing Flame Retardant can also improve fire-retardant base because the characteristic of itself not only has good flame retardant effect in use
The mechanical performance of material, however, expensive cost strongly limits its further application.And phosphorus flame retardant is each based flame retardant
In it is most complicated, be also that research is relatively adequately a kind of, have many advantages, such as that low toxicity, low cigarette, environmental protection, flame retarding efficiency be high and additive amount less,
Meet the developing direction of fire retardant, there is good development prospect.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention proposes a kind of preparation method of phosphorus-nitrogen extinguishing waterborn polyurethane,
Phosphorus obtained-nitrogen extinguishing waterborn polyurethane have flame retardant property is good, thermal stability is high, carbon yield is high, add it is a certain amount of fire-retardant
Agent has the characteristic of easy self-extinguishment after fire retardant or burning.
The technical scheme of the present invention is realized as follows:
A kind of preparation method of phosphorus-nitrogen extinguishing waterborn polyurethane, including following step are poly-:
S1, mass fraction is pressed, there-necked flask is added in 13-39 parts of pentaerythrites and 89-267 parts of phosphorus oxychloride, is heated to reflux stirring,
1-2h is reacted at 60 DEG C, until 7-10h to no HCl releasing is then reacted at 105 DEG C, cooling filters to obtain white solid product,
It is first washed with methylene chloride, then is washed with dehydrated alcohol, it is dry to constant weight, obtained intermediate that 60 DEG C of vacuum drying ovens are put into after suction filtration
PDD；
S2, press mass fraction, by PDD, 7.2-21.6 parts of piperazine ethanols made from 9-27 parts of S1,5.8-17.4 parts of triethylamines and
There-necked flask is added in 150-450 parts of acetonitriles, is warming up to 55 DEG C, reacts 8-10h, and magnetic agitation is condensed back, then filters, then use
The repeatedly washing respectively of n,N-Dimethylformamide (DMF) washing, acetone and ether, is finally putting into oven drying, is made a kind of solid
Body small molecule phosphorus-nitrogen combustion inhibitor；
S3, by polyether polyol, isophorone diisocyanate, dihydromethyl propionic acid, 1,4-butanediol, di lauric dibutyl
Phosphorus-nitrogen combustion inhibitor vacuum dehydration of tin and S2 preparation；
S4, mass fraction is pressed, by 15-45 part polyether polyol after S3 vacuum dehydration, 14.5-43.5 parts of isophorones two
There-necked flask is added in isocyanates, 1.5-4.5 part dibutyl tin dilaurate (catalyst), is heated to 80 DEG C of insulated and stirred reaction 2-
Then 3h is added 1.5-11 parts of phosphorus-nitrogen combustion inhibitors, continues insulated and stirred 1-2h at 80 DEG C, then add 0.9-2.7 part 2,2-
Dihydromethyl propionic acid after reacting 1-1.5h, is cooled to 60 DEG C after 3 parts of 1,4-butanediol of 0- the reaction was continued 0.5-1h is added, is added
Then 0.6-1.8 parts of triethylamine neutralization reaction 0.5-1h are added 30-90 parts of distilled water, quickly stir 30min, reaction terminates；
S5, S4 reaction solution obtained is poured on ready polyfluortetraethylene plate in advance, room temperature 1d, then in an oven
2d is dried at 40 DEG C, obtains phosphorus-nitrogen extinguishing waterborn polyurethane.
Sharp phosphorus-nitrogen extinguishing waterborn polyurethane obtained with the aforedescribed process.
The phosphorus-nitrogen extinguishing waterborn polyurethane highest phosphorus content is 1.3%, nitrogen content 1.2%.
Beneficial effects of the present invention: the present invention proposes a kind of phosphorus-nitrogen extinguishing waterborn polyurethane, using phosphorus oxychloride and season penta
Tetrol reaction, the product of preparation react that prepare a kind of solid small with piperazine ethanol, triethylamine in the case where acetonitrile is solvent condition again
Molecular phosphorus-nitrogen combustion inhibitor, finally using phosphorus-nitrogen combustion inhibitor of preparation as a kind of small molecule chain extender and polyether polyol, different Buddhist
A kind of intrinsically flame retarded aqueous poly- ammonia is made in that ketone diisocyanate, butanediol and 2, the substance reactions such as 2- dihydromethyl propionic acid
Ester, the flame retardant property of last test aqueous polyurethane have many advantages, such as that flame retardant property is good, thermal stability is high and carbon yield is high.
The present invention synthesizes a kind of solid small molecule compound phosphorus-nitrogen combustion inhibitor, and it is good with substrate compatibility to have, and is not easy to move
The advantages that shifting, decomposition temperature with higher are added in polyurethane material as fire retardant, can greatly improve polyurethane material
The temperature of initial decomposition of material can effectively improve the flame retardant effect of polyurethane material.
Detailed description of the invention
Fig. 1 is extinguishing waterborn polyurethane thermal multigraph.
Specific embodiment
Combined with specific embodiments below, the present invention will be further described.It should be understood that following embodiment is merely to illustrate this
The person skilled in the art of the range of invention and is not intended to limit the present invention, the field can make one according to the content of foregoing invention
A little nonessential modifications and adaptations.
Comparative example 1
A kind of phosphorus-nitrogen extinguishing waterborn polyurethane preparation method that this comparative example proposes, steps are as follows:
S1, mass fraction is pressed, there-necked flasks is added in 13 parts of pentaerythrites and 89 parts of phosphorus oxychloride, be heated to reflux stirring, at 60 DEG C
1h is reacted, until 7h to no HCl releasing is then reacted at 105 DEG C.Cooling filters to obtain white solid product, first uses methylene chloride
Washing, then washed with dehydrated alcohol, it is dry to constant weight, obtained intermediate PDD that 60 DEG C of vacuum drying ovens are put into after suction filtration；
S2, mass fraction is pressed, PDD made from 9 parts of steps 1,7.2 parts of piperazine ethanols, 5.8 parts of triethylamines and 150 parts of acetonitriles is added
Enter there-necked flask, be warming up to 55 DEG C, react 8h, magnetic agitation is condensed back, then filters, then use n,N-Dimethylformamide
(DMF) washing, acetone and ether repeatedly washing respectively, is finally putting into oven drying, it is fire-retardant that a kind of solid small molecule phosphorus-nitrogen is made
Agent；
S3, by phosphorus-nitrogen combustion inhibitor of preparation, polyether polyol, isophorone diisocyanate, dihydromethyl propionic acid, Isosorbide-5-Nitrae-fourth
Two pure and mild dibutyl tin dilaurate vacuum dehydrations；
S4, mass fraction is pressed, by S3 treated 15 parts of polyether polyol, 14.5 parts of isophorone diisocyanate, 1.5 parts
There-necked flask is added in catalyst, is heated to 80 DEG C of insulated and stirreds reaction 2h, is then added 0.75 part of phosphorus-nitrogen combustion inhibitor, at 80 DEG C after
Continuous insulated and stirred 1h, then adds 0.9 part of 2,2- dihydromethyl propionic acid, after reacting 1h, 2 parts of 1,4-butanediol is added and continue instead
60 DEG C are cooled to after answering 0.5h, 0.6 part of triethylamine neutralization reaction 0.5h is added, 30 parts of distilled water are then added, quickly stir
30min, reaction terminate；
S5, S4 reaction solution obtained is poured on ready polyfluortetraethylene plate in advance, room temperature 1d, then in an oven
2d is dried at 40 DEG C, obtains phosphorus-nitrogen extinguishing waterborn polyurethane.
Phosphorus made from this comparative example-nitrogen extinguishing waterborn polyurethane phosphorus-nitrogen combustion inhibitor content (wt%) is 2%.
Embodiment 1
The phosphorus of the present embodiment-nitrogen extinguishing waterborn polyurethane the preparation method is as follows:
S1, mass fraction is pressed, there-necked flasks is added in 13 parts of pentaerythrites and 89 parts of phosphorus oxychloride, be heated to reflux stirring, at 60 DEG C
1h is reacted, until 7h to no HCl releasing is then reacted at 105 DEG C.Cooling filters to obtain white solid product, first uses methylene chloride
Washing, then washed with dehydrated alcohol, it is dry to constant weight, obtained intermediate PDD that 60 DEG C of vacuum drying ovens are put into after suction filtration；
S2, mass fraction is pressed, PDD made from 9 parts of S1,7.2 parts of piperazine ethanols, 5.8 parts of triethylamines and 150 parts of acetonitriles is added three
Mouth bottle, is warming up to 55 DEG C, reacts 8h, and magnetic agitation is condensed back, then filters, then washed with n,N-Dimethylformamide (DMF)
It washs, the repeatedly washing respectively of acetone and ether, is finally putting into oven drying, a kind of solid small molecule phosphorus-nitrogen combustion inhibitor is made；
S3, by phosphorus-nitrogen combustion inhibitor of preparation, polyether polyol, isophorone diisocyanate, dihydromethyl propionic acid, Isosorbide-5-Nitrae-fourth
Two pure and mild dibutyl tin dilaurate vacuum dehydrations；
S4, mass fraction is pressed, by S3 treated 15 parts of polyether polyol, 14.5 parts of isophorone diisocyanate, 1.5 parts
There-necked flask is added in catalyst, is heated to 80 DEG C of insulated and stirred reaction 2h, 1.5 parts of phosphorus-nitrogen combustion inhibitors are then added, continue at 80 DEG C
Insulated and stirred 1h then adds 0.9 part of 2,2- dihydromethyl propionic acid, after reacting 1h, 1.8 parts of 1,4-butanediol is added and continue instead
60 DEG C are cooled to after answering 0.5h, 0.6 part of triethylamine neutralization reaction 0.5h is added, 30 parts of distilled water are then added, quickly stir
30min, reaction terminate;
S5, S4 reaction solution obtained is poured on ready polyfluortetraethylene plate in advance, room temperature 1d, then in an oven
2d is dried at 40 DEG C, obtains phosphorus-nitrogen extinguishing waterborn polyurethane.
Phosphorus made from the present embodiment-nitrogen extinguishing waterborn polyurethane phosphorus-nitrogen combustion inhibitor content (wt%) is 4%.
Embodiment 2
The phosphorus of the present embodiment-nitrogen extinguishing waterborn polyurethane the preparation method is as follows:
S1, mass fraction is pressed, there-necked flasks is added in 13 parts of pentaerythrites and 89 parts of phosphorus oxychloride, be heated to reflux stirring, at 60 DEG C
1h is reacted, until 7h to no HCl releasing is then reacted at 105 DEG C.Cooling filters to obtain white solid product, first uses methylene chloride
Washing, then washed with dehydrated alcohol, it is dry to constant weight, obtained intermediate PDD that 60 DEG C of vacuum drying ovens are put into after suction filtration；
S2, mass fraction is pressed, PDD made from 9 parts of steps 1,7.2 parts of piperazine ethanols, 5.8 parts of triethylamines and 150 parts of acetonitriles is added
Enter there-necked flask, be warming up to 55 DEG C, react 8h, magnetic agitation is condensed back, then filters, then use n,N-Dimethylformamide
(DMF) washing, acetone and ether repeatedly washing respectively, is finally putting into oven drying, it is fire-retardant that a kind of solid small molecule phosphorus-nitrogen is made
Agent；
S3, by phosphorus-nitrogen combustion inhibitor of preparation, polyether polyol, isophorone diisocyanate, dihydromethyl propionic acid, Isosorbide-5-Nitrae-fourth
Two pure and mild dibutyl tin dilaurate vacuum dehydrations；
S4, mass fraction is pressed, S3 treated 15 parts of polyether polyol, 14.5 parts of isophorone diisocyanate, 1.5 parts is urged
There-necked flask is added in agent, is heated to 80 DEG C of insulated and stirred reaction 2h, 2.25 parts of phosphorus-nitrogen combustion inhibitors are then added, continue at 80 DEG C
Insulated and stirred 1.5h then adds 0.9 part of 2,2- dihydromethyl propionic acid, after reacting 1h, 1.4 parts of 1,4-butanediol is added and continue
60 DEG C are cooled to after reaction 0.5h, 0.6 part of triethylamine neutralization reaction 0.5h is added, 30 parts of distilled water are then added, quickly stir
30min, reaction terminate.
S5, S4 reaction solution obtained is poured on ready polyfluortetraethylene plate in advance, room temperature 1d, then dried
2d is dried at 40 DEG C in case, obtains phosphorus-nitrogen extinguishing waterborn polyurethane.
Phosphorus made from the present embodiment-nitrogen extinguishing waterborn polyurethane phosphorus-nitrogen combustion inhibitor content (wt%) is 6%.
Embodiment 3
The phosphorus of the present embodiment-nitrogen extinguishing waterborn polyurethane the preparation method is as follows:
S1, mass fraction is pressed, there-necked flasks is added in 39 parts of pentaerythrites and 267 parts of phosphorus oxychloride, be heated to reflux stirring, at 60 DEG C
2h is reacted, until 10h to no HCl releasing is then reacted at 105 DEG C.Cooling filters to obtain white solid product, first uses dichloromethane
Alkane washing, then washed with dehydrated alcohol, it is dry to constant weight, obtained intermediate PDD that 60 DEG C of vacuum drying ovens are put into after suction filtration；
S2, mass fraction is pressed, by PDD made from 27 parts of steps 1,21.6 parts of piperazine ethanols, 17.4 parts of triethylamines and 450 parts of acetonitriles
There-necked flask is added, is warming up to 55 DEG C, reacts 10h, magnetic agitation is condensed back, then filters, then use n,N-Dimethylformamide
(DMF) washing, acetone and ether repeatedly washing respectively, is finally putting into oven drying, it is fire-retardant that a kind of solid small molecule phosphorus-nitrogen is made
Agent；
S3, by phosphorus-nitrogen combustion inhibitor of preparation, polyether polyol, isophorone diisocyanate, dihydromethyl propionic acid, Isosorbide-5-Nitrae-fourth
Two pure and mild dibutyl tin dilaurate vacuum dehydrations；
S4, mass fraction is pressed, S3 treated 45 parts of polyether polyol, 43.5 parts of isophorone diisocyanate, 4.5 parts is urged
There-necked flask is added in agent, is heated to 80 DEG C of insulated and stirred reaction 3h, 8 parts of phosphorus-nitrogen combustion inhibitors are then added, continue to keep the temperature at 80 DEG C
2h is stirred, 2.7 parts of 2,2- dihydromethyl propionic acids are then added, 0.314 part of 1,4-butanediol continuation is added instead after reacting 1.5h
60 DEG C are cooled to after answering 0.5h, 1.8 parts of triethylamine neutralization reaction 1h are added, 90 parts of distilled water are then added, quickly stir
30min, reaction terminate；
S5, S4 reaction solution obtained is poured on ready polyfluortetraethylene plate in advance, room temperature 1d, then in an oven
2d is dried at 40 DEG C, obtains phosphorus-nitrogen extinguishing waterborn polyurethane.
Phosphorus made from the present embodiment-nitrogen extinguishing waterborn polyurethane phosphorus-nitrogen combustion inhibitor content (wt%) is 8%.
Embodiment 4
The phosphorus of the present embodiment-nitrogen extinguishing waterborn polyurethane the preparation method is as follows:
S1, mass fraction is pressed, there-necked flasks is added in 39 parts of pentaerythrites and 267 parts of phosphorus oxychloride, be heated to reflux stirring, at 60 DEG C
2h is reacted, until 10h to no HCl releasing is then reacted at 105 DEG C.Cooling filters to obtain white solid product, first uses dichloromethane
Alkane washing, then washed with dehydrated alcohol, it is dry to constant weight, obtained intermediate PDD that 60 DEG C of vacuum drying ovens are put into after suction filtration；
S2, mass fraction is pressed, by PDD made from 27 parts of steps 1,21.6 parts of piperazine ethanols, 17.4 parts of triethylamines and 450 parts of acetonitriles
There-necked flask is added, is warming up to 55 DEG C, reacts 10h, magnetic agitation is condensed back, then filters, then use n,N-Dimethylformamide
(DMF) washing, acetone and ether repeatedly washing respectively, is finally putting into oven drying, it is fire-retardant that a kind of solid small molecule phosphorus-nitrogen is made
Agent；
S3, by phosphorus-nitrogen combustion inhibitor of preparation, polyether polyol, isophorone diisocyanate, dihydromethyl propionic acid, Isosorbide-5-Nitrae-fourth
Two pure and mild dibutyl tin dilaurate vacuum dehydrations；
S4, mass fraction is pressed, S3 treated 45 parts of polyether polyol, 43.5 parts of isophorone diisocyanate, 4.5 parts is urged
There-necked flask is added in agent, is heated to 80 DEG C of insulated and stirred reaction 3h, then 11 parts of phosphorus-nitrogen combustion inhibitors of addition, after continuation of insurance at 80 DEG C
Temperature stirring 2h, then adds 2.7 parts of 2,2- dihydromethyl propionic acids, is cooled to 60 DEG C after reacting 1.5h, 1.8 parts of triethylamines are added
Then neutralization reaction 1h is added 90 parts of distilled water, quickly stirs 30min, reaction terminates；
S5, S4 reaction solution obtained is poured on ready polyfluortetraethylene plate in advance, room temperature 1d, then in an oven
2d is dried at 40 DEG C, obtains phosphorus-nitrogen extinguishing waterborn polyurethane.
Phosphorus made from the present embodiment-nitrogen extinguishing waterborn polyurethane phosphorus-nitrogen combustion inhibitor content (wt%) is 10%.
The test of 1 phosphorus of table-nitrogen extinguishing waterborn polyurethane flame retardant property
As it can be seen from table 1 extinguishing waterborn polyurethane fire retardant prepared by the present invention has good anti-flammability when a certain amount of
Can, molten drop will not ignite combustibles when burning.When fire retardant additive amount is 2%, do not have flame retardant effect, fire retardant additive amount is got over
The flame retardant effect of the extinguishing waterborn polyurethane more prepared is better.
It is mainly step burning that the thermal multigraph of two groups of aqueous flame retardant polyurethane, which can be seen that combustion process, in Fig. 1,
Conflagration at 250-370 DEG C, at this time material mass variation are very fast.Extinguishing waterborn polyurethane material burning after carbon left compared with
The burning of height, fire proofing can generate one layer of fine and close protective film in substrate surface, play good flame retardant effect to material.Resistance
Carbon left is more after firing the extinguishing waterborn polyurethane burning more than agent additive amount, therefore has better flame retardant effect.
Basic principles and main features and advantages of the present invention of the invention have been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (3)
1. a kind of phosphorus-nitrogen extinguishing waterborn polyurethane preparation method, which is characterized in that poly- including following step:
S1, mass fraction is pressed, there-necked flask is added in 13-39 parts of pentaerythrites and 89-267 parts of phosphorus oxychloride, is heated to reflux stirring,
1-2h is reacted at 60 DEG C, until 7-10h to no HCl releasing is then reacted at 105 DEG C, cooling filters to obtain white solid product,
It is first washed with methylene chloride, then is washed with dehydrated alcohol, it is dry to constant weight, obtained intermediate that 60 DEG C of vacuum drying ovens are put into after suction filtration
PDD；
S2, press mass fraction, by PDD, 7.2-21.6 parts of piperazine ethanols made from 9-27 parts of S1,5.8-17.4 parts of triethylamines and
There-necked flask is added in 150-450 parts of acetonitriles, is warming up to 55 DEG C, reacts 8-10h, and magnetic agitation is condensed back, then filters, then use
The repeatedly washing respectively of n,N-Dimethylformamide (DMF) washing, acetone and ether, is finally putting into oven drying, and phosphorus-nitrogen resistance is made
Fire agent；
S3, by polyether polyol, isophorone diisocyanate, dihydromethyl propionic acid, 1,4-butanediol, di lauric dibutyl
Phosphorus-nitrogen combustion inhibitor vacuum dehydration of tin and S2 preparation；
S4, mass fraction is pressed, by 15-45 part polyether polyol after S3 vacuum dehydration, 14.5-43.5 parts of isophorones two
There-necked flask is added in isocyanates, 1.5-4.5 parts of dibutyl tin dilaurates, is heated to 80 DEG C of insulated and stirred reaction 2-3h, then
1.5-11 parts of phosphorus-nitrogen combustion inhibitors are added, continues insulated and stirred 1-2h at 80 DEG C, then adds 0.9-2.7 part 2,2- dihydroxy first
Base propionic acid after reacting 1-1.5h, is cooled to 60 DEG C after 3 parts of 1,4-butanediol of 0- the reaction was continued 0.5-1h is added, 0.6- is added
Then 1.8 parts of triethylamine neutralization reaction 0.5-1h are added 30-90 parts of distilled water, quickly stir 30min, reaction terminates；
S5, S4 reaction solution obtained is poured on ready polyfluortetraethylene plate in advance, room temperature 1d, then in an oven
2d is dried at 40 DEG C, obtains phosphorus-nitrogen extinguishing waterborn polyurethane.
2. utilizing phosphorus-nitrogen extinguishing waterborn polyurethane made from method described in claim 1.
3. phosphorus according to claim 2-nitrogen extinguishing waterborn polyurethane is it is characterized by: the phosphorus-poly- ammonia of nitrogen extinguishing waterborn
The highest phosphorus content of ester is 1.3%, nitrogen content 1.2%.
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