# US 10,501,602 B2 · Flame retardant and flame retardant uses

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- Number: US 10,501,602 B2
- Document ID: US10501602B2
- Status: Granted
- Kind: B2
- Application number: 15/323,960
- Filed: 2015-12-12
- Published: 2017-07-20
- Granted: 2019-12-10
- Earliest claimed: 2015-12-12
- Applicants: Robert Valentine Kasowski
- Inventors: Robert Valentine Kasowski
- Web page: https://patentgrep.com/patent/US10501602B2

## CPC

- C08K 5/521: Esters of phosphoric acids, e.g. of H3PO4
- A62C 3/0278: {by creating zones devoid of flammable material}
- C07C 209/68: from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton
- C07C 211/10: Diaminoethanes
- C07F 9/09: Esters of phosphoric acids
- C07F 9/3873: {containing nitrogen substituent, e.g. N.....H or N-hydrocarbon group which can be substituted by halogen or nitro(so), N.....O, N.....S, N.....C(=X)- (X =O, S), N.....N, N...C(=X)...N (X =O, S)}
- C08K 7/02: Fibres or whiskers
- D06M 13/322: with compounds containing nitrogen
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- A62C: FIRE-FIGHTING (fire-extinguishing compositions, use of chemical substances in extinguishing fires A62D1/00; spraying, applying liquids or other fluent materials to surfaces in general B05; alarm arrangements G08B, e.g. fire alarms actuated by smoke or gases G08B17/10)
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07F: ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM (metal-containing porphyrins C07D487/22)
- D06M: TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS

## Abstract

The flame-retardants of this invention were formed by the direct reaction of ethyleneamines and commercial polyphosphoric acid at an elevated temperature. It was unexpected that a high temperature had to be used to overcome reaction barrier to formation. These compounds are found to be efficient flame retardants.

## Claims

### Claim 1

A method for preparing sodium free ethyleneamine polyphosphate (EAPPA), the method comprising the step of reacting an ethyleneamine (EA) and polyphosphoric acid (PPA) without water or other solvent at a EA/PPA reaction ratio and at a reaction temperature so that the reaction of EA and PPA goes to completion, and wherein the EA/PPA ratio is operative such that the pH of a 10% aqueous solution by weight of the resulting EAPPA is in the range 2 to 7.5.

### Claim 2 (depends on 1)

The method according to claim 1, further comprising the step of subjecting the resulting EAPPA to subsequent condensation.

### Claim 3 (depends on 2)

The method to form sodium free ethyleneamine polyphosphate (EAPPA), as claimed in claim 2, wherein the condensation reaction of resulting EAPPA is such that thermo gravimetric analysis (TGA) weight loss of the EAPPA to 325° C. is less than 1% by weight, at a heating rate of 20° C. per minute in nitrogen atmosphere.

### Claim 4 (depends on 2)

The method to form sodium free ethyleneamine polyphosphate (EAPPA), as claimed in claim 2, wherein the condensation reaction is such that 500 g sample of the resulting EAPPA with surface area at least 25 sq. in. subjected to heating under vacuum at a temperature between 200° C. and 250° C. has a vacuum pressure less than 20 Torr for at least 15 minutes, with the vacuum system able to attain vacuum pressure of less than 5 Torr.

### Claim 5 (depends on 1)

The method to form sodium free ethyleneamine polyphosphate (EAPPA) of claim 1, wherein the reaction ratio of EA to PPA is at least 0.45 by weight of composition and the grade of PPA is PPA 105% to PPA 117%.

### Claim 6 (depends on 1)

The method according to claim 1, wherein said step of reacting comprises mixing EA and PPA in a closed container and the final temperature sufficient is to melt the formed EAPPA composition.

### Claim 7 (depends on 1, 2)

The method according to claim 1 or 2, wherein the ethyleneamine is selected from the group consisting of ethylenediamine (EDA), diethylenetriamine (DETA), piperazine (PIP), triethylenetetramine (TETA), tetraethylenepentamine (TEPA), and pentaethylenehexamine (PEHA).

### Claim 8 (depends on 1, 2)

A method for preparing an aqueous solution, the aqueous solution comprises the sodium free EAPPA prepared according to the method of claim 1 or 2 at a ratio of at least 20% by weight.

### Claim 9 (depends on 8)

The method for containing or fighting fires of claim 8 wherein said step of applying comprises spraying the aqueous solution on to surfaces of fuel in front of the fire in a quantity or form that is operative to wet at least 25% of the surface at a thickness of at least 0.25 mil.

### Claim 10 (depends on 8)

The method for containing or fighting fires of claim 8 wherein the quantity or form of the aqueous solution is operative to wet wooden surface to stop the formation of embers and reduce the amount of heat released.

### Claim 11 (depends on 8)

A method for decreasing the heat flux that a wood emits comprising coating the wood with the aqueous solution prepared according to the method of claim 8 at a thickness of the aqueous solution of at least 1 mil.

### Claim 12 (depends on 1, 2)

A method for preparing an aqueous solution comprising adding water and mixing after the reaction of EA and PPA goes to completion in the method of claim 1 or 2.