Flame retardant polynitrogen containing salt of boron compounds

Details Flame retardant polynitrogen containing salt of boron compounds Flame retardant polynitrogen containing salt of boron compounds

2000-10-20

2002-09-24

Warden, Jill (Department: 1743)

Compositions

Fire retarding

C252S609000

Reexamination Certificate

active

06454968

ABSTRACT:

FIELD
The invention concerns novel polynitrogen containing salts of polyboron oxyacids compounds. The invention also concerns their preparation and use. The use can additionally concern flame retardants compounds and compositions in which said polynitrogen containing boron compounds are employed and their preparations.
BACKGROUND
Certain useful boron compounds are known such as boric acid, orthoboric acid, metaboric acid, tetraboric acid, borax (Na
2
B
4
O
7
), kernite, calemonito, ammonium tetraborate (NH
4
HB
4
O
7
), ammonium tetraborate (NH
4
)
2
B
4
O
7
), zinc borate (Zn)
2
(B
2
O
3
)
3
which is sold under the tradename “FIREBRAKE ZB” by U.S. Borax, Inc. These boron compounds must be used with other flame retardant compounds such as phosphorus compounds or halide compounds in order to produce a satisfactory flame retardant compound. Many U.S. Patent include boron acids and their derivities utilized with another flame retardant agent such as halogen containing compounds, nitrogen containing compounds, phosphorus containing compounds and sulfur containing compounds. It is well known in the Arts that the known salts of boron compounds alone are not a satisfactory flame retardant compound whereas the novel flame retardant polynitrogen containing salts of boron oxyacid compounds are good flame retardant compounds and may be used alone. The known basic salts of boron compounds form complex, large molecule compounds by the reaction of the boron atoms reacting with the oxygen atoms on other boron radicals. These complex salts of boron oxyacid do not beak down into acid compounds which produce char which protect the flammable material. This condensation process can be prevented by the process of this invention while producing novel flame retardant polynitrogen containing salts of boron oxyacids. These complex, large molecule salts of boron compounds such as ammonium borate (NH
4
HB
4
O
7
are broken down into smaller molecules by the molecules reacting with water in the present of a strong bases such as ammonium hydroxide and at the same time the ammonia reacts with the smaller molecule of salt of boron compounds to form polyammonium salt of polyboron oxyacid. This reaction also prevents the reformation of large complex molecules when the compounds are dried. On page 637 of General Chemistry by Mebergall-Schmidt-Holtzclaw, 4th addition published by D.C. Heath and Company, Lexington, Mass., illustrates that the borate salts form large molecules in units of B
4
O—
2
, such as ammonium borate, This formation of large molecules interfere with the flame retardant properties of the known boron salts. These large complex molecules of the salts of boron compounds when heated in a flame does not break down into sufficient acidic radical which produce charring of the burning flammable material. This charring is necessary to stop the flame by forming a char over the burned area. The flame retardant polynitrogen containing boron oxyacid compounds of this invention when heated by a flame breaks down into acidic radicals which produce charring and also the nitrogen containing radical also has flame retardant properties.
SUMMARY
In one aspect, the invention comprises polynitrogen containing salts of boron oxyacids.
Another aspect of the invention is a process to prepare polynitrogen containing salts of boron oxyacids comprising serially contacting
A) boron oxide, dried boric acid and/or salts of boron compounds; 25 to 100 parts by weight;
B) nitrogen containing salt forming compounds; 25 to 100 parts by weight;
C) water, free or attached to molecules; 10 to 100 parts by weight; under conditions sufficient to prepare a polynitrogen containing salt of boron oxyacid compound. These polynitrogen containing salts of boron oxyacid compounds are useful flame retardant compounds and surfactant.
The flame retardant use comprises contacting an otherwise more flammable organic material with the polynitrogen containing salts of boron oxyacids thereof under conditions sufficient to lower the combustibility of the otherwise more flammable organic material, for example, an otherwise more combustible plastics, polyurethanes and natural products. Thus, a further aspect of the invention is a flame retardant composition comprising an otherwise more flammable organic material incorporated therewith a flame retardant amount of a polynitrogen containing salt of boron oxyacid.
Illustrature Embodiments
In general, the polynitrogen containing salt of boron oxyacids of this invention are produced utilizing boron oxide, dried boric acid and/or salts of boron oxyacids which are reacted with a strong basic compound in water such as concentrated aqueous ammonia. The large complex molecule salts of boron are broken down into smaller molecules by reacting water with one or more of the crosslinking oxygens which are then reacted with the strong basic compound to form a polynitrogen salt of boron oxyacids, such as polyammonium salt of boron oxyacids. The polynitrogen containing salts on the boron oxyacid molecules prevent the formation of large complex molecules. The ability of the polynitrogen containing salts of boron oxyacids of this invention to breakdown when heated into acidic radicals which produce a char on the flammable material along with a nitrogen containing flame retardant radical to stop the flames are improvements over the known salts of boron.
When one mol of boron oxide (B
2
O
3
) or dried boric acid are added to concentrated aqueous ammonia containing 2 or more mols of ammonia they react to produce a mixture of ammonium diborate (NH
4
)HB
2
O
5
, diammonium diborate [(NH
2
)
2
H
2
B
2
O
5
] and ammonium salt of boric acid (NH
4
BO
3
) but predominately diammonium diborate. When the mixture is dried two mols of ammonium salt of boric acid loss a mol of water and form more diammonium diborate.
When boric acid is added to an excess amount of concentrated aqueous ammonia they react to produce ammonium borate ( NH
4
BO
3
) then upon drying two moles of the ammonium borate react to form diammonium diborate.
The polynitrogen containing salt of polyboron oxyacid compounds of this invention can be represented by the general formula of
(y)
n
(M)
e
H
v
B
x
O
z
wherein y is a nitrogen containing salt forming radical, n is a number 2-4, M is a metal radical, e is a number 0-2, v is a number 0-3, x is a number 1-2 and z is a number 5-7.
The fire retardant polyammonium polyborate of this invention has the general formula of
(NH
4
)
n
H
v
B
x
O
z
wherein n is a number 2-4, v is a number 0-3, x is a number 2-4 and z is a number 3-7.
Basic salts of boron oxyacids such as monoammonium pentaborate tetrahydrate produced by U.S Borax, Inc. is broken into smaller molecules by adding it to a concentrated aqueous solution of ammonia thereby producing a polyammonium salt of a polyboron oxyacid. When zinc borate [(ZnO)
2
(B
2
O
3
)
3
trihydrate] produce by U.S. Borax, Inc, is added to an excess of concentrated aqueous ammonia the zinc borate is split into smaller molecules by water then the ammonia reacts with the molecules to produce ammonium zinc borate and polyammonium zinc borate which are good flame retardant compounds. When amino borates such as melamine borate produced by Chemie Linz is added to an excess of concentrated aqueous ammonia the melamine borate is split into smaller molecules by the addition of water then the ammonia react with these molecules. Other alkaline metal borates such as borax and alkaline earth metal borates such as calemanito will react with concentrated aqueous ammonia to produce smaller molecules of ammonium alkali metal borate, polyammonium alkali metal borate, ammonium alkaline earth metal borates or polyammonium alkaline earth metal borates.
Any suitable boron compound may be used in this invention. Suitable boron compound include, but not limited to, boron oxide, dried boric acid which was heated to remove water, boron oxyacids such as orthoboric acid, metaboric acid and tetraboric acid, metal borates, alkali metal borates, alkaline earth metal borates, ammonium borates, amine b

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