US 5,089,559 AGrant
Fire-Retardant Organic-Phosphorus Salts
Issue Date:1992-02-18
•9 Claims
Abstract
Fire retardant salts of organic-phosphorus acid compounds are produced by mixing and reacting an organic compound with an acidic salt-forming phosphorus compound to produce an organic-phosphorus acidic compound which is then reacted with a salt-forming basic compound. These fire retardant compounds are mixed with plastics to produce fire retardant plastics.
Metadata
Inventor
- David H. Blount
Application Information
Application Number:US 6096379
Filing Date:1990-11-06
Priority Date:1989-02-13
Art Unit:153
Classifications
IPC:
C08F 840C08L 8502C08F 8504
Field of Search:
525107;123;134;165;177;187;190;326.1;327.3;327.6;332.1;437;418;452;480;509;538
Patent Drawings
This patent does not have any drawings.
Description
Description of Preferred Embodiments
My invention will be illustrated in greater detail in the specific examples which follow, which detail the preferred embodiment of my process. It should be understood that the scope of my invention is not limited to the specific processes set out in the examples. Parts and percentages are by weight unless otherwise indicated.
Example 1
About 20 parts by weight of a propylene oxide 20 parts by weight of 75% phosphoric acid are slowly mixed then agitated for about 30-40 minutes thereby producing an acidic propylene phosphate with free acid radicals, then 20 parts by weight of urea are admixed and heated while agitated until the urea melts thereby producing a fire-retardant urea salt of propylene phosphate.
Example 2
About 40 parts by weight of melamine and 20 parts by weight of 80% phosphoric acid are mixed and agitated for about one hour, then 20 parts by weight of urea are admixed then heated while agitating until the urea melts thereby producing a fire-retardant urea salt of melamine phosphate.
Example 3
About 100 parts by weight of a liquid phenol-formaldehyde resin produced with an alkali catalyst and 15 parts by weight of 75% phosphoric acid are added then agitated at ambient temperature for about one hour then 20 parts weight of melamine are added while agitated, the mixture reacts thereby producing a fire-retardant resin, melamine salt of phenol-formaldehyde phosphate.
Example 4
80 parts by weight of phenol containing 10% water is mixed with 10 parts by weight of phosphorus oxide while agitating for about one hour the 10 parts by weight of urea are added. The mixture is heated while agitating until the urea melts thereby producing a fire-retardant urea salt of phenol phosphate.
Example 5
Example 4 is modified wherein another phosphorus compound is used in place of phosphorus oxide and selected from the group below:
a) phosphorus trichloride
b) phosphoric acid
c) polyphosphoric acid
d) pyrophosphoric acid
e) phosphorus oxychloride
Example 6
Example 1 is modified wherein another organic compound is used in place of propylene oxide and selected from the list below:
a) glycerine
b) sawdust
c) sucrose polyol (hydroxyl no. 380)
d) polyester polyol
e) propylene glycol
f) liquid polyamide
g) polyepoxy resin (Bisphenol A epoxy resin)
h) polypropylene glycol epoxy resin
i) p-amine phenol epoxy resin
j) maleic anhydride-adipic acid-diethylene, glycol-methyl methacrylate polyester resin
k) poly (furfural) polymer
e) fumaric acid-propylene glycol-styrene polyester resin
m) poly (methyl acrylic acid) resin
n) poly epichlorohydrin
o) poly (acetone-fufural) polymer
p) poly (allyl alcohol) polymer
q) poly (formaldehyde-urea) resin
r) diethylenetriamine fatty acid condensation product
s) poly (formaldehyde-melamine) resin
t) poly (vinylacetate - vinyl alcohol) resin
u) vinyl acetate-ethylene copolymer emulsion
v) poly (methyl methacrylate-acrylic acid) polymer
w) starch
x) sucrose
y) butylene oxide
Example 7
Example 1 is modified wherein another basic salt forming compound is used in place of urea and selected from the group below:
a) melamine
b) sodium silicate
c) talc
d) zinc oxide
e) aluminum hydroxide
f) aluminum powder
g) ammonium silicate
h) ammonium borate
i) diethylenetriamine
j) ethylene amine
k) polyamide with free amine radicals
l) aqueous ammonia
m) potassium carbonate
n) antimony oxide
o) magnesium
p) sodium borax
q) urea-formaldehyde resin
r) cyanurdiamide
s) cyanuramide
t) dicyandiamide
u) ammonium acetate
v) ammonium oxalate
w) ammonium carbonate
x) quaternary ammonium hydroxide
y) ethylene amine
z) ammonium polyphosphate
Example 8
About 5 parts by weight of polyepoxy resin (Bisphenol A epoxy resin) and 4 parts by weight of 75% phosphoric acid was slowly admixed while agitating for 20-30 minutes, then 5 parts by weight of melamine was added and agitated about 10 minutes, then 15 parts by weight of the polyepoxy resin was admixed, then 5 parts by weight of an amine epoxy catalyst was admixed. The resin solidified and was flame tested after 24 hours. The solid resin was subject to a 1/2" propane torch flame for about 2 minutes. The superficial layer of the plastic burned and formed a char. The flame did not spread and went out as soon as the torch was removed.
Example 9
Example 8 was modified wherein another polyepoxy resin was used in place of and selected from the list below:
a) phenol novalac epoxy resin
b) triphenylol epoxy resin
c) methylene dramiline epoxy resin
d) p-amino phenol epoxy resin
e) dimer acid epoxy resin
f) mixtures thereof
Example 10
About 30 parts by weight of a polyvinyl acetate emulsion and 4 parts by weight of phosphoric acid are mixed slowly and agitated for about 30-40 minutes, then 4 parts by weight of melamine is added and thoroughly mixed. The mixture was poured into a polyethylene sheet and allowed to dry for 24 hours. The flame resistant plastic was then tested by placing a 1/2" propane torch flame on the material for about 2 minutes. A char was produced on the surface and the flame did not spread. The flame went out as soon as the torch was removed.
Example 11
Example 10 is modified wherein another resin is used in place of polyvinyl acetate and selected from the list below and gives
a) poly(vinylacetate-ethylene) copolymer
b) poly(vinyl acetate-vinyl alcohol) resin
c) poly(allyl alcohol) resin
d) poly(vinyl chloride-vinyl acetate) emulsion
e) poly(vinyl chloride-acrylonitrile) emulsion
f) Polyvinyl-alcohol emulsion
g) poly(vinyl acetate formaldehyde) emulsion
h) poly(acrylic acid) emulsion
i) poly(methacrylic acid) emulsion
j) poly(methacrylic acid-acrylic acid) emulsion
k) poly(butadiene-styrene) emulsion
l) liquid phenol-formaldehyde resin
m) liquid urea-formaldehyde resin
n) liquid melamine-Formaldehyde resin
o) hydroxyethyl cellulose emulsion
p) starch emulsion
q) poly(butadiene-acrylonitrile) emulsion
r) poly(butadiene-styrene) emulsion
s) polybutadiene resin (hydroxyl No. 466)
t) polybutadiene-styrene resin (hydroxyl No. 365)
Example 12
About 100 parts by weight of a meltable plastic selected from the list below and 20 parts by weight of the flame-retardant compound produced in Example 1 are mixed then heated to until the plastic melts and then the flame-retardant compound is thoroughly mixed in the melted plastic. The mixture is poured into a mold wherein the plastic is about one-eight of an inch thick and cooled. The solidified plastic is then tested with a 1/2" propane torch flame for about 1 minute and on removal of the torch the flame goes out and it does not spread.
a) polystyrene
b) polyethylene
c) polypropylene
d) polyester
e) polyamide
f) polyurethane
g) polyvinyl chloride
h) polymethyl methacrylate
i) polybutylene
Example 13
About 20 parts by weight of 30% formaldehyde in water and 10 parts by weight of 75% phosphoric acid are mixed together then 10 parts by weight of urea are added and the mixture reacts to produce fire-retardant urea salt of urea formaldehyde phosphate resin. The resin is mixed with 80 parts by weight of saw dust, then 10 parts by weight of an alkali catalytized urea-formaldehyde syrup are thoroughly mixed then packed into a mold under pressure. The resin hardens to form a sawdust panel.
The sawdust panel was treated with a propane torch with a 1/2" flame for 2 minutes. The flamed area formed a char and the flame did not spread.
Example 14
Example 13 is modified wherein an alkali catalytized phenel-formaldehyde resin syrup is used in place of the alkali catalytized urea-formaldehyde syrup. The sawdust panel is cured under heat and pressure. This panel was tested with a propane torch with a 1/2" flame for 2 minutes. The flamed area formed a char and the flame did not spread.
Example 15
Example 13 is modified wherein melamine is used in place of urea to produce fire-retardant melamine-formaldehyde phosphate resin then utilized in Example 13 in place of the urea-formaldehyde phosphate resin.
Example 16
Example 1 is modified wherein a basic salt of a boron compound is used in place of urea and selected from the list below:
a) potassium borate
b) sodium borate
c) ammoniun borate
d) zinc borate
e) urea borate
f) diethylene amine borate
g) ethyl amine borate
h) calcium borate
Although specific materials and conditions were set forth in the above examples, these are merely illustrative of preferred embodiments of my invention. Various other compositions, such as the typical materials listed above may be used where suitable. The reactive mixtures and products of my invention may have other agents added hereto enhance or otherwise modify the reaction and products.
Other modifications of my invention will occur to those skilled in the Art upon reading my disclosure. These are intended to be included within the range of my invention as defined in the appended claims.
Claims
I claim:
1. A fire retardant plastic comprising a plastic resin composition combined with a slat of an organic-phosphorus acid compound, wherein the said salt is produced by mixing and reacting the following components: A) organic compound that will react with a phosphorus acid compound in the amount of 100 parts by weight and selected from the group consisting of polyols, polyester, polyamides, polyepoxy, alcohols, polyethers, polycarboxyl, phenoplasts, aminoplasts, amines, polyamines, polythioesters, polyacetols, polycabonates, silicones, vegetable oils, ketones, aldehydes, epoxides, organic acids, cellulose, vinyl polymers, vinyl co-polymers, vinyl-diene co-polymers, diene polymers, polyimides, polyesteramides, organic borates and mixtures thereof; B) acidic salt forming compound of phosphorus in the amount of 5 to 100 parts by weight; C) salt forming basic compound in the amount of 1 to 200 parts by weight; the said mixing is carried in such a way that component A and B are reacted first to produce an organic-phosphorus acid compound then component C is reacted with the organic-phosphorus acid compound.
2. The fire retardant plastic of claim 1 wherein the plastic resin composition is combined with 5% to 100% by weight of the salt of an organic-phosphorus acid compound.
3. The fire retardant plastic of claim 1 wherein the acidic salt forming compounds of phosphorus is selected from the group consisting of phosphoric acid, phosphinic acid, phosphinous acid, phosphine oxide, phosphorus trichloride, alkylchlorophosphines, organic acid phosphates, phosphorus oxychloride, monoaluminum phosphate, dihydrogen containing salts of phosphoric acid, hypophosphorus acid, polyphosphoric acid, pyrophosphoric acid and mixtures thereof.
4. The fire retardant plastic of claim 1 wherein the salt forming basic compound is selected from the group consisting of alkali metal compounds, alkaline earth metal compounds, metal compounds, ammonia compounds, compounds containing ammonium radicals, amino compounds, amine and mixtures thereof.
5. The fire retardant plastic of claim 4 wherein the ammonia compound is selected from the group consisting of ammonia, urea, alkylurea, dicyandiamide, melamine, guanidine, aminoguanidine and mixtures thereof.
6. A fire retardant plastic produced by mixing and reacting the following components: A. A solid organic plastic that will react with a phosphorus acid compound in the amount of 100 parts by weight; B. Acidic salt forming compound of phosphorus in the amount of 5 to 100 parts by weight; C. Salt-forming basic compound in the amount of 1 to 200 parts by weight; the said mixture is carried out in such a way that component B reacts with components A and C.
7. A process for the production of a fire-retardant plastic comprising a plastic resin composition combined with a fire retardant salt of an organic phosphorus acid compound, wherein the said salt is produced by mixing and reacting the following components: A) Organic compound that will react with a phosphorus acid compound in the amount of 100 parts by weight and selected form the group consisting of polyols, polyester, polyamide, polyepoxy, alcohols, polyethers, polycarboxyl, phenophlasts, aminoplasts, amines, polyamines, polythioethers, polyacetols, polycarbonates, silicones, vegetable oils, ketones, aldehydes, epoxides, organic acids, cellulose, vinyl polymers, vinyl co-polymers, vinyl-diene co-polymers, diene polymers, polyimides, polyesteramides, organic borates and mixtures thereof; B) acidic salt forming compound of phosphorus in the amount of 5 to 100 parts by weight; C) salt forming basic compound in the amount of 1 to 100 parts by weight; the said mixing is carried out in such a way that components A and B are reacted first to produce an organic-phosphorus acid then component C is reacted with the organic-phosphorus acid compound.
8. A fire retardant plastic comprising a plastic resin composition combined with a salt of an organic-phosphorus acid compound wherein the said salt is produced by mixing and reacting the following components: A) organic compound that will react with a phosphorus acid compound in the amount of 100 parts by weight; B) acidic salt-forming compound of phosphorus in the amount of 5 to 100 parts by weight; C) basic salt of a boron compound; the said mixing is carried out in such a way that component A and B are reacted first to produce an organic phosphorus acid compound then component C is reacted with the organic phosphorus acid compound.
9. A fire retardant plastic comprising a plastic resin composition combined with a salt of an organic phosphorus acid compound, wherein the said salt is produced by mixing and reacting the following components: A) organic borate compound in the amount of 100 parts by weight; B) acidic salt forming compound of phosphorus in the amount of 5 to 100 parts by weight; C) salt forming basic compound in the amount of 1 to 200 parts by weight; the said mixing is carried out in such a way that component A and B are reacted first to produce an organic phosphorus acid compound then component C is reacted with the organic phosphorus acid compound.
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