Mixtures of ammonium polyphosphate and at least one soluble ionic compound containing sulfate and/or is capable of releasing sulfate ions

Patent metadata

Field	Value
Publication number	US-11628589-B2
Application number	US-201615769219-A
Country	US
Kind code	B2
Filing date	Oct 18, 2016
Priority date	Oct 20, 2015
Publication date	Apr 18, 2023
Grant date	Apr 18, 2023

Abstract

The invention relates to mixtures containing, as component (A) ammonium polyphosphate and, as component (B) a soluble ionic compound which contains sulfate and/or is capable of releasing sulfate ions. The invention also relates to a method for producing such mixtures and to the use thereof.

First claim

The invention claimed is:

1. An intumescent formulation for a fire protection coating, comprising a mixture of:
as component (A) ammonium polyphosphate; and
as component (B) lithium sulfate, magnesium sulfate, calcium sulfate, barium sulfate, iron (III) sulfate, iron (II) sulfate, titanium sulfate, cerium sulfate, melamine sulfate, urea sulfate, ammonium sulfate or a mixture thereof,
wherein the mixture has a water solubility of less than 0.5 (10% suspension in water at 25° C.),
wherein the mixture comprises 99.55 to 99.99% by weight of component (A); and 0.01% to 0.45% by weight of component (B), and
wherein the sum total of the components is 100% by weight.

2. The intumescent formulation as claimed in claim 1 , wherein the ammonium polyphosphate is of the crystal form I, II, III, IV, V, VI, a branched ammonium polyphosphate or a mixture thereof.

3. The intumescent formulation as claimed in claim 1 , wherein the ammonium polyphosphate is one of the crystal form I, II, V or a mixture thereof.

4. The intumescent formulation as claimed in claim 1 , wherein the ammonium polyphosphate is of the formula (NH 4 ) n+2 P n O 3n+1 with n≥2.

5. The intumescent formulation as claimed in claim 1 , wherein the ammonium polyphosphate is of the formula (NH 4 ) n+2 P n O 3n+1 with n from 10 to 10 000.

6. The intumescent formulation as claimed in claim 1 , wherein component (B) is ammonium sulfate.

7. The intumescent formulation as claimed in claim 1 , comprising:
99.60% to 99.80% by weight of component (A); and
0.20% to 0.40% by weight of component (B),

wherein the sum total of the components is 100% by weight.

8. The intumescent formulation as claimed in claim 1 , comprising:
99.60% to 99.80% by weight of component (A); and
0.20% to 0.40% by weight of component (B),

wherein component (B) is ammonium sulfate, and
wherein the sum total of the components is 100% by weight.

9. The intumescent formulation as claimed in claim 1 , wherein the mixture has:
a residual moisture content of less than 0.5%,
a bulk density of 0.3 to 0.9 g/cm 3 ,
a viscosity of less than 40 mPas (Brookfield DV3T, spindle 1) (10% suspension in water at 25° C.),
a particle size d 50 of 5 to 35 μm,
a chain length of n greater than 1000 for the ammonium polyphosphate; and
a pH of 4 to 8.

10. A process for producing a mixture as claimed in claim 1 , comprising mixing component (A) and component (B) together, each in pulverulent or granular form, or introducing component (B) in dissolved form into component (A).

11. The process as claimed in claim 10 , wherein 99.55% to 99.99% by weight of component (A) and 0.01% to 0.45% by weight of component (B) are mixed with one another,
wherein component (B) is ammonium sulfate, and
wherein the sum total of the components is 100% by weight.

12. A process for producing a mixture as claimed in claim 1 , comprising heating equimolar amounts of ammonium dihydrogen orthophosphate and urea to a temperature of 250 to 300° C. for a period of 0.5 to 4 hours with simultaneous addition of component (B).

13. A process for producing a mixture as claimed in claim 1 , comprising heating equimolar amounts of ammonium orthophosphate and urea to a temperature of 250 to 305° C. for a period of 0.1 to 4 hours under a moist ammonia atmosphere with simultaneous addition of component (B).

14. A process for producing a mixture as claimed in claim 1 , comprising heating equimolar amounts of ammonium orthophosphate and urea to a temperature of 320 to 350° C. for a period of 0.1 to 4 hours under a moist ammonia atmosphere with simultaneous addition of component (B).

15. A process for producing a mixture as claimed in claim 1 , comprising mixing and reacting phosphorus pentoxide, diammonium orthophosphate and component (B) together in molarity ratios of 1:1:0.01 to 0.08 in ammonia gas atmosphere over a period of 5 to 10 minutes and then successively
a) conducting a polymerization reaction over a period of 15 to 45 minutes with supply of ammonia gas at a maximum reactor pressure of 490 to 980 Pa and at a minimum temperature of 180 to 200° C.,
b) feeding in ammonia gas at a temperature in the range from 200 to 220° C. and a minimum reactor pressure between 0 and 980 Pa for a period of 2 to 4 hours,
c) separating off and working up the products obtained,

wherein component (B) is ammonium sulfate.

Assignees

• Clariant Plastics & Coatings Ltd
• Clariant Int Ltd

Inventors

• Termath Andreas

Classifications

• B27K3/166

  Compounds of phosphorus · CPC title

• B27K3/20 Primary

  Compounds of alkali metals or ammonium · CPC title

• C01B25/28

  Ammonium phosphates · CPC title

• C01B25/405

  of ammonium · CPC title

• C09D5/185

  Intumescent paints · CPC title