MXPA97009775A - Coloid particles of solid flame retardant compounds and smoke suppressors and methods to prepare - Google Patents

Coloid particles of solid flame retardant compounds and smoke suppressors and methods to prepare

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Publication number
MXPA97009775A
MXPA97009775A MXPA/A/1997/009775A MX9709775A MXPA97009775A MX PA97009775 A MXPA97009775 A MX PA97009775A MX 9709775 A MX9709775 A MX 9709775A MX PA97009775 A MXPA97009775 A MX PA97009775A
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Mexico
Prior art keywords
particles
antimony trioxide
micron
grinding
less
Prior art date
Application number
MXPA/A/1997/009775A
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Spanish (es)
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MX9709775A (en
Inventor
Mclaughlin John
C Morley John
S Podwirny Philip
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Anzon Inc
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Application filed by Anzon Inc filed Critical Anzon Inc
Publication of MX9709775A publication Critical patent/MX9709775A/en
Publication of MXPA97009775A publication Critical patent/MXPA97009775A/en

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Abstract

The present invention relates to finely divided particles of compounds that provide flame retardant and / or smoke suppression properties for fibers, textiles, polymeric articles, paper, paint, coatings and insulations. More particularly, the present invention relates to colloidal sized particles of hydrated salts, organic phosphates, metal borates, polyamides, halogenated flame retardant solids with melting points greater than 250 degrees Celsius, molybdenum compounds, metallocenes, antimony compound, Composed of zinc, bismuth compounds and other solid chemicals that act as flame retardants or smoke suppressants. The present invention also relates to various milling processes for reducing these materials to colloidal sizes and for dispersing them in water, in organic liquids and in fusible solids.

Description

COLOID PARTICLES DB COMPOUNDS SOLID FLAME RETARDANTS AND SMOKE SUPPRESSORS AND METHODS TO PREPARE THEM FIELD OF THE INVENTION The present invention concerns finely divided particles of compounds that provide flame retardancy and / or smoke suppressing properties for fibers, textile products, polymeric articles, paper, paint, coatings and insulation. More particularly, the present invention concerns colloidal sized particles of hydrated salts, organic phosphates, metal borates, polyamides, flame retardants, solids, halogenated, with a melting point greater than 250 ° C, molybdenum compounds, metallocenes, antimony compounds, zinc compounds, bismuth compounds, and other solid chemicals that act as flame retardants or smoke suppressants. The present invention also concerns various milling processes to reduce these materials to colloidal sizes and to disperse them in water, organic liquids and in solids that can be melted.
REF: 26403 BACKGROUND OF THE INVENTION The ability of several solids to act as flame retardants and / or smoke suppressors is known in the art. Said solids act by several mechanisms in order to provide flame retardancy including the following: a) Release of water and / or carbon dioxide - The hydrated salts of carbon dioxide (such as magnesium sulphate pentahydrate aluminum trihydrate, magnesium hydroxide, magnesium carbonate hydrate, etc.), which decompose at high temperatures, and release water and / or carbon dioxide in an endothermic reaction to put out a fire. b) Carbonization Formation - When exposed to high temperatures, carbonization formers that include organic phosphates, zinc compounds, nitrogen compounds (such as melamine esters and polyamides) and metal borates form carbon barriers that insulate materials fire fuels. c) Free radical capture / oxygen deprivation - Halogen compounds alone or in combination with antimony will prevent combustion. The primary mechanism is thought to be the formation of a dense layer of gas above the burning substances that inhibits or prevents oxygen from reaching the combustible material. There is also evidence in support of the ability of antimony halides to sequester free radicals in the flame, interrupting the reaction. d) Smoke suppression - Smoke suppressors work by helping to completely oxidize the carbonaceous materials formed in the flame and / or the formation of carbon or glass. They are generally catalysts for oxidation reactions and / or carbon or glass formers. Typical smoke suppressors are molybdenum oxide and ferrocene or other metallocenes.
All the previously listed solids are commercially used to provide either flame retardation or low smoke generation for plastics, carpets, fabrics, paper, paints, coatings, adhesives, wood composites, etc. Unfortunately, the use of such solids often imparts other undesirable properties in the article to which they are added. Typical undesirable properties that result from adding solid flame retardant particles or smoke suppressant compounds include: pigmentation (e.g., addition of undesirable colors), opacity (e.g., loss of light transmission), stiffness (e.g. of softness in textiles), decreased impact resistance (which results, for example, in increased crack propagation), and deposition of solids (in, for example, paints, coatings, and adhesives). Such undesirable properties can be reduced or eliminated by reducing the average particle size and substantially removing all particles above about 1 micron.
BRIEF DESCRIPTION OF THE INVENTION ThereforeIt is an object of this invention to provide colloidal particles (particles having a size that is comprised between 10"9 to 10" 6m) of solid smoke suppressant and / or flame retardant compounds including hydrated salts (such as aluminum trihydrate) , magnesium sulfate pentahydrate, magnesium hydroxide and hydrous magnesium carbonate), ammonium polyphosphate, organic phosphates (such as melamine pyrophosphate), metal borates (such as zinc borate and barium metaborate), polyamides, melamine, retardants of halogenated flame with a melting point above 250 ° C (such as brominated polymers, decabromodiphenyloxide, ethylene bis-tetrabromophthalamide, decabromodiphenylethane and dodecachlorodiodehydrodimethoxybenzocyclooctene), molybdenum compounds (such as molybdenum oxide and ammonium octamolybdate), metallocenes ( as ferrocer.o), antinomial compounds (such as antimony metals, antimony trioxide, pent antinomy oxide of antinomy and sodium), zinc compounds (such as oxides of zinc mixed metal and magnesium, or zinc sulfide) and bismuth compounds (such as bismuth subcarbonate), as well as a process for producing.
It is also an object of the present invention to provide stable dispersions of these materials in water, organic liquids and fusible solids, and to provide a method for producing them.
The colloidal particles of solid smoke suppressant and / or flame retardant compounds have advantages for use as external coatings for flame retardant in textiles or as internal flame retardant additives for systems such as coatings, plastics, textiles and rubber.
Dispersions of such particles are convenient, because they allow the particles to be transported while simultaneously inhibiting the coalescence of the particles in larger agglomerates.
These and other objects and advantages have been obtained by the present invention, in which colloidal size particles of insoluble solid compounds, smoke suppressants and / or flame retardants are provided by a high energy mill, such as a mill with means, even though commercial suppliers of such milling equipment do not suggest that such particle sizes can be obtained.
According to one embodiment of the present invention, a mill with agitated media loaded with grinding media is provided with a suspension comprising a fluid carrier and particles of a solid compound having flame retardant or smoke suppressing properties. The suspension is processed in the mill with agitated media until the particle size is reduced by at least 10%, more preferably 50 to 90%, and even more preferably 10 to 99%. In addition, the particles have an average volumetric particle size of less than 0.5 microns, preferably 0.01 to 0.5 microns, more preferably 0.01 to 0.25 microns, and even more preferably 0.01 to 0, 1 micron It is preferred that at least 99% of said particles have sizes less than 1 micron. More preferably at least 99.9% of the particles should have sizes less than 1 micron. It is also preferred that the suspension further comprises a dispersing agent.
Other objects and advantages of the invention and alternative embodiments will be readily apparent to those skilled in the art particularly after reading the detailed description, and the examples given below.
DETAILED DESCRIPTION OF THE PREFERRED MODALITIES Grinding with wet media is the preferred method for preparing the finely divided particles of the present invention. In general, the final characteristics of the material crushed in a mill with wet media, particularly the particle size, will be determined by several process variables.
For example, the type of mill can affect the final characteristics of the crushed materials. The type of mill can also determine how quickly a particular result can be achieved.
Other factors also determine the final characteristics of the crushed material as well as the time and energy consumed to achieve them. Examples of such factors include the following: (1) In grinding with wet media, smaller media is more efficient at producing finer particles in periods of time of 10 minutes and less. (2) Heavier means and higher tip speeds are desirable to impart more energy to the particles that are being crushed. (3) Low viscosities of fluid are beneficial for crushing particles. (4) As the diameter of the particles decreases, increase. the exposed surface areas, and a dispersing agent is generally used to prevent small particles from agglomerating. In some cases dilution alone can help achieve a particle size, but a dispersing agent is generally employed to obtain long-term stability against agglomeration. The preceding factors and others that influence the crushing performance are discussed in the following paragraphs.
As used herein, "particle size" refers to an average volumetric particle size measured by conventional techniques for measuring particle size such as sedimentation, photon correlation spectroscopy, field flow fractionation, disk centrifugation, microscope. electronic transmission and dynamic light scattering. A dynamic light scattering device such as particle size analyzer Horiba LA-900 Laser Scattering (Horiba Instruments, Irvine, California) is preferred by the present inventors, because it has advantages of easy sample preparation and speed. The volumetric distribution of the sample refers to the weight distribution.
Equipment grinding The preferred grinding equipment for practicing the present invention is generally known as agitated media mills where the grinding media is agitated in a grinding chamber. The preferred method of agitation is effected by a stirrer comprising a rotary shaft such as those found in grinding mills. The shaft may be provided with discs, arms, bolts or other accessories. The portion of the attachment that is radically further from the axis is mentioned here as the "tip". The mills can be batch or continuous, vertical or horizontal. A ball mill is an example of a mill of a rudimentary agitator medium.
A horizontal continuous media mill equipped with an internal screen having holes of sizes that are 1/2 to 1/3 the average diameter, is preferred as an efficient mill with means for practicing the present invention. High media loads (eg, 92% loads) are possible.
An increase in the amount of crushing media in the chamber will increase the grinding efficiency by decreasing the distances between the individual particles of grinding media and increasing the amount of surface available to cut the material to be crushed. The volume of the grinding media can be increased until the grinding media constitutes approximately 92% of the mass volume of the grinding chamber (the dead space between the particles is excluded). At levels substantially above this point, the media is blocked.
Starting Materials By the present invention, smoke suppressants or flame retardants can be wet milled at levels that would not ordinarily be achievable with dry milling techniques.
Within reason, the size of the feed material to be crushed is not critical. For example, antimony trioxide can be reduced to an average particle size of 0.10 microns with a stirred media mill using the method of the present invention, either from particles having an average particle size of 4. 3 microns 2.0 microns or 0.6 microns. However, in general, the feed material should not be larger than 10% of the grinding media. Other flame retardants such as decabromodiphenyl oxide and zinc borate can be reduced similarly to 0.25 and 0.14 microns or less, respectively, in short crushing times.
Faster milling times can be achieved if small starting materials are used. Therefore, it is preferred to start with particles that are as small as is economically feasible to reduce milling time. For example, a 0.5 micron antimony trioxide feedstock (measured by Electronic Transmission Microscope) can be shredded to the desired size (e.g., 0.1 micron) in a shorter period of time than a stock material. 4.3 microns. For this reason, antimony trioxide with an average particle size of 0.5 microns is preferred to a material having a larger particle size. When the material is used, a narrow particle distribution and a shorter grinding time are achieved.
Crusher Media Suitable crusher means for carrying out the present invention include sand, glass granules, metals and ceramics. Preferred glass granules include barium titanium (with lead), caustic soda (no lead), and borosilicate. Preferred metals include carbon steel, stainless steel and tungsten carbide. Preferred ceramics include zirconium oxide stabilized with yttrium, zirconium silicate and alumina. The most preferred grinding medium for the purpose of the invention is zirconium oxide stabilized with ire.
Each type of medium has its own advantages. For example, metals have high specific weights, which increases crusher efficiency due to an increased impact. The costs of metals range from low to high, and pollution can be a problem. Glasses are advantageous from the point of view of low cost and the availability of small sizes as low as 0.004 mm. These small sizes make it possible to obtain a finer particle size. The specific weight of the glasses however is lower than that of other media and more grinding time is necessary. Finally, ceramics are advantageous from the point of view of low wear, low porosity and ease of cleaning.
The grinding media used to reduce the particle size is preferably spherical. As previously indicated, the smaller grinding media sizes result in smaller final particle sizes. The grinding media for carrying out the present invention preferably have an average size comprised between 0.004 and 1.2 mm, more preferably 0.012 to 0.2 mm.
By using appropriately selected grinding media, the grinding process of the present invention actually grinds the particles, instead of de-agglomerating the particle lumps - a task for which mills with means are normally used.
Vehicles for Fluids Vehicles for fluids in which particles can be comminuted and dispersed include water, organic liquids (such as dimethylacetamide or ethylene glycol), polyvinyl chloride plasticizers (such as diisodecylphthalate), and low melting solids such as waxes or fats in which the grinding is carried out at temperatures higher than the melting point of waxes or fats. In general, as long as the used fluid vehicle has a reasonable viscosity and does not adversely affect the chemical or physical characteristics of the particles, the choice of fluid vehicle is optional. Water is usually preferred.
Dispersing Agents The dispersing agents preferably act to wet the newly exposed surfaces which result when the particles break. The dispersing agents also preferably stabilize the resultant suspension of ground particles by providing either (1) a positive or negative electrical charge on the ground particles or (2) steric blocking through the use of a large mass molecule. Preferably an electrical charge is introduced by anionic and cationic surfactants while the steric block is preferably carried out by the polymers absorbed with particle charges that repel each other. Zwitterionic surfactants may have characteristics of anionic and cationic surfactant in the same molecule.
Preferred dispersing agents for carrying out the invention include wetting agents (such as Triton X-100 and Triton CF-10, sold by Union Carbide, Danbury, Connecticut, and Neodol 91-6, sold by Shell Chemical); anionic surfactants (such as Tamol 731, Tamol 931 and Tamol-SN, sold by Rohm '& Hass, Philadelphia, Pennsylvania, and Colloid 226/35, sold by Rhone Poulenc); cationic surfactants (such as Disperby e 182 sold by By e Chemie, Wellingford, Connecticut); amphoteric surfactants (sold by Crosultain T-30 and Incrosoft T-90, sold by Croda, Inc., Parsippany, New Jersey); and non-ionic surfactants (such as Disperse-Ayd W-22 sold by Daniel Products Co., Jersey City, New Jersey). The most preferred dispersing agents are anionic surfactants such as Tamol-SN.
Other Parameters of Grinding The relative proportions of particles to be ground, the vehicles for fluids, the grinding media and the dispersing agents can be optimized to carry out the present invention.
Preferably, the final suspension leaving the mill comprises the following: (1) 5 to 60% by weight, more preferably 15 to 45% by weight of the particles to be comminuted; (2) 40 to 95%, more preferably 55 to 85% by weight of the fluid vehicle; and (3) 2 to 15% by weight, more preferably 6 to 10% by weight of the dispersing agent.
Preferably the loading of grinding media as a percentage of the volume of the mill chamber is from 80 to 92%, more preferably from 85 to 90%.
The speed of the agitator controls the amount of energy that enters the mill. The higher the speed of the agitator, the more kinetic energy enters the mill. Higher kinetic energy results in higher crushing efficiency due to higher impact and cut. Therefore, an increase in the RPM of the agitator will result in an increase in the grinding efficiency. While generally desirable, those skilled in the art understand that an increase in grinding efficiency will be accompanied by a concurrent increase in the chamber temperature of the chamber pressure and the rate of wear.
The speed of the tip of the agitator represents the maximum speed (and therefore the kinetic energy) experienced by the particles that must be ground. Therefore, larger diameter mills can impart media speeds equal to those of smaller mills at lower RPM.
The residence time (referred to cumulatively as retention time) is the amount of time that elapses with the material in the crushing chamber while it is exposed to the crushing media. The residence time is calculated by simply determining the grinding volume that is available to the mill and dividing this amount by the flow rate through the mill (exit rate). In general, a certain dwell time will be necessary to achieve the desired final product characteristics (for example, the final product size). If this time of permanence can be reduced, a higher production regime will be achieved while minimizing capital costs. In order to carry out the present invention, the dwell time may vary but preferably it will be less than 15 minutes and more preferably less than 10 minutes. 8 It is often convenient to have two or more mills in series, particularly when dramatic reductions in particle size are necessary to optimize the grinding efficiency. A maximum reduction in particle size within a given milling step is typically between about 10: 1 to as high as about 40: 1 and depends to some extent on the size of the media. As a result, the number of milling stages increases as the overall size reduction requirements increase. Effects similar to those of step mills can also be achieved by using a single mill to collect the product at the outlet and repeatedly feed the product through the mill. However, longer dwell times can be arranged to achieve similar final particle sizes.
EXAMPLES The following examples, as well as the foregoing description of the invention and its various embodiments are not intended to be limiting of the invention but are intended to illustrate the same. Those skilled in the art will be able to formulate other embodiments encompassed within the scope of the present invention.
Example 1 A horizontal 10-liter mill with continuous media (Netzsch, Inc., Exton, Pennsylvania) was filled to 90% with YTZ (zirconium oxide stabilized with a glass) media with an average diameter of 0.2 mm and a weight specific 5.95 (Tosoh Corp., Bound Broo, New Jersey). A 0.1 mm sieve was installed inside the mill at the exit.
Forty-five pounds of antimony trioxide with an average particle size of 0.2 microns (Cookson Specialty Additives, Anzon Division, Philadelphia, Pennsylvania) were left in suspension in 55 pounds of water and 4.5 pounds of Tamol-SN.
The mill operated with a tip speed that averaged 2856 feet per minute. After 7.5 minutes of retention time (5 passes through the mill), the average particle size was reduced, by volume, 0.102 microns and 99.9% of the particles had sizes less than 0.345 microns.
Example 2 The same mill, media and filler were used as in example 1. This time, an antimony trioxide feed having an average particle size of 0.6 microns was used (Cookson Specialty Additives, Anzon Division, Philadelphia , Pennsylvania). Thirty pounds of antimony trioxide were left in suspension with 70 pounds of water and 1.8 pounds of Tamol-SN and 0.9 pounds of Triton CF-10.
The speed of the tip during the trial averaged 2878 feet per minute. After 4.8 minutes of retention time in the mill (4 passes), the average particle size volume was 0.11 microns and 99.9% of the particles had sizes less than 0.31 microns.
Example 3 The same mill, the same media, antimony trioxide and the filler of Example 1 were used. This time no surfactants were used.
Twenty-eight pounds of antimony trioxide were left in suspension with 100 pounds of water. The tip speed was 3023 feet per minute. After 2.4 minutes of retention time (2 passes). The average particle size was 0.13 microns, 99.9% of the particles having sizes less than 1.06 microns.
Since the viscosity of the product was high, an additional 35 pounds of water was added. After 1.8 minutes of additional retention time (2 extra passes), the average particle size was further reduced to 0.10 microns, 99.9% of the particles having sizes less than 0.32 microns.
Example 4 The same mill, the same media and filler were used as in Example 1. Thirty pounds of a 4 micron antimony trioxide feed material (Cookson Specialty Additives, Anzon Division) were left in suspension with 70 pounds of water and 2.8 pounds of Tamol-SN. The tip speed was 2860 feet per minute. After 7 minutes of retention time (5 passes), the average particle size was 0.10 microns, 99.9% of the particles having sizes less than 1.2 microns.
Example 5 Using the same mill, the same media and filler as in Example 1, 80 pounds of a brominated organic flame retardant (odophenyl decayl oxide) was left in suspension (Arblemarle, Inc. Baton Rouge, Louisiana, Great Lakes, Lafayette, Indiana; Ameribrom, Inc., New York, New York) in a suspension with 55 pounds of water. The starting particle size averaged 2.7 microns with some particles as large as 10 microns. After 10.4 minutes of retention time (6 passes), the average particle size was 0.25 microns, 99.9% of the particles having sizes less than 2.70 microns.
Example 6 The horizontal 10-liter mill of Example 1 was filled to 90% with 4-6 mm electrofused zirconia / silica ceramic granules having a specific gravity of 3.85 (SEPR, Mountainside, New Jersey). The same 0.1 mm sieve of Example 1 was used inside the mill.
Fifty pounds of 2 micron antimony trioxide feed was mixed with 11 pounds of water and 5 pounds of Tamol-SN. After 7.8 minutes of retention time, the average particle size was 0.20 microns, with 99.9% of the particles sizes below 0.46 microns.
Example 7 A 10 liter mill with horizontal means according to Example 1 was loaded to 90% with borosilicate glass granules having an average diameter of 0.093 mm and a specific gravity of 2.6 sold by Potters Industries. A 0.025 mm sieve was used in the mill.
Fifty pounds of 0.6 micron antimony trioxide were left in suspension with 61 pounds of water and 5 pounds of Tamol-SN. The speed of the tip was 3420 feet per minute. The amperage of the mill was only 67% similar to that of similar tests using media with a specific gravity of 5.95. The resulting antimony trioxide product had an average particle size of 0.09 microns, with 100% of the particles having sizes less than 0.30 microns.
Example 8 The 10 liter continuous horizontal media mill of Example 1 was loaded to 90% with the YTZ media of Example 1. Fifty pounds of zinc borate with a particle size of 9.8 microns (Cookson Specialty Additives, Anzon Division, Philadelphia, Pennsylvania) were suspended with 93 pounds of water and 3 pounds of Tamol-SN, The tip speed was 2788 feet per minute. After 8.9 minutes (4 passes) of retention time, the average particle size was reduced to 0.14 microns, with 99.9% of the particles being less than 0.41 microns.
Example 9 A shredder (Union Process, Inc., Akron Ohio) with a tank volume of 750 cm3 was loaded with 250 cm3 of YTZ powder (Metco, Inc., Westbury, NY) sieved to a size of 0.053 mm. . 180 g of the suspension of Example 1 was added to the grinder. After operating the shredder at 4,000 RPM (tip speed 3 600 feet / minute) for 60 minutes, the average particle size of the resulting product was 0.07 microns.
Having thus specially described and determined the nature of the present invention and the manner in which it is to be put into practice, it is hereby declared to claim as property and exclusive right the following:

Claims (1)

  1. CLAIMS Finally divided particles of a solid chemical compound having properties of flame retardation or smoke suppression, characterized in that said particles have an average volumetric size less than less than 0.1 micron, said particles have a size distribution such that at least 99% of said particles have sizes of less than about 1 micron, and said particles are produced by grinding. Finally divided particles of claim 1, characterized in that at least 99% of said particles have sizes less than 1 micron. The finally divided particles of claim 1, characterized in that said solid chemical compound is selected from the group consisting of hydrated salts, organic phosphates, metal borates, polyamides, halogenated solid flame retardants with a melting point greater than 250 ° C, of molybdenum, metallocenes, antimony compounds, zinc compounds and bismuth compounds. The finely divided particles of claim 1, characterized in that each solid chemical compound is selected from the group consisting of aluminum trihydrate, magnesium sulfate pentahydrate, magnesium hydroxide, magnesium carbonate hydrate, ammonium polyphosphate, melamine pyrophosphate, metaborate barium, melamine, brominated polymers, ethylene bis-tetrebromophthalamide, decabromodiphenylethane, dodecachlorodiodecahydrodimethane-dibenzocyclooctene, molybdenum oxide, ammonium octamolybdate, ferrocene, antimony metal, antimony pentoxide, sodium antimonate, zinc oxide and magnesium oxide mixture , zinc sulphide and bismuth subcarbonate. The finely divided particles of claim 1, characterized in that said solid chemical compound is zinc borate. The finely divided particles of claim 1, characterized in that said solid chemical compound is decarbromodiphenyloxide. The finely divided particles of claim 1, characterized in that said solid chemical compound is antimony trioxide. A dispersion comprising a fluid carrier, characterized in that it comprises a dispersing agent and the particles of claim 1. The dispersion of claim 8, characterized in that said fluid carrier is selected from the group consisting of organic liquids, polyvinyl chloride plasticizers and waxes or low melting point fats. The dispersion of claim 8, characterized in that said fluid carrier is selected from the group consisting of dimethylacetamide, ethylene glycol and diisodecylphthalate. The dispersion of claim 8, characterized in that the fluid vehicle is water. The dispersion of claim 8, characterized in that the dispersing agent is selected from the group consisting of cationic surfactants, amphoteric surfactants and non-ionic surfactants. The dispersion of claim 8, wherein said dispersing agent is selected from the group consisting of anionic wetting agents and suctants. 14. A process for producing finely divided particles of a solid compound having flame retardant or smoke suppression properties characterized in that it comprises: loading the stirred media mill, with grinding media, a fluid vehicle and starting particles of a solid compound having flame retardant or smoke suppressing properties; Y stirring said shredding medium, said fluid vehicle and starting particles until said size particles are reduced by at least 10%, and the shredded particles are produced within the stirred medium of the mill having a size distribution where said particles have an average volumetric less than 0.1 micron and where at least 99% of said crushed particles is less than 1 micron in size. 15. The process of claim 14, characterized in that said suspension further comprises a dispersing agent. The method of claim 14, characterized in that said stirred media mill operates with a tip speed comprised between 1,000 to 6,000 feet per minute. The method of claim 14, characterized in that said grinding media is provided in an amount that is sufficient to fill approximately 80 to 92% of the volume of mass inside said mill. The method of claim 14, characterized in that said crushed media are selected from the group consisting of sand, glass granules, metals and ceramics. The process of claim 18, characterized in that said grinding media are selected from the group consisting of barium titanite, lead caustic soda, borosilicate, carbon steel, stainless steel, tungsten carbide, zirconium silicate, and alumina. The method of claim 19, characterized in that said medium is zirconium oxide stabilized with yttrium. The process of claim 14, characterized in that said solid chemical compound is selected from the group consisting of hydrated salts, organic phosphates, metal borates, polyamides, halogenated solid flame retardants with a melting point greater than 250 ° C, molybdenum compounds , metallocenes, antimony compounds, zinc compounds and bismuth compounds. The process of claim 14, characterized in that said solid chemical compound is selected from the group consisting of zinc borate, decabromodiphenyloxide and antimony trioxide. The method of claim 14, characterized in that said fluid carrier is selected from the group consisting of organic liquids, polyvinyl chloride plasticizers and waxes or low melting point fats. The process of claim 14, characterized in that said fluid carrier is selected from the group consisting of dimethylacetamine, ethylene glycol and diisodecylphthalate. The process of claim 14, characterized in that said fluid vehicle is water. 6. The method of claim 15, characterized in that said dispersing agent is selected from the group consisting of cationic surfactants, amphoteric surfactants and non-ionic surfactants. 7. The process of claim 14, characterized in that said dispersing agent is selected from the group consisting of wetting agents and anionic surfactants. 8. Finely divided particles of a solid chemical compound characterized in that it has flame retardant or smoke suppressing properties produced by the process of claim 14. 9. The method of claim 14, characterized in that the grinding medium has an average size ranging from about 0.012 to 0.2 microns. 30. The process of claim 29 characterized in that the grinding medium is zirconium stabilized with yttrium. 31. The method of claim 30, characterized in that the grinding medium has an average diameter of approximately 0.2 mm. 32. A process for producing finely divided antimony trioxide characterized in that it comprises: loading the agitated media mill, with ceramic grinding media, a fluid vehicle, a dispersing agent and antimony trioxide starting particles; Y stirring said grinding medium, said fluid carrier, dispersing agent and antimony trioxide starting particles until said starting particles of antimony trioxide are reduced in size by at least 10% and the crushed particles of antimony trioxide are produced within the agitated medium of the mill having a size distribution where the crushed particles of antimony trioxide have a volumetric average particle size of less than 0.1 micron and where at least 99% of said crushed particles of antimony trioxide are in size less than 1 micron. 3. The process of claim 32 characterized in that the dispersing agent in an anionic surfactant. . The method of claim 32 characterized in that said fluid vehicle is water. 35. The process of claim 32 characterized in that said grinding media is zirconium oxide stabilized with yttrium having an average diameter of about 0.2 mm. 36. Finely divided particles of antimony trioxide characterized in that they have a particle size with a volumetric average less than 0.1 micron, at least 99% of said particles have sizes less than 1 micron, said particles are produced by grinding and are dispersed in a fluid vehicle containing a dispersing agent. 37. The finely divided particles of claim 36 characterized in that the dissolving agent in an anionic surfactant. 3. The process of claim 32 characterized in that the dispersing agent in. an anionic surfactant 34. The method of claim 32 characterized in that said fluid vehicle is water. 35. The process of claim 32 characterized in that said grinding media is zirconium oxide stabilized with yttrium having an average diameter of about 0.2 mm. 36. Finely divided particles of antimony trioxide characterized in that they have a particle size with a volumetric average less than 0.1 micron, at least 99% of said particles have sizes less than 1 micron, said particles are produced by grinding and are dispersed in a fluid vehicle containing a dispersing agent. 37. The finely divided particles of claim 36 characterized in that the dissolving agent in an anionic surfactant. 8. The finely divided particles of claim 36 characterized in that said fluid carrier is water. 39. A process for producing finely divided particles of a solid compound having flame retardant or smoke suppression properties characterized in that it comprises: loading the stirred media mill, with grinding media, a fluid vehicle, and starting particles of a solid compound having flame retardant or smoke suppressing properties; Y stirring said grinding medium, said fluid vehicle and starting particles until said starting particles of size are reduced by at least 10% and the crushed particles are produced within the stirred medium of the mill having a size distribution where each particle has a volumetric average particle size smaller than 0.25 microns and where at least 99% of said crushed particles is smaller than 1 micron, where said size distribution is produced in a residence time of less than 15 minutes. 40. A process for producing finely divided antimony trioxide characterized in that it comprises: loading the agitated media mill, with ceramic grinding media, a fluid vehicle, a dispersing agent and antimony trioxide starting particles; Y stirring said grinding medium, said fluid carrier, dispersing agent and antimony trioxide starting particles until said starting particles of antimony trioxide are reduced in size by at least 10% and the crushed particles of antimony trioxide are produced within the agitated medium of the mill having a size distribution where the crushed particles of antimony trioxide have a volumetric average particle size of less than 0.25 micron and where at least 99% of said crushed particles of antimony trioxide are in size less than 1 micron, where said size distribution is produced in a residence time of less than 15 minutes.
MXPA/A/1997/009775A 1995-06-07 1997-12-05 Coloid particles of solid flame retardant compounds and smoke suppressors and methods to prepare MXPA97009775A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US48303295A 1995-06-07 1995-06-07
US08483032 1995-06-07

Publications (2)

Publication Number Publication Date
MX9709775A MX9709775A (en) 1998-10-31
MXPA97009775A true MXPA97009775A (en) 1999-01-11

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