TW200806581A - Coated aluminum hydroxide particles produced by mill drying - Google Patents

Abstract

Coated, mill-dried ATH particles, methods of making them, their use in flame retarded polymer formulations, and molded or extruded articles made from the flame retarded polymer formulations.

Description

200806581 IX. DESCRIPTION OF THE INVENTION: TECHNICAL FIELD OF THE INVENTION The present invention relates to novel coated aluminum hydroxide flame retardants, processes for their preparation, and uses thereof. [Prior Art]

Aluminum hydroxide has a number of different names, such as hydrated aluminum, aluminum trihydrate, aluminum trihydroxide, etc., but is commonly referred to as ATH. Granular aluminum hydroxide, hereinafter referred to as ATH, has many uses, such as in many materials (e.g., paper, resin, rubber, plastic, etc.). One of ATH's most widely used uses is as a flame retardant in synthetic resins such as plastics and in wires and cables. The industry application force of ATH has been known for some time. In the field of flame retardants, ATH is used in synthetic resins (such as plastics) and wire and cable applications to impart flame retardant properties. In an effort to provide better compatibility with resins, ATH particles have been coated with various surface active materials, including decane, fatty acids, and the like. In general, it deposits surface-active treatment unevenly on the ATH particles, such that the coupling agent or the surface-active coating acts as a binder to strongly agglomerate the ATH particles with each other. This cohesive degraded ATH particle disperses in the resin, which is an undesirable property. However, when a uniform surface treatment is obtained, the coupling agent or the surface-active coating cannot be used as a binder, and a good dispersing power in the selected resin can be maintained. Thus as the demand for coated ATH particles increases, so does the need to make a process for uniformly coating ATH particles. SUMMARY OF THE INVENTION In one embodiment, the present invention is directed to ATH particles comprising a surface coating agent selected from the group consisting of i) fatty acids 200806581; ii) oxoxane derivatives; and Hi) mixtures thereof. The ATH particles are produced by honing and drying a slurry or filter cake containing from about 1 to about 85% by weight of ATH particles, based on the slurry or filter cake, in the presence of a surface coating agent. In another embodiment, the present invention is directed to a method for making coated ruthenium particles comprising, in the presence of a surface coating agent, honing and drying from about 1 to about 85 weights based on the slurry or filter cake. A slurry or filter cake of ATH particles in the range of %, thus producing coated honed dry ATH particles. The surface φ face coating agent may be suitably selected from the group consisting of i) fatty acids; ii) oxirane derivatives; and iii) mixtures thereof. In another embodiment, the invention is directed to a method for making coated aluminum hydroxide particles comprising: a) honing and drying in a honing drying unit comprising from about 1 to about 1% by weight of slurry or cake a slurry or filter cake of about 85 wt% aluminum hydroxide; and b) when honing the slurry or filter cake, it will be selected from the group consisting of i) fatty acid; ii) a oxane derivative; and iii) A surface coating agent of the mixture is introduced into the honing drying unit, thereby producing coated honed dried aluminum hydroxide particles. In this embodiment, the surface coating agent can be introduced into the honing drying unit as a batch or it can be continuously metered into the honing drying unit, or it can be introduced or continuously before the honing drying. Measured into a filter cake or slurry. In yet another embodiment, the invention is directed to a method for making a coated aluminum hydroxide particle according to 200806581, comprising: a) comprising a filter cake or slurry 1 to about 85 wt% of a slurry or filter cake of aluminum hydroxide introduced into the honing drying unit jb) before or after the introduction of the slurry or filter cake, will be selected from the group consisting of i) fatty acid; hydrazine) decane derivative; And iii) a surface coating agent of the mixture thereof is simultaneously and continuously introduced into the honing drying unit; and φ c) honing the slurry or filter cake in the presence of the surface coating agent until the surface coating agent is produced The dried aluminum hydroxide particles are coated and honed. [Embodiment] ATH as used herein means aluminum hydroxide, and various names commonly used in the art refer to the mineral flame retardant such as aluminum hydrate, aluminum trihydrate, aluminum hydride hydroxide and the like. This invention relates to the manufacture of coated honed dry ATH particles. These coated honed dry ATH granules can be suitably produced by honing and drying a slurry or filter cake containing ATH granules in the presence of a surface coating agent. Spirit liquid and filter cake

The slurry or filter cake useful in the practice of the present invention generally comprises from about 1 to about 85 weight percent of ATH particles, based on the total weight of the slurry or filter cake, i.e., sometimes using filter cakes in the practice of the invention, while A slurry is used in the examples. In a preferred embodiment, the slurry or filter cake contains from about 25 to about 70 weight percent ATH particles, more preferably from about 55 to about 65 weight percent ATH 200806581 particles' which are all based on the same calculations. In other preferred embodiments, the slurry or filter cake contains from about 40 to about 60 weight percent ATH particles, more preferably from about 45 to about 55 weight percent ATH particles, which are all based on the same calculation basis. In still other preferred embodiments, the slurry or filter cake contains from about 25 to about 50 weight percent ATH particles, more preferably from about 30 to about 45 weight percent ATH particles, which are all based on the same calculations. The slurry or filter cake used in the practice of the present invention can be obtained by any method for making ATH particles. Preferably, the slurry or filter cake is obtained by a process involving the production of ruthenium particles by precipitation and φ-filtration. In an exemplary embodiment, the slurry or filter cake is formed by a process comprising dissolving the crude aluminum hydroxide in caustic to form a sodium aluminate solution, cooling and filtering, thereby forming an aluminum that can be used in the exemplary embodiment herein. The sodium liquid method is obtained. The sodium aluminate solution so produced generally has a Na20 to Α12〇3 molar ratio ranging from about 1.4:1 to about 1.55:1. In order to precipitate the cerium particles from the sodium aluminate solution, the cerium seed is added to the sodium aluminate solution in an amount of about 1 gram of cerium seed per liter of sodium aluminate solution to about 3 gram of cerium seed per liter of sodium aluminate solution, A method mixture is formed. # Add the barium grain to the sodium aluminate solution when the sodium aluminate solution is at a liquid temperature of about 45 to about 80 °C. After the addition of the ATH kernel, the process mixture is stirred for about 100 hours, or until the Na20 to Al2〇3 molar ratio is in the range of from about 2.2:1 to about 3.5··1, thus forming an ATH suspension. The resulting hydrazine suspension typically comprises from about 80 to about 160 grams per liter of ATH, based on the suspension. However, the ATH concentration can be varied to fall within the above range. The resulting ATH suspension is then filtered and washed to remove impurities therefrom, thus forming a filter cake. The filter cake may be washed once with water (preferably with demineralized water) or, in some embodiments, over 200806581. This filter cake can then be directly honed and dried in the presence of a surface coating agent. 'However, in certain preferred embodiments, the filter cake may be repulped in water to form a slurry, or in other preferred embodiments, at least one (preferably only one) dispersant is added to the filter cake to form an ATH concentration. A slurry of the above range. It should be noted that it is also within the scope of the invention to repulse the filter cake in a combination of water and dispersant. Non-limiting examples of dispersants suitable for use herein include polyacrylates, organic acids, naphthalene sulfonate/formaldehyde condensates, fatty alcohol-poly propylene alcohol ethers, polypropylene-ethylene oxide, polyglycol esters, Polyamine-ethylene oxide, phosphate ester, polyvinyl alcohol. If the slurry comprises a dispersant, the slurry may contain up to about 85 weight percent ruthenium based on the total weight of the slurry due to the effect of the dispersant. In this particular embodiment, the remaining slurry or filter cake (i.e., excluding ATH particles and dispersant) is typically water, although certain reagents, contaminants, and the like may be present as a result of precipitation. In certain embodiments, the ATH particles in the slurry or filter cake are typically characterized by a BET having a range of from about 1.0 to about 30 square meters per gram. In a preferred embodiment, the ATH particles in the slurry or filter cake have a BET in the range of from about 1.0 to about 4.0 square meters per gram, preferably from about 1.5 to about 2.5 square meters per gram. The ATH particles in the slurry or filter cake can be further characterized as having d5() in the range of from about 1.8 to about 3.5 microns. In a preferred embodiment, the ATH particles in the slurry or filter cake have a d50 in the range of from about 1.8 to about 2.5 microns. In other embodiments, the ATH particles in the slurry or filter cake are characterized by a BET having a range of from about 4<0>0 to about 8.0 square meters per gram. In a preferred embodiment, the ATH particles in the slurry or filter cake have a BET in the range of from about 5 to about 7 square meters per 200806581 grams. The AT ruthenium particles in the slurry or filter cake can be further characterized as d5 具有 having a range of from about 1.5 to about 2.5 microns. In a preferred embodiment, the ATH particles in the slurry or filter cake have a d5G in the range of from about 1.6 to about 2.0 microns which is coarser than the honed dry ATH particles produced in the present invention.

In still other embodiments, the ATH particles in the slurry or filter cake are characterized by having an amount ranging from about 8.0 to about 14 square meters per gram. In a preferred embodiment, the ATH particles in the slurry or filter cake have a BET in the range of from about 9 to about 12 square meters per gram. The ATH particles in the slurry or filter cake can be further characterized as d5Q having a range of from about 0.5 to about 1.6 microns. In a preferred embodiment, the ATH particles in the slurry or filter cake have a d50 in the range of from about 0.8 to about 1.4 microns. Surface Coating Agent The surface coating agent used herein may be selected from the group consisting of i) fatty acids; ii) oxirane derivatives; and i i i) at least one of its mixtures, sometimes only one. In certain embodiments, the surface coating agent is selected from the group consisting of a decane derivative or a fatty acid, and in other embodiments, the surface coating agent is a combination of a decane derivative and a fatty acid. The oxane derivative suitable for use herein may be selected from any one or more of an oligoalkyl oxane; a polydialkyl decane such as polydimethyl methoxy oxane or polydiethyl decane; A polyalkylaryl siloxane, such as polyphenylmethyl oxane; or a polydiaryl fluorene, such as polyphenyl siloxane. These oxane derivatives may be functionalized with a reactive group such as a hydroxyl group, an amine group, a vinyl group, a methacryl group, a carboxyl group, or a cyclopropoxy group. -10- 200806581 Fatty acids suitable for use herein may be selected from any one or more of saturated fatty acids, unsaturated fatty acids, and fatty acids having additional functional groups, such as amino* or hydroxy fatty acids, suitable for use herein. Isostearic acid can also be used. The fatty acids used herein are generally those having from about 8 to about 30 carbon atoms. Preferably, the fatty acid used herein is a saturated fatty acid having from about 10 to about 24 carbon atoms. It can be used as a pure or industrially pure substance and as a homogeneous mixture (i.e., from the decomposition of natural fat). This fatty acid is also commercially available. The surface coating agent may be uniformly introduced into the honing drying unit φ with the slurry or the filter cake, or the slurry or filter cake may be honed and dried for a while before the introduction of the surface coating agent, or the surface agent may be fed to the crucible. The slurry or filter cake is metered before grinding the drying unit. In a particular embodiment, the surface coating agent can be introduced before or after introduction of the filter cake. It is feasible because most commercially available honing drying units have multiple points at which the feed material can be introduced into the honing drying unit. Further, the surface coating agent may be introduced into the batch drying unit or continuously metered into the honing drying unit while honing the dried slurry or filter cake. Preferably, the surface coating agent is continuously metered into the 磨# grinding drying unit. In this embodiment, the feed rate of the surface coating agent is dependent on factors such as honing drying conditions, surface coating agents, etc., and the feed rate of the surface coating agent can be readily known and familiar to those skilled in the art. Variable choice. In general, the surface coating amount introduced into the honing and drying unit is effective for producing a honed dry coating comprising a surface coating agent of from about 5% to about 5.0% by weight based on the weight of the uncoated ATH. The amount of ATH particles. For example, 1 °/ used here. The degree of coating means that 1 kg of surface coating agent, i.e., fat -11-200806581 acid, is added to a slurry or filter cake containing 1 〇 kg of ATH, so that 1 kg of coated ATH is prepared. Thus, coated honed dry ATH from 15% by weight of fatty acid containing 55% by weight of ATH is used to add f% by weight of fatty acid to the slurry or filter cake. In other words, 0.55 fatty acid was added to 100 kg of a slurry containing 55 kg of uncoated ATH. The amount of surface coating agent typically employed herein is in the range of from about 0.25 to about 3% by weight, based on the weight of the slurry or filter cake ATH, preferably in the range of from about 5% to about 2.0% by weight. If the surface φ fatty acid/oxane derivative is combined, the surface coating slurry or filter cake used herein has a weight of uncoated ATH of from about 0.3 to about 1,500 Å, preferably from about 0.5 on the same basis. To about 3.0 honing and drying, "honing and drying" ("^11-〇11^1^) and "mill-dried" as used herein means that the ATH particles in the slurry or filter cake are in the presence of a watch. The turbulent flow of the turbulent drying unit is simultaneously enthalpy. The honing drying unit includes a rotor that is rigidly mounted at a high peripheral speed. The rotational movement in combination with the high air output will flow through the extremely fast air whirl, which drives the slurry to be dried and coated, accelerates, and distributes and dries the slurry or filter cake to produce coated ATH particles. After it has been completely dried, it is honed and dried. The particles are transported out of the honing machine by turbulent air and separated by air and steam using conventional filters. After another embodiment of the present invention is completely dried, the ATH granules are subjected to honing and drying, and the ash particles are irritated by a flow of i 10.1 g or a filter cake to humiliate 0.55 kg of the fat liquid or the filter cake is not coated as the same paint. The amount of the fat agent is 5% by weight: the amount of % is dried by the dry surface coating agent and dried by the solid shaft hot air transfer liquid or the filter cake is covered and dried. The i ATH system is self-heating, and has been transported in the gas- 12-200806581 The air sorter integrated into the honing machine is then transported out of the honing machine by turbulent air and separated from the hot air and steam using a conventional filter system. ~ The output of hot air for honing the drying unit is generally greater than about 3,000 B m 3 /hour, preferably greater than about 5,000 〇. B m3 / hour, more preferably greater than about 3,000 Bm3 / hour to about 40,000 Bm3/hour, and most preferably from about 5,000 Bm3/hour to about 30,000 Bm3/hour. To achieve this high output, the rotor of the honing and drying unit typically has a greater than about 40 meters per second, preferably greater than about 60 meters per second, more preferably greater than about 70 millimeters per second, and most preferably about 70 meters per second. The peripheral speed in the range of seconds to about 140 m/s. The high rotational speed of the rotor and the high hot air output result in a hot air flow with a Reynolds number greater than about 3,000. The temperature of the hot gas used to honed the drying unit is typically greater than about 15 ° C, preferably greater than about 270 ° C. In a more preferred embodiment, the temperature of the hot gas stream is in the range of from about 150 it to about 550 T:, preferably in the range of from about 270X: to about 500 °C. The ATH granules are dried by coating honing. • Drying the dried slurry or filter cake in the presence of a surface coating agent as described above to produce coated honed dry ATH granules. Thus, in one embodiment, the invention is directed to coated honed dry ATH particles characterized by having d5 小 less than about 15 microns. The coated honed dry ATH particles produced in accordance with the present invention may also be characterized as having d5G in the range of from about 0.5 to 2.5 microns. In a preferred embodiment, the coated honed dry ATH particles produced in accordance with the present invention have a d5 range in the range of from about 1.5 to about 2.5 microns, more preferably from about 1.8 to about 2.2 microns. In other preferred embodiments, the coated 硏-13-200806581 mill dried ATH granules of the present invention have a range of from about 3.4 to about 2.0 microns, more preferably from about 1.4 to about 1.8. D5 微米 in the micrometer range. In still other preferred embodiments, the coated honed dry ATH particles produced by the present invention have a d5 range in the range of from about 0.5 to about 1.8 microns, more preferably from about 0.8 to about 1.4 microns. The coated honed dry ATH particles in accordance with the present invention are also characterized by a degree of coating of a surface coating agent having a range of from about 0.05 to about 5.0 weight percent, based on the weight of the coated honed dry ATH particles. The coated honed dry ATH particles in accordance with the present invention may also be characterized as having a BET surface area ratio ("BET") ranging from about 1 to about 30 square meters per gram as measured by DIN-66 131. In certain embodiments, the BET is in the range of from about 3 to about 6 square meters per gram, more preferably from about 3.5 to about 5.5 square meters per gram. In other embodiments, the BET is in the range of from about 6 to about 9 square meters per gram, more preferably from about 6.5 to about 8.5 square meters per gram. In still other embodiments, the BET is in the range of from about 9 to about 15 square meters per gram, more preferably from about 10.5 to about 12.5 square meters per gram. It should be noted that all particle size measurements disclosed herein, i.e., d5G, can be measured by laser diffraction using a C i 1 a s 1 0 6 4 L laser spectrometer from Q u a n t a c h r 〇 m e . Typically this step can be carried out by first introducing a suitable water-dispersant solution (prepared see below) into the sample preparation vessel of the apparatus. Then select the standard measurement called “Particle Expert” and also select the measurement model “Range 1” and then select the internal parameters of the device that are suitable for the expected particle size distribution. It should be noted that during the measurement, the sample is typically exposed to the ultrasonic wave for about 60 seconds during the dispersion and during the measurement. After the background measurement is completed, about 75 to about 100 milligrams of the sample to be measured is placed in a sample container with a water/dispersant solution and measured at 14-200806581. The water/dispersant solution can be prepared by first preparing a concentrate from 500 grams of Calgon from KMF Laborchemie and 3 liters of CAL Polysalt' from BASF. This solution was made up of 1 liter of deionized water. 100 ml of the original 10 liters was taken and then further diluted to 10 liters with deionized water, and this final solution was used as the above water-dispersant solution. Coating with honed dry ATH granules The coated honed dry ATH granules according to the present invention can be used as a flame retardant in various synthetic resins. Thus, in one embodiment, the invention relates to a flame retardant polymerization comprising at least one, in some embodiments, only one synthetic resin, and a flame retardant amount of coated honed dry ATH particles in accordance with the present invention. Formulations, and molded and/or extruded articles made from flame retardant polymer formulations. The flame retardant coated honed dry ATH granules generally represent from about 5% by weight to about 90% by weight, preferably from about 20% by weight, based on the weight of the flame retardant polymer formulation. A range of about 70% by weight. In a preferred embodiment, the amount of flame retardant is on the same basis as the range of from about 30% by weight to about 65% by weight of the coated honed dry ATH particles. Thus, the flame retardant polymer formulation generally comprises at least one synthetic resin in the range of from about 1 Torr to about 95% by weight, preferably from about 30% to about 10% by weight, based on the weight of the flame retardant polymer formulation. The range of 40% by weight, more preferably at least one synthetic resin in the range of from about 35 to about 70% by weight based on the same calculation basis. Non-limiting examples of thermoplastic resins in which ATH particles can be used include polyethylene, ethylene-propylene copolymers, C2 to C8 olefins (α-olefins) -15-200806581 Polymers and copolymers (such as polybutene, poly( 4-methylpentene-1), etc., copolymer of these olefins and diene, ethylene-acrylate copolymer, polystyrene, ABS resin, AAS resin, AS resin, MBS resin, ethylene-vinyl chloride Copolymer resin, ethylene-vinyl acetate copolymer resin, ethylene-vinyl chloride-vinyl acetate graft polymer resin, vinylidene chloride, polyvinyl chloride, chlorinated polyethylene, vinyl chloride-propylene copolymer, vinyl acetate Resin, phenoxy resin, etc. Further examples of suitable synthetic resins include thermosetting resins such as epoxy resins, phenol resins, melamine resins, unsaturated polyester resins, alkyd resins, and urea resins, and natural or synthetic rubbers such as EPDM, butyl rubber, and isoprene. Diene rubber, SBR, NIR, urethane rubber, polybutadiene rubber, acrylic rubber, polyoxyxene rubber, also include fluoroelastomers, NBR' and chlorosulfonated polyethylene. It further comprises a polymerization suspension (latex). Preferably, the synthetic resin is a polyethylene-based resin, such as high-density polyethylene, low-density polyethylene, olefin, linear low-density polyethylene, ultra-low-density poly-ethylene, EVA ( Ethylene-vinyl acetate resin), EEA (ethylene-ethyl acrylate resin) Φ, EMA (ethylene-methyl acrylate copolymer resin), EAA (ethylene-acrylic acid copolymer resin), and ultrahigh molecular weight polyethylene; and C2 Polymers and copolymers of C8 suspected hydrocarbons (α-olefins), such as polybutene and poly(4-methylpentene-1), polyvinyl chloride and rubber. In a more preferred embodiment, the synthetic resin is a polyethylene based resin. The flame retardant polymer formulation may also contain other additives commonly used in the art. Non-limiting examples of other additives suitable for use in the flame retardant polymer formulations of the present invention include extrusion aids such as polyethylene wax, S i as the primary extrusion aid, fat-16 - 200806581 acid; coupling agents such as amines Base-, vinyl- or alkyl-decane or maleic acid graft polymer; barium stearate or calcium stearate; organic peroxide; dye stomach; pigment; Heat stabilizer; antioxidant; antistatic agent; strengthening agent; metal scavenger or passivating agent; impact modifier; processing aid; mold release aid, lubricant; anti-blocking agent; other flame retardant; Agent; plasticizer; flow aids, etc. If desired, a nucleating agent such as calcium citrate or indigo may also be included in the flame retardant polymer formulation. The ratio of other optional additives is conventional and can be varied to meet any particular condition. The method of incorporation and addition of the components of the flame retardant polymer formulation, and the method of molding are not critical to the invention, and can be known in any art, as long as the method of choice involves homogeneous mixing and molding. For example, a Buss Ko-kneader, an internal mixer, a Farr el continuous mixer, or a twin screw extruder, or in some cases a single screw extruder or a two-roll honing machine, may be used to mix the above components and select The additive, if used, is then molded into a flame retardant polymer formulation in a subsequent processing step. In addition, the flame retardant polymer formulation ® molded article can be used after manufacturing applications such as drawing, embossing, coating, printing, electroporation, perforation, or cutting. The kneaded mixture may also be subjected to inflation molding, injection molding, extrusion molding, blow molding, compression molding, rotational molding, or calender molding. In the case of extruding articles, it is possible to use any extrusion technique known to be effective for synthetic resins for flame retardant polymer formulations. In one exemplary technique, a synthetic resin, honed dry ATH granules are compounded with optional ingredients (if selected) in a laminating machine to form a flame retardant resin formulation. The flame retardant resin formulation is then heated to a molten state in an extruder of -17-200806581, and then the molten flame retardant resin formulation is extruded through a selective die to form an extruded article, or coated with, for example, a metal for data transfer. Line or fiberglass. The above description is directed to a number of specific embodiments of the invention. Those skilled in the art will appreciate that they can be designed to be otherwise effective in the spirit of the present invention. It should also be noted that the preferred embodiments of the present invention are intended to cover any range of any lower amount to any higher amount. The following examples describe the invention but are in no way limiting. EXAMPLES Unless otherwise indicated, all d5〇, BET, oil absorption, etc. were measured in accordance with the above techniques. The "phr" used herein is a shorthand for "parts per hundred resin." Example 1 A 420 liter/hour slurry (containing 5% by weight of ATH based on the total weight of the slurry) and water were fed to a dry honing machine. The ATH in the slurry had a BET surface area ratio of 3.9 m 2 /g and a median particle size of 1.8 μm Φ before dry honing. The honing machine operates under conditions including an air flow rate of 41 00-4200 Bm3/small time, a temperature in the range of 290 to 3 20 °C, and a rotor speed of 80 m/s. The coating agent is introduced into the honing drying unit simultaneously and continuously before the slurry. It used a fatty acid (P. r i s t e r e n e 4 9 0 0 from U n i c h e m a ) and a polyoxygenated oil (AK 3 50 from Wacker) as a coating agent. The feed rate of the fatty acid is selected to result in a coating level of 1 · 重量 by weight based on the weight of the uncoated ATH in the slurry. The feed rate of the polyoxygenated oil was selected to produce a degree of coating of 0.5% by weight of the polyoxygenated oil based on the weight of the uncoated ATH in the slurry of -18-200806581. The two coating agents are fed into the honing drying unit while approaching the slurry inlet. The coated honed dry aluminum hydroxide particles are collected by a hot gas stream through an air filtration system. Example 2 In a general manner well known to those skilled in the art, 100 phr (about 39 8.8 grams) of ethylene vinyl acetate (EVA) EscoreneTM Ultra UL001 from ExxonMobil was obtained from a two-roll honing machine W150M from Collin. 19 mixing 150 phr (about 5 98.2 grams) of the inventive aluminum hydroxide grade produced in Example 1 with about 0.75 phr (about 3.8 grams) of antioxidant Ethanox® from Albemarle Corporation over a period of about 20 minutes. 310. The temperature of the two rolls was set to 130 °C. The resulting compound is removed from the honing machine and further reduced in size after cooling to room temperature to obtain pellets suitable for compression molding in a two-stage press, or fed to an experimental extruder for further evaluation. Beading. To determine the mechanical properties of the flame retardant resin formulation, the pellet was extruded into a 2 mm thick strip using a Haake Polylab System with a Haake Rheomex extruder. The test strip according to DIN 5 3 5 04 is obtained by perforating the strip. The results of this experiment are shown in Table 1 below. Example 3 - Comparison 1 100 phr (approximately 3 98 · 8 g) of ethylene vinyl acetate from ExxonMobil was obtained from Collin's two-roll honing machine W150M. EscoreneTM Ultra UL 001 19 Mix 150 phr (approximately 5 98.2 grams) of uncoated mash during 20 minutes. The uncoated AT -19-19-200806581 used in this comparative example had the same BET and d5G 如 as in Example 1 before coating, i.e., each of 3.9 m 2 /g and 1.8 μm. In a two-roll honing machine mixing system, in a general manner familiar to those skilled in the art B, with 0.75 phr (about 3 · 0 g)

Albemarle Corporation's antioxidant Ethanox® 310 is complete. The temperature of the two rolls was set to 130 °C. The resulting compound is removed from the honing machine and further reduced in size after cooling to room temperature to obtain pellets suitable for compression molding in a two-stage press, or fed to an experimental extruder for further evaluation. Beading. To determine the mechanical properties of the flame retardant resin formulation, the Haake Polylab System of the Haake Rheomex extruder extruded the pellet into a 2 mm thick strip. The test strip according to DIN 5 3 5 04 is obtained by perforating the strip. The results of this experiment are shown in Table 1 below. Example 4 - Comparison 2 100 phr (about 3 9 8.8 g) of ethylene vinyl acetate (EVA) EscoreneTM ultra UL00119 from ExxonMobil was mixed in a two-roll honing machine W150M from Collin. 150 phr was mixed during about 20 minutes. (about 5 9 8 2 g) coated with ATH. This non-inventive ATH coating was carried out in the conventional manner using the same coating agent and degree of Example 1, but was carried out in accordance with the teachings of U.S. Patent No. 5,827,906. The ruthenium used in this comparative example had the same BET and d5 Å as in Example 1 before coating, i.e., each of 3.9 m 2 /g and 1.8 μm. In a two-roll honing machine mixing system, in a general manner familiar to those skilled in the art, with 0.75 phr (about 3.0 gram) from 八匕6 111&1*16(:〇"〇1^11〇11 The antioxidants were completed at £111 & 11 〇 \@310. The temperature of the two rolls was set to 130 ° C. The resulting compound was removed from the honing machine and further reduced in size after cooling to room temperature. It is suitable to compress the molded pellets in the press of the two platform-20-200806581, or to feed the experimental extruder to further evaluate the extruded strip. In order to determine the mechanical properties of the flame retardant resin formulation, use Haake Rheomex The Haake Polylab System of the extruder extrudes the granules into a 2 mm thick strip. The strips are perforated to obtain a test strip according to DIN 5 3 5 04. The results of this experiment are shown in Table 1 below. Table 1 Comparison 1 (uncoated覆) Comparison 2 (Priority Coating) The melting rate of the material of the present invention is @190°C/10 kg (g/10 min) 1.6 2.3 3 Tensile strength (MPa) 9 9.6 10.0 Burst elongation (%) 125 497 510 LOI ( % O2) 38 35 39 Resistance before water aging (Ohnrcm) 3.1 X 1011 8.3 X 1013 1.0 xlO14 7d@70°C Water aging resistance (Ohnvcm ) 7.1 X 108 2.5 X 1012 63 X 1012 suction; d < sex (%) 3.0 2.0 1.3

It can be seen in Table 1 that the aluminum hydroxide of the present invention according to the present invention provides optimum rheological, mechanical, flame retardant, and electrical properties due to relatively uniform coating, and exhibits the lowest water absorption. Melting flow rate according to DIN-ISO 1133, tensile strength and elongation at break according to DIN 5 3 5 04 and EN ISO 5 27, limited oxygen index LOI for 150 X 6x3 cubic millimeters according to ISO 45 89-2, and electrical properties (Resistance after 7 days of water aging at 70 ° C) is measured in accordance with DIN 5 3 4 82/VDE 03 03 part 3. -twenty one-

Claims (1)

200806581 X. Patent Application Range: 1. An ATH particle comprising: * a) a surface coating agent selected from the group consisting of i) fatty acids; hydrazine) a oxane derivative; and in) a mixture thereof, wherein the ATH The granules are produced by honing and drying a slurry or filter cake containing from about 1 to about 85% by weight of ATH granules, based on the slurry or filter cake, in the presence of a surface coating agent. 2. ATH granules according to the scope of claim 2, wherein Φ d5 ATH of the ATH particles is less than about 15 microns, as determined by laser diffraction according to 130 9276: and a BET surface area ratio of from about 1 to about 30 square meters / The range of grams is as determined by DIN-66132. 3. The ATH granule according to claim 1, wherein the fatty acid is selected from the group consisting of a saturated fatty acid, an unsaturated fatty acid, and a fatty acid having an additional functional group. 4. The ATH granule of claim 3, wherein the fatty acid contains from about 8 to about 30 carbon atoms and the decane derivative is selected from the group consisting of oligoalkyl oxane, polydialkyl oxime Alkane, polyalkylaryl siloxane or polydiaryl oxalate. 5. The ATH particle of claim 4, wherein the surface coating agent is a combination of a fatty acid and a decane derivative. 6. The ATH particle of claim 1, wherein the surface coating agent is a combination of a fatty acid and a decane derivative. 7. The ATH particle of claim 1, wherein the slurry or filter cake is derived from a method involving the manufacture of ATH particles by precipitation and filtration. -22-200806581 8. The ATH granule according to claim 1, wherein the filter cake is obtained from a method comprising the following: a) dissolving crude aluminum hydroxide in caustic to form sodium aluminate solution, Cooling and filtering, thereby forming a sodium aluminate solution having a Na20 to Α12〇3 molar ratio ranging from about 1.4:1 to about 1.55:1; b) adding a sodium aluminate solution in an amount of about 1 gram of cerium seed per liter of sodium aluminate solution to about 3 grams of ATH grain per liter of sodium aluminate solution, thus forming a method mixture in which sodium aluminate is formed When the liquid is at a liquid temperature of about 4 5 to about 80 ° C, the ATH grain is added to the sodium aluminate solution; the sodium aluminate containing the grain is stirred for about 100 hours, or until the ratio of Na20 to A12 〇3 mole is A range of from about 2.2:1 to about 3:5:1, thus forming an ATH suspension comprising from about 80 to about 16 g/L of ATH on a suspension; d) washing and filtering the ATH suspension, such Forming a filter cake; and e) optionally washing the filter cake one or more times with water. 9. The ATH granule according to claim 8 wherein the syrup is obtained by repulping the filter cake with water. 1 〇 A A Η granule according to item 8 of the patent application, wherein the syrup is obtained by repulping the filter cake, the repulping comprising adding at least one dispersing agent to the filter cake. The granule of the ninth aspect of the invention, wherein the dispersant is selected from the group consisting of polyacrylate, organic acid, naphthalene sulfonate/formaldehyde condensate, fatty alcohol-polyglycol ether, polypropylene-ring Oxyethane, polyglycol ester, polyamine _ ethylene oxide, phosphate ester, polyvinyl alcohol. -23-200806581 1 2 ATH granules according to claim 8 wherein the syrup is formed by repulping the filter cake in a combination of water and a dispersing agent. #13. The granule of claim 8 wherein the bismuth particles in the filter cake have a BET in the range of from about 1.0 to about 30 square meters per gram and a d50 in the range of from about 1.5 to about 2.5 microns. 14. The granule of claim 1 wherein the bismuth particles in the syrup have a BET in the range of from about 1.0 to about 30 square meters per gram and a d50 in the range of from about 1.5 to about 2.5 microns. Φ- 15. A method comprising: a) honing and drying in a honing drying unit in the presence of a surface coating agent selected from the group consisting of i) fatty acids; ii) decane derivatives; and iii) mixtures thereof A slurry or filter cake containing from about 1 to about 85% by weight aluminum hydroxide, based on the slurry or filter cake, is thus produced to produce coated honed dry ATH particles. The method of claim 15, wherein the honing drying unit is operated under conditions comprising a hot gas flow output of greater than about 3,000 Bm 3 /hour and a rotor peripheral speed of greater than about 40 m / s, Wherein the hot gas stream has a temperature greater than about 150 ° C and a Reynolds number greater than about 3000. The method of claim 15, wherein the honing and drying unit is operated under conditions comprising a hot gas flow output of greater than about 5,000 Bm 3 /hour and a rotor peripheral speed of greater than about 60 m / sec, Wherein the hot gas stream has a temperature greater than about 270 ° C and a Reynolds number greater than about 3,000. 18. The method of claim 15, wherein the honing drying unit is a condition comprising a hot gas flow output of greater than about 5000 Bm3/hr to about 7000 Bm3/hr and a rotor peripheral speed of greater than about 70 m/s. The following operation, -24-200806581 wherein the hot gas stream has a temperature of from about 270 ° C to about 450 ° C and a Reynolds number of greater than about 3 Torr. ^ 1 9 · The method of claim 15 wherein the d5G coated with honed dry ATH particles is less than 15 microns, as measured by laser diffraction according to ISO 9276; and coated by honing The BET particles have a BET surface area ratio in the range of about 1 to about 30 square meters per gram as determined by DIN-66132. The method of claim 15, wherein the coated honed dry ATH particles comprise a surface coating in the range of from about 0.05 to about 5 weight percent based on the uncoated ATH particles in the slurry or filter cake. Covering agent. The method of claim 15, wherein the fatty acid is selected from the group consisting of a saturated fatty acid, an unsaturated fatty acid, and a fatty acid having an additional functional group. 22. The method of claim 15 wherein the The fatty acid contains from about 8 to about 30 carbon atoms and the decane derivative is selected from the group consisting of oligoalkyl oxanes, polydialkyl oxanes, polyalkylaryl oxanes or polydiaryl cleavage Oxygen oxime. 23. The method of claim 15, wherein the surface coating agent is a combination of a fatty acid and a decane derivative. 24. The method of claim 15, wherein the slurry or filter cake is obtained from a method involving the manufacture of ATH particles by precipitation and filtration. 25. The method of claim 24, wherein the filter cake is obtained from a method comprising: a) dissolving the crude aluminum hydroxide in caustic to form a sodium aluminate solution, which is cold--25- 200806581 However, it is filtered to form a sodium aluminate solution having a Na20 to Al2〇3 molar ratio of about 1 · 4 : 1 to about 1 · 5 5 : 1; b) ATH grains per liter of sodium aluminate solution Adding a sodium aluminate solution to the amount of about 3 grams of ATH kernel per liter of sodium aluminate solution, such as a method mixture, wherein the sodium citrate solution is from about 45 to about 80. Adding ATH grain to sodium aluminate solution; c) disturbing the sodium salt containing the good grain for about 100 hours, or until the ratio of N a 2 〇 to Ah 〇 3 mole is about 2 · 2 : 1 to about 3 · 5 : 1 Forming an ATH suspension comprising from about 80 to about 160 grams per liter of ATH; d) washing and filtering the ATH suspension to form a cake; and e) optionally washing the filter cake with water One or more times. 26. The method of claim 25, wherein the slurry is obtained by repulping the filter cake with water. 27. The method of claim 25, wherein the slurry is obtained by repulping the filter cake, the repulping comprising adding at least one dispersant to the filter cake. The method of claim 27, wherein the dispersant is selected from the group consisting of polyacrylates, organic acids, naphthalenesulfonate/formaldehyde condensates, fatty alcohol-polyglycol ethers, polypropylene-epoxy Ethane, polyglycol ester, polyamine-ethylene oxide, phosphate ester, polyvinyl alcohol. 29. The method of claim 25, wherein the slurry is formed by repulping the filter cake in a combination of water and a dispersant. The method of claim 15, wherein the filter cake or the ATH granule of the slurry -26-200806581 has a BET ranging from about 1 〇 to about 30 square meters per gram and a BET of about 1.5 to about Dso in the 2·5 micron range. 3 1 The method of claim 15 wherein the filter cake or the slurry and the surface coating agent are introduced into the honing drying unit by: 丨) continuously measuring the surface coating agent to In the honing drying unit; 11) continuously introducing the filter cake or the slurry into the honing drying unit; iH) continuously introducing the surface coating agent into the honing drying unit in a batch manner; iv) The filter cake or the slurry is continuously introduced into the honing drying unit in batch mode; or v) a combination of i)-iv). The method of claim 15, wherein the filter cake or the slurry is honed and dried in the honing drying unit for a while before the surface coating agent is introduced into the honing drying unit. The method of claim 15, wherein the slurry or filter cake is combined with the surface coating agent prior to honing and drying. 3 4. A method for producing coated aluminum hydroxide particles, comprising: a) introducing a slurry or filter cake comprising from about 1 to about 85 weight percent aluminum hydroxide, based on a filter cake or slurry, In the honing drying unit; b) simultaneously introducing a surface coating agent selected from the group consisting of i) fatty acids; ii) a oxane derivative; and iii) a mixture thereof before or after the introduction of the slurry or filter cake And c) honing the slurry or filter cake in the presence of the surface coating agent until the coated honed dry aluminum hydroxide particles containing the surface coating agent are produced. 35. The method of claim 34, wherein the honing drying unit is comprised of a hot gas flow output comprising greater than about 3,000 B m3 /hour, and a rotor peripheral speed greater than about -27 - 200806581 40 m / sec. Operating under conditions wherein the hot gas stream has a temperature greater than about 15 〇 ° C and a Reynolds number greater than about 3,000. 36. The method of claim 34, wherein the honing drying unit is a condition comprising a hot gas flow output of greater than about 5000 Bm3/hr to about 7000 Bm3/hr and a rotor peripheral speed of greater than about 70 m/s. The operation is wherein the hot gas stream has a temperature of from about 270 ° C to about 450 ° C and a Reynolds number of greater than about 3,000. The method of claim 4, wherein the d5G coated with honed dry ATH particles is less than 15 microns, as determined by laser diffraction according to ISO 9276; and coated honed dry ATH particles The BET surface area ratio is in the range of about 1 to about 30 square meters per gram as determined by DIN-66 1 32. The method of claim 3, wherein the coated honed dry ATH particles comprise a surface coating agent in the range of from about 0.05 to about 5 weight percent, based on uncoated honed dry ATH particles. . 3. The method of claim 4, wherein the fatty acid is selected from the group consisting of a saturated fatty acid, an unsaturated fatty acid, and a fatty acid having an additional functional group. 4. The method of claim 39, wherein The fatty acid contains from about 8 to about 3 carbon atoms and the decane derivative is selected from the group consisting of oligomeric polysiloxanes, polydialkyl siloxanes, polyalkylaryl oximes, or polydiaryls. Oxane. The method of claim 34, wherein the surface coating agent is a combination of a fatty acid and a decane derivative. -28-200806581 42. The method of claim 34, wherein the slurry or filter cake is obtained from a method involving the manufacture of ATH particles by precipitation and filtration. 43. The method of claim 42, wherein the filter cake is obtained from a method comprising: a) dissolving the crude aluminum hydroxide in caustic to form a sodium aluminate solution, cooling and filtering, Forming a sodium aluminate solution having a Na20 to Al2〇3 molar ratio ranging from about 1 · 4 : 1 to about 1.5 5 : 1; b) adding ATH grain to about 1 gram of ATH grain per liter of sodium aluminate to about 3 grams of ATH grain per liter of sodium aluminate solution, thus forming a method mixture in which sodium aluminate is formed The ATH grain is added to the sodium aluminate solution at a liquid temperature of about 4 5 to about 80 ° C; c) the sodium aluminate containing the grain is stirred for about 100 hours, or until Na20· is for A1 2 Ο 3 The ratio of ears is from about 2 · 2 : 1 to about 3.5 : 1 , thus forming an ATH suspension comprising from about 80 to about 160 grams per liter of suspension; d) washing and filtering the ATH Suspension, thus forming a filter cake; and e) optionally washing the filter cake one or more times with water. 44. The method of claim 43, wherein the slurry is obtained by repulping the filter cake with a) additional water; b) additional dispersing agent; or c) a) and b). 45. The method of claim 44, wherein the slurry is obtained by repulping the filter cake by adding at least one dispersant to the filter cake, the dispersant being selected from the group consisting of polyacrylates, organic acids, Naphthalene sulfonate/formaldehyde condensate, fatty alcohol-polyglycol ether, polypropylene-ethylene oxide, polyglycol ester, polyamine _29-200806581 Ethylene oxide, phosphate ester, polyvinyl alcohol. The method of claim 5, wherein the A TH particles in the filter cake or slurry have a BET in the range of from about 1.0 to about 30 square meters per gram and a d50 in the range of from about 1.5 to about 2.5 microns. 4 7 · The method of claim 34, wherein the method is continuous. The method of claim 4, wherein the filter cake or the slurry and the surface coating agent are introduced into the honing drying unit by: i) continuously measuring the surface coating agent to The honing drying unit; ii) continuously introducing the filter cake or the slurry into the honing drying unit; iii) continuously introducing the surface coating agent into the honing drying unit in a batch manner; iv) The filter cake or the slurry is continuously introduced into the honing drying unit in batch mode; or v) a combination of i)-iv). The method of claim 4, wherein the coated honed dry ATH particles are used in a flame retardant polymer formulation. a flame retardant polymer formulation comprising a synthetic resin and a coated honed dry ATH granule, wherein the coated honed dry ATH granule is in the presence of a surface coating agent in 硏The pulverizing drying unit is honed and dried to prepare a slurry or filter cake containing about 1 to about 85% by weight of aluminum hydroxide based on the paddle or filter cake. 5. The flame retardant polymer formulation of claim 50, wherein the flame retardant polymer formulation comprises from about 10 to about 95 weight percent of the coated honed dry ATH particles, and The synthetic resin ranges from 5 to about 90% by weight, based on the total weight of the flame retardant polymer formulation. 52. The flame retardant polymer formulation of claim 50, wherein the -30-200806581 surface coating agent is selected from the group consisting of i) a fatty acid; i i) at least one of a decane derivative 〇 P 5. The flame retardant polymer formulation of claim 5, wherein the flame retardant polymer formulation further comprises at least one i} extrusion aid; π) fatty acid; iii) coupling agent; iv) hard Barium sulphate; ν) calcium stearate; vi) organic peroxide; viii) dye; ix) pigment; χ) 塡; χ丨) blowing agent; xii) deodorant; xiii) thermal stabilizer; Xiv) antioxidant; χν) antistatic agent; xvi) enhancer; xvii) metal scavenger or passivator; xviii) impact modifier; xix) processing aid; xx) mold release aid; xxi) lubricant; Anti-blocking agent; xxiii) other flame retardants; xxiv) UV stabilizer; XXV) plasticizer; xxvi) flow aid; xxv) nucleating agent: and XXV i) others. 5 4 - A molded or extruded article made from a flame retardant polymer formulation of claim 50. 5 5 . A molded or extruded article made from a flame retardant polymer formulation of claim 5 of the patent application. # 56.—The honing drying unit produces a coated honed dry ATH containing a surface coating agent from a slurry or filter cake containing from about 1 to about 85 weight percent ATH granules by weight of the slurry or filter cake. For the use of granules, the surface coating agent is selected from the group consisting of i) fatty acids, ii) decane, and iii) a mixture of i) and hydrazine. -31 - 200806581 VII. Designation of representative representatives: (1) The representative representative of the case is: None. (2) A brief description of the symbol of the representative figure: Μ 〇 Φ 8. If there is a chemical formula in this case, please disclose the chemical formula that best shows the characteristics of the invention: