v v200811047 九、發明說明： 【發明所屬之技術領域】 本發明係關於製造礦物阻燃劑。更特別，本發明係關 於用於製造氫氧化鋁阻燃劑之新穎方法。 【先前技術】 氫氧化鋁具有各種交替名稱例如鋁水合物，鋁三水合 物，三氫氧化鋁等，但是一般稱爲A TH。顆粒狀氫氧化鋁 ，下文中稱爲ATH供給許多用途在許多材料中，舉例而言 ，例如紙、樹脂、橡膠，塑膠等中作爲塡料。ATH的最廣 布用途之一是在合成樹脂例如塑膠及電線電纜中作爲阻燃 劑。 ATH的工業上應用性已久熟知歷經相當多的時間。在 阻燃領域方面，使用ATH粒子在合成樹脂例如塑膠中及在 電線和電纜應用方面來授予阻燃性質。含有ATH粒子之合 成樹脂的配合性能（compounding performance)及黏度是決 定性特質其與ATH粒子相關連。在合成樹脂工業中，爲了 顯著的原因，要求較佳之配合性能日漸增加。 因此，當要求較佳之配合性能增加時，該項技藝中有 一種需要就是迎合此等要求，製造A TH粒子的方法。 【發明内容】 本發明係關於用於製造乾式硏磨之ATH之方法。該方 法通常包括： a)噴霧乾燥氫氧化鋁漿體或濾餅以產生經噴霧乾燥之 氫氧化鋁粒子；及 -5- 200811047 b)乾式硏磨該經噴霧乾燥之氫氧化鋁粒子因此產生乾 式硏磨之ATH粒子。 其中該乾式硏磨之ATH具有自約0.09至約0.33 μιη範 圍內之中値孔隙半徑（「r5〇」）及 i)自約3至約6m2/g的BET比表面積；及 自約3 90至約480mm3/g的在約1 000巴之最大比孔隙 體積； 或 φ ii)自約6至約9m2/g的BET比表面積；及 自約400至約600mm3/g的在約1000巴之最大比孔 隙體積； 或 iii)自約9至約15m2/g的BET比表面積；及 自約300至約700mm3/g的在約1000巴之最大比孔 隙體積。 在另外實施例中，本發明係關於用於製造乾式硏磨之 φ ΑΤΉ之方法。該方法通常包括： a) 噴霧乾燥氫氧化鋁漿體或濾餅以產生經噴霧乾燥之 氣氧化銘粒子；及 b) 乾式硏磨該經噴霧乾燥之氫氧化鋁粒子因此產生乾 式硏磨之ATH粒子， 其中該乾式硏磨之ATH粒子具有： i)自約3至約6m2/g的BET比表面積；及 自約390至約480mm3/g的在約1000巴之最大比孔隙 體積； -6- 200811047 ， 或 ii) 自約6至約9m2/g的BET比表面積；及 自約400至約600mm3/g的在約1 000巴之最大比孔隙 體積； 或 iii) 自約9至約15m2/g的BET比表面積；及 自約300至約700mm3/g的在約1000巴之最大比孔隙 體積。 _ 【實施方式】 ATH粒子與樹脂的潤濕性係基於ATH粒子的形態，關 於此，發明人意外地發現經由使用本發明的方法，相對於 目前可供利用之ATH粒子，可製造具有改良潤濕性之ATH 粒子。雖然不希望受學說所約束，關於此，發明人確信此 改良之潤濕性可歸因於經由本文中所揭示之方法所產生之 ATH粒子的形態改良。 漿體和濾餅 ® 在本發明的一實施例中，將含有ATH粒子之漿體或濾 餅噴霧乾燥以產生經噴霧乾燥之ATH粒子，然後將它乾式 硏磨，因此產生乾式硏磨之ATH粒子。一較佳實施例中， 將漿體噴霧乾燥但在另外較佳實施例中，將濾餅噴霧乾燥 漿體或濾餅典型含有基於漿體或濾餅的總重量，範圍 自約1至約85 wt%ATH粒子。較佳實施例中，漿體或濾餅 含有範圍自約25至約70wt%ATH粒子。更佳含有範圍自約 200811047 ' 55至約65wt%ATH粒子粒子，兩者基於相同基礎。其他較 佳之實施例中，漿體或濾餅含有範圍自約 40至約 60wt%ATH粒子，更佳含有範圍自約45至約55wt%ATH粒 子，兩者基於相同基礎。更有其他較佳實施例中，漿體或 濾餅含有範圍自約25至約50wt%ATH粒子，更佳含有範圍 自約30至約45wt%ATH粒子，兩者基於相同基礎。 實施本發明時所使用之漿體或濾餅可自使用以製造 ATH粒子之任何方法獲得。漿體或濾餅較佳係自一種方法 Φ 而獲得，此方法包括通過沉澱和過濾來產生ATH粒子。一 例示之實施例中，漿體或濾餅係自一種方法獲得，此方法 包括溶解粗氫氧化鋁在苛性鈉中以形成鋁酸鈉液，將其冷 卻並過濾因此形成使用於此例示實施例中之鋁酸鈉液。如 此產生之鋁酸鈉液典型具有範圍自約1.4 : 1至約1.5 5 : 1 之Na2〇對Al2〇3的莫耳比。爲了自鋁酸鈉液中沈澱ATH粒 子，將ATH晶種粒子加至鋁酸鈉液其數量在自每升之鋁酸 鈉液約1克的ATH晶種粒子至每升之鋁酸鈉液約3克的 m W ΑΤΉ晶種粒子之範圍內，因此形成程序混合物（process mixture)。當鋁酸鈉液是在自約45至約80°C的液溫時，將 ATH晶種粒子加至鋁酸鈉液。在添加ATH晶種粒子之後， 將該程序混合物攪拌歷約100小時或者直至Na2〇對Al2〇3 之莫耳比是在自約2.2: 1至約3.5: 1的範圍內，因此形成 ATH懸浮液。所獲得之ATH懸浮液典型包括基於該懸浮液 ，自約80至約160g/l ATH。然而，可將ATH濃度變更屬 於上述之範圍以內。然後將所獲得之ATH懸浮液過濾並洗 -8· 200811047 滌自其中移除雜質，因此形成濾餅。可將濾餅用水洗滌一 次，或在某些實施例中，用水洗滌一次以上，較佳是用去 鹽之水（de-salted water)洗滌。然後將此濾餅直接噴霧乾燥 〇 然而，在某些較佳實施例中，可將濾餅用水再造成漿 體以形成漿體，或在一較佳實施例中，將至少一種，較佳 僅一種分散劑加至濾餅以形成具有ATH濃度在上述範圍內 之漿體。請注意，使用水和分散劑的組合而將濾餅再造成 Φ 漿體亦係在本發明的範圍以內。適合於本文中使用之分散 劑的無限制實例包括聚丙烯酸酯，有機酸，磺酸酯/甲醛 縮合物，脂肪醇-聚乙二醇醚，聚丙烯-環氧乙烷，聚乙二 醇酯，多元胺環氧乙烷，磷酸鹽、聚乙烯醇。如果漿體包 括分散劑，因爲分散劑的效果，該漿體可含有基於漿體之 總重量高達約80wt%ATH。此實施例中，剩餘的漿體或濾餅 (即，不包括ATH粒子和分散劑）典型是水，唯某些反應物 、污染物等可能自沉澱而存在。 ® 漿體或濾餅中之ATH粒子一般其特徵爲具有範圍_約v v200811047 IX. Description of the invention: [Technical field to which the invention pertains] The present invention relates to the manufacture of a mineral flame retardant. More particularly, the present invention relates to novel methods for making aluminum hydroxide flame retardants. [Prior Art] Aluminum hydroxide has various alternate names such as aluminum hydrate, aluminum trihydrate, aluminum trihydroxide, etc., but is generally referred to as A TH. Granular aluminum hydroxide, hereinafter referred to as ATH supply, is used in many materials, for example, as paper, resin, rubber, plastic, etc. as a dip. One of the most widely used uses of ATH is as a flame retardant in synthetic resins such as plastics and wire and cable. The industrial applicability of ATH has long been known for quite a considerable amount of time. In the field of flame retardancy, ATH particles are used to impart flame retardant properties in synthetic resins such as plastics and in wire and cable applications. The compounding properties and viscosity of synthetic resins containing ATH particles are decisive properties associated with ATH particles. In the synthetic resin industry, for a significant reason, a better blending performance is required. Therefore, there is a need in the art to meet the requirements for the manufacture of A TH particles when better matching performance is required. SUMMARY OF THE INVENTION The present invention is directed to a method for making ATH for dry honing. The method generally comprises: a) spray drying an aluminum hydroxide slurry or filter cake to produce spray dried aluminum hydroxide particles; and -5 - 200811047 b) dry honing the spray dried aluminum hydroxide particles thereby producing a dry form Honing the ATH particles. Wherein the dry honing ATH has a 値 pore radius ("r5〇") in the range of from about 0.09 to about 0.33 μηη and i) a BET specific surface area from about 3 to about 6 m 2 /g; and from about 3 90 to a maximum specific pore volume of about 480 mm 3 /g at about 1000 bar; or φ ii) a BET specific surface area of from about 6 to about 9 m 2 /g; and a maximum ratio of from about 400 to about 600 mm 3 /g at about 1000 bar Pore volume; or iii) a BET specific surface area from about 9 to about 15 m2/g; and a maximum specific pore volume of from about 300 to about 700 mm3/g at about 1000 bar. In a further embodiment, the invention relates to a method for making φ ΑΤΉ for dry honing. The method generally comprises: a) spray drying an aluminum hydroxide slurry or filter cake to produce a spray dried gas oxidized crystal grain; and b) dry honing the spray dried aluminum hydroxide particles thereby producing a dry honed ATH Particles, wherein the dry honed ATH particles have: i) a BET specific surface area from about 3 to about 6 m2/g; and a maximum specific pore volume of from about 390 to about 480 mm3/g at about 1000 bar; 200811047, or ii) a BET specific surface area from about 6 to about 9 m2/g; and a maximum specific pore volume of from about 400 to about 600 mm3/g at about 1000 bar; or iii) from about 9 to about 15 m2/g. The BET specific surface area; and a maximum specific pore volume of from about 300 to about 700 mm 3 /g at about 1000 bar. EMBODIMENT The wettability of ATH particles and resin is based on the morphology of ATH particles. In this regard, the inventors have unexpectedly discovered that by using the method of the present invention, it is possible to manufacture improved ATH particles with respect to currently available ATH particles. Wet ATH particles. While not wishing to be bound by the doctrine, in this regard, the inventors believe that this improved wettability can be attributed to the morphological improvement of the ATH particles produced by the methods disclosed herein. Slurry and Filter Cake® In one embodiment of the invention, a slurry or filter cake containing ATH particles is spray dried to produce spray dried ATH particles which are then dry honed to produce a dry honed ATH particle. In a preferred embodiment, the slurry is spray dried but in a further preferred embodiment, the filter cake spray dried slurry or filter cake typically contains a total weight based on the slurry or filter cake, ranging from about 1 to about 85. Wt%ATH particles. In a preferred embodiment, the slurry or filter cake contains from about 25 to about 70 weight percent ATH particles. More preferably ranges from about 200811047 '55 to about 65 wt% ATH particle particles, both based on the same basis. 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, both based on the same basis. In still other preferred embodiments, the slurry or filter cake contains from about 25 to about 50 wt% ATH particles, more preferably from about 30 to about 45 wt% ATH particles, both based on the same basis. The slurry or filter cake used in the practice of the invention can be obtained by any method used to make ATH particles. Preferably, the slurry or filter cake is obtained from a method Φ which comprises producing ATH particles by precipitation and filtration. In one exemplary embodiment, the slurry or filter cake is obtained from a process comprising dissolving the crude aluminum hydroxide in caustic soda to form a sodium aluminate solution, cooling it and filtering thereby forming the use of the illustrated embodiment. Sodium aluminate solution. The sodium aluminate solution thus produced typically has a molar ratio of Na2? to Al??3 ranging from about 1.4:1 to about 1.55:1. In order to precipitate ATH particles from sodium aluminate solution, the ATH seed particles are added to the sodium aluminate solution in an amount of about 1 gram of ATH seed particles per liter of sodium aluminate solution to about liters of sodium aluminate per liter. 3 grams of m W seed crystal particles are within the range, thus forming a process mixture. When the sodium aluminate solution is at a liquid temperature of from about 45 to about 80 ° C, the ATH seed particles are added to the sodium aluminate solution. After the addition of the ATH seed particles, the procedure mixture is stirred for about 100 hours or until the molar ratio of Na2〇 to Al2〇3 is in the range from about 2.2:1 to about 3.5:1, thus forming an ATH suspension. . The ATH suspension obtained typically comprises from about 80 to about 160 g/l ATH based on the suspension. However, the ATH concentration change can be within the above range. The obtained ATH suspension is then filtered and washed. -8·200811047 The polyester is removed therefrom to form a filter cake. The filter cake may be washed once with water or, in some embodiments, with water more than once, preferably with de-salted water. The filter cake is then spray dried directly. However, in certain preferred embodiments, the filter cake can be reconstituted with water to form a slurry, or in a preferred embodiment, at least one, preferably only A dispersant is added to the filter cake to form a slurry having an ATH concentration within the above range. It is noted that it is within the scope of the invention to re-inject the filter cake into a Φ slurry using a combination of water and dispersant. Non-limiting examples of dispersants suitable for use herein include polyacrylates, organic acids, sulfonate/formaldehyde condensates, fatty alcohol-polyglycol ethers, polypropylene-ethylene oxide, polyethylene glycol esters. , polyamine ethylene oxide, phosphate, polyvinyl alcohol. If the slurry comprises a dispersant, the slurry may contain up to about 80% by weight ATH based on the total weight of the slurry due to the effect of the dispersant. In this embodiment, the remaining slurry or filter cake (i.e., excluding ATH particles and dispersant) is typically water, although only certain reactants, contaminants, and the like may be present from the precipitate. ® ATH particles in a slurry or filter cake are generally characterized by a range of
1.0至約4.0m2/g之BET。較佳實施例中，ATH粒子具有範 圍自約1.5至約2.5m2/g之BET。漿體或濾餅中之ATH粒子 能進一步予以特徵化爲具有範圍自約2.0至約3.5μιη之d50 。較佳實施例中，漿體或濾餅中之ATH粒子具有範圍自約 1.8至約2.5μιη之d5Q。其比經由本發明所產生之乾式硏磨 之ATH粒子較爲粗糙。其他較佳實施例中，漿體或濾餅中 之ATH粒子之特徵爲具有範圍自約4.0至約8.0m2/g之BET -9- 200811047 。其他較佳實施例中，漿體或濾餅中之ATH粒子 自約5至約7m2/g之BET。此實施例中，漿體或、 ATH粒子能進一步予以特徵化爲具有範圍自約 2.5μιη之d5G。其他較佳實施例中，漿體或濾餅中： 子具有範圍自約1 . 6至約2.0 μ m之d 5 〇，其比經由 產生之乾式硏磨之ATH粒子較爲粗糙。其他較佳 ，漿體或濾餅中之ATH粒子之特徵爲具有範圍自 約14m2 /g之BET。其他較佳實施例中，漿體或 # ATH粒子具有自約9至約12m2/g之BET。此等較 中，漿體或濾餅中之ATH粒子可另外述其特徵爲 自約1 . 5至約2.0 μιη之d 5 〇。較佳實施例中，漿體 之ATH粒子具有範圍自約1.5至約1·8μιη之d50, 本發明所產生之乾式硏磨之ATH粒子較爲粗糙。 按較乾式硏磨之ATH粒子爲粗糙，其意指漿 中ATH粒子的d5G値之上限通常是至少約〇·2μιη 本發明所產生之乾式硏磨ATH粒子的d5G之上限 ® 雖然不希望受學說所約束，關於此發明人確 發明所產生之ATH粒子的改良形態是至少部分地 沉澱ATH所使用之方法。因此，雖然乾式硏磨技 技藝中係熟知，但是關於此，發明人發現經由使 所敘述之沉澱和過濾方法，包括較佳實施例’連 所敘述之乾式硏磨方法，能容易製造具有改良形 粒子，如下文所述。 噴霧乾燥BET from 1.0 to about 4.0 m2/g. In a preferred embodiment, the ATH particles have a BET ranging from about 1.5 to about 2.5 m2/g. The ATH particles in the slurry or filter cake can be further characterized as having a d50 ranging from about 2.0 to about 3.5 μηη. In a preferred embodiment, the ATH particles in the slurry or filter cake have a d5Q ranging from about 1.8 to about 2.5 μηη. It is rougher than the dry honed ATH particles produced by the present invention. In other preferred embodiments, the ATH particles in the slurry or filter cake are characterized as having a BET -9-200811047 ranging from about 4.0 to about 8.0 m2/g. In other preferred embodiments, the ATH particles in the slurry or filter cake have a BET of from about 5 to about 7 m2/g. In this embodiment, the slurry or ATH particles can be further characterized as having d5G ranging from about 2.5 μηη. In other preferred embodiments, the slurry or filter cake has a d 5 〇 ranging from about 1.6 to about 2.0 μm which is coarser than the ATH particles produced by dry honing. Preferably, the ATH particles in the slurry or filter cake are characterized by a BET having a range of from about 14 m2/g. In other preferred embodiments, the slurry or #ATH particles have a BET of from about 9 to about 12 m2/g. In such a comparison, the ATH particles in the slurry or filter cake may additionally be characterized as d 5 自 from about 1.5 to about 2.0 μηη. In a preferred embodiment, the ATH particles of the slurry have a d50 ranging from about 1.5 to about 1.8 μm, and the dry honed ATH particles produced by the present invention are relatively rough. Roughness of the ATH particles in the dry honing means that the upper limit of the d5G ATH of the ATH particles in the slurry is usually at least about 〇·2 μιη. The upper limit of the d5G of the dry honing ATH particles produced by the present invention, although not wishing to be learned Constrained, a modified form of the ATH particles produced by the inventors of the present invention is a method used to at least partially precipitate ATH. Thus, while well-known in the art of dry honing, in light of this, the inventors have discovered that it is easy to manufacture an improved shape by the precipitation and filtration methods described, including the dry honing method described in the preferred embodiment Particles, as described below. Spray drying
具有範圍 濾餅中之 1.5至約 之ATH粒 本發明所 實施例中 約8.0至 濾餅中之 佳實施例 具有範圍 或濾餅中 其比經由 體或濾餅 高於經由 〇 信經由本 可歸因於 術在該項 用本文中 同本文中 態之ATH -10- 200811047 噴霧乾燥是通常使用於製造氫氧化鋁之技術。此技術 一般包括通過使用噴嘴及/或旋轉霧化器將ATH進料霧化 ，在此之進料是硏磨之ATH漿體或濾餅。然後使經霧化之 進料與熱氣，一般是空氣接觸，然後將噴霧乾燥之ATH自 熱氣流中回收。可將霧化之進料的接觸以逆向流或同向流 方式實施，且可控制氣體溫度、霧化、接觸和氣體及/或 霧化之進料的流速來製造具有所需要產物性質之ATH粒子 〇 # 噴霧乾燥之ATH的回收可通過使用回收技術例如過濾 予以實現或直接容許噴霧乾燥之粒子散落在噴霧乾燥器中 收集’在此情況下，可將彼等取出，但是可使用任何適當 回收技術。較佳實施例中，將噴霧乾燥之ATH經由容許它 沉降’自噴霧乾燥器回收，及螺旋運送機自噴霧乾燥器中 回收它，隨後藉壓縮空氣通過管子輸送進入筒倉中。 噴霧乾燥之條件是習用之條件且具有通常知識之熟習 技藝者藉由下述所需要的ATH粒子產物品質的知識而容易 ® 選擇。通常，此等條件包括典型在2 5 0至5 5 0 °C間之入口空 氣溫度及典型在105至150。(：間之出口空氣溫度。 乾式硏磨ATH particles having a range of from about 1.5 to about 5% of the filter cake in the embodiment of the invention from about 8.0 to a preferred embodiment of the filter cake having a range or a filter cake which is higher than the passage via the body or the filter cake Spray drying of ATH -10- 200811047, which is used in this document, is a technique commonly used in the manufacture of aluminum hydroxide. This technique generally involves atomizing the ATH feed by using a nozzle and/or a rotary atomizer where the feed is a honed ATH slurry or filter cake. The atomized feed is then contacted with hot gas, typically air, and the spray dried ATH is then recovered from the hot gas stream. The contact of the atomized feed can be carried out in a countercurrent or cocurrent manner, and the gas flow, atomization, contact, and flow rate of the gas and/or atomized feed can be controlled to produce an ATH having the desired product properties. Particle 〇# Spray-dried ATH can be recovered by using recycling techniques such as filtration or directly allowing spray-dried particles to be collected in a spray dryer. In this case, they can be removed, but any suitable recycling can be used. technology. In the preferred embodiment, the spray dried ATH is recovered from the spray dryer by allowing it to settle, and the screw conveyor recovers it from the spray dryer, which is then conveyed through the tube into the silo by compressed air. The conditions of spray drying are the conditions of the conventional and skilled in the art, and are readily selected by the knowledge of the quality of the ATH particle product required as described below. Typically, these conditions include inlet air temperatures typically between 250 and 550 °C and typically between 105 and 150. (:external air temperature. dry honing
按乾式硏磨’係意指使經噴霧乾燥之ATH歷經進一步 處理其中利用稍微減少經噴霧乾燥之ATH的粒子大小而將 ATH去凝聚。按「稍微減少粒子大小」係意指乾式硏磨之 ATH的d5Q是在噴霧乾燥前之漿體或濾餅中ATH的自約 40%至約90%的範圍內。較佳實施例中，乾式硏磨之ATH -11- 200811047 的d5Q是在噴霧乾燥前之漿體或瀘餅中ath的自約60%至 約80%的範圍內，更佳爲在噴霧乾燥前之漿體或濾餅中ΑΤΗ 的自約70%至約75 %的範圍內。 乾式硏磨經噴霧乾燥之ΑΤΗ時所使用之磨機可選自該 技藝中所已知之任何乾式硏磨機。適當乾式硏磨機的非限 制實例包括球或介質磨機、錐形和迴轉壓碎機、圓盤磨耗 磨機，膠體和輥磨機、篩磨機和粗碎機、錘和籠式磨機、 針和通用磨機、衝擊磨機和碎機、顎碎機、噴射和流體能 Φ 量硏磨機、輥壓碎機、圓盤磨機、垂直輥和乾盤磨機、振 動磨機。 因爲在乾式硏磨期間，基於所使用之磨機可能產生凝 聚物，可將自乾式硏磨經噴霧乾燥之ΑΤΗ所回收之乾式硏 磨ΑΤΗ經由已知之任何分類技術予以分類。適當分類技術 的非限制性實例包括空氣分級。請注意某些磨機具有內建 的空氣分級器，如果不是該種情況，可使用分開之空氣分 級器。如果在乾式硏磨時未使用針磨機，可使經乾式硏磨 ® 之ΑΤΗ在一個以上之針磨機中歷經進一步處理。 乾式硏磨經噴霧乾燥之ΑΤΗ係在有效製造具有改良形 態之乾式硏磨ΑΤΗ之條件下予以實施，下文予以論述。 改良形態學乾式硏磨之ΑΤΗ 就大體而論，本發明的方法可使用來製造具有許多不 同性質之乾式硏磨ΑΤΗ粒子。通常，可使用該方法來製造 具有如經由IS 0 7 8 7 - 5 : 1 9 8 0所測定之範圍自約1至約3 5 % 的油吸收；如經由DIN-66 1 32所測定之範圍自約1至15 m2/g -12- 200811047 之BET比表面積及範圍自約0.5至2.5 μιη之d5G的乾式硏磨 之經乾燥ATH粒子。 然而，當與現時可利用之ATH相比較，本發明的方法 特別充分適合製造具有改良形態之乾式硏磨之ATH粒子。 再次，雖然不希望受學說所約束，關於此，發明人確信此 改良形態可歸因於乾式硏磨之 ATH粒子的總比孔隙體積 (total) specific pore volume)及 / 或中値孔隙半徑（median pore vadius)「r5〇」）。關於此，發明人確信，關於指定之聚 Φ 合物分子，具有較高結構化凝集體之ATH含有較多且較大 之孔隙且似乎更難以潤濕，導致在捏合機中配合期間之各 種困難（電動機上輸出功率之變動較大），捏合機例如Buss Κο捏合機或雙螺桿擠壓機或該技藝方面已知且爲此目的 而使用之其他機器。因此，關於此，發明人已發現本發明 的方法製成之乾式硏磨ΑΤΗ粒子其特徵爲較小之中値孔隙 大小及/或較低之總孔隙體積，此特徵與使用聚合物材料 之改良潤濕相互關聯而因此導致改良之配合性質，即，配 ® 合含有乾式硏磨之ATH塡料之阻燃樹脂時所使用之配合機 器的引擎（電動機）的輸出功率變動較少）。 經由本發明所產生之乾式硏磨之 ATH粒子的r5Q和 Vmax可自水銀孔隙度測定法衍生出。水銀孔隙度測定法的 理論係基於物理原理就是：無反應性，非潤濕液體不會穿 透孔隙直至施加充分壓力來強制它進入。因此，使液體進 入孔隙所必須之壓力愈高，孔隙大小愈小。發現較小之孔 隙大小及/或較低之總比孔隙體積與經由本發明所產生之 -13- 200811047 乾式硏磨ATH粒子的較佳潤濕性相互關連。經由本發明所 產生之乾式硏磨ΑΤΗ粒子的孔隙大小可自使用來自義大利 ，C a r 1 ο E r b a S t r u m e n t a z i ο n e 之孔隙 g十 2 0 0 0 進 ί了之水銀孔隙 度測定法所衍生之數據予以計算。根據孔隙計2 0 0 0的手冊 ，使用下列方程式自所測得之壓力來計算孔隙半徑r : p : r = - 2 τ cos(0 ) /p 其中0是潤濕角，r是表面張力。本文中所取得之量測使 用 0 =141.3° 並將 τ 設定爲 480dyn/cm。 Φ 爲了改良測量的再現性，ΑΤΗ粒子的孔隙大小自第二 ΑΤΗ注入試驗操作予以計算，如孔隙計2000的手冊中所述 。使用第二試驗操作因爲發明人注意到在擠壓之後，即， 在放釋壓力至周圍壓力之後，大量之具有體積V〇之汞殘留 在ATH粒子的樣品中。因此，r5Q可自此數據衍生出，如下 文中所解釋連同參照第1、2和3圖。 第一試驗操作中，經由本發明所產生之乾式硏磨ATH 粒子的樣品係如孔隙計2000的手冊中所述予以製備，並使 — 用約1000巴的最大壓力，將孔隙體積量測爲所施加之注入 壓力P的函數。於完成第一試驗操作時，釋放壓力並容許 達到周圍壓力。利用來自第一試驗操作，無摻雜之相同ATH 樣品實施第二注入試驗操作（根據孔隙計2000之手冊），於 此情況，第二試驗操作之比孔隙體積V(p)的量測採用體積 V〇作爲新開始體積，然後將它設定爲零供第二次試驗操作 用。 第二注入試驗操作時，使用約1000巴的最大壓力，再 • 14- 200811047 實施ATH樣品的比孔隙體積V(P)之量測係所施加之注入壓 力的函數。第1圖顯示與現時商業上可供應之ATH產物比 較，關於第二注入試驗操作和根據本發明所產生之ATH級 ，比孔隙體積V係所施加之壓力的函數。在約1 〇〇〇巴時之 孔隙體積，即，量測時所使用之最大壓力本文中稱爲Vmax 〇 自第二ATH注入試驗操作，孔隙半徑r藉由孔隙計 2000根據下式予以計算： _ r = -2r cos(0 )/ρ 其中0是潤濕角，r是表面張力及ρ是注入壓力。關於本 文中所記錄之所有r量測，使用0 = 1 4 1 · 3 °並將r設定爲 4 8 0dyn/Cm。因此可將比孔隙體積對孔隙半徑r繪圖。第2 圖顯示第二注入試驗操作（使用相同樣品）的比孔隙體積V 對孔隙半徑r繪圖。 第3圖顯示第二注入試驗操作的常態化比孔隙體積對 孔隙半徑r之繪圖，即，此曲線中，將第二注入試驗操作 ® •的在1 000巴時之最大比孔隙體積Vmax設定爲100%，並將 特別ATH之其他比容除以此最大値。按照定義，本文中將 在50%的相對比孔隙體積時之孔隙半徑稱爲中値孔隙半徑 r50。舉例而言，根據第3圖，根據本發明之ATH，即發明 創造之ATH的中値孔隙半徑r5。是〇.33μπι。 使用根據本發明所產生之ΑΤΗ粒子的樣品而重複上述 之步驟，並發現經由本發明所產生之乾式硏磨ΑΤΗ粒子具 有範圍自約〇·〇9至約0·33μιη之r5()，即在50%的最大比孔 -15- 200811047 隙體積時之孔隙半徑。本發明的較佳實施例中’經由本發 明所產生之乾式硏磨ATH粒子的r5G是在自約〇·20至約 0.3 3μιη之範圍內，更佳在自約〇·2至約〇·3μπι之範圍內。 其他較佳實施例中，該是在自約〇·185至約0·325 μιη之 範圍內，更佳在自約0.185至約0·25μιη的範圍內。在其他 較佳實施例中，該Bo是在自約〇.〇9至約〇·21μιη之範圍內 ，更佳在自約0.09至約0.1 65 μιη的範圍內。 經由本發明所產生之乾式硏磨ΑΤΗ粒子亦可述其特徵 # 爲具有自約300至約700mm3/g範圍內之Vmax，即在1〇〇〇 巴時之最大比孔隙體積。本發明的較佳實施例中’經由本 發明所產生之乾式硏磨ATH粒子的Vmax是在自約390至約 480mm3/g之範圍內，更佳在自約410至約450mm3/g之範 圍內。在其他較佳之實施例中，該V^ax是在自約400至約 600mm3/g之範圍內，更佳在自約450至約550mm3/g之範 圍內。尙有其他較佳之實施例中，該Vmax是在自約300至 約700mm3/g之範圍內，更佳在自約350至約550mm3/g之 籲範圍內。 經由本發明所產生之乾式硏磨ATH粒子亦可述其特徵 爲具有如經由ISO 7 87-5:1 980所測定，在自約1至約35% 範圍內之油吸收。某些較佳實施例中，經由本發明所產生 之乾式硏磨ATH粒子之特徵爲具有在自約23至約30%範圍 內之油吸收，更佳爲在自約25%至約28%範圍內之油吸收 。其他較佳實施例中，經由本發明所產生之乾式硏磨ATH 粒子之特徵爲具有自約25%至約32%範圍內之油吸收，更 -16- 200811047 佳爲在自約26%至約30%之範圍內之油吸收。尙有其他較 佳實施例中，經由本發明所產生之乾式硏磨ATH粒子之特 徵爲具有自約2 5至約3 5 %範圍內之油吸收’更佳爲在自約 27%至約32%之範圍內。其他實施例中，經由本發明所產生 之乾式硏磨A TH粒子的油吸收是在自約1 9 %至約2 3 %之範 圍內，其他實施例中，經由本發明所產生之乾式硏磨ATH 粒子的油吸收是在自約21%至約25 %之範圍內。 經由本發明所產生之乾式硏磨ATH粒子亦可述其特徵 # 爲具有如經由DIN-66 1 3 2所測定，自約1至15m2/g範圍內 之BET比表面積。較佳實施例中，經由本發明所產生之乾 式硏磨ATH粒子具有自約3至約6m2/g之BET比表面積， 更佳在自約3.5至約5.5 m2/g範圍內。在其他較佳實施例中 ，經由本發明所產生之乾式硏磨ATH粒子具有自約6至約 9m2/g範圍內之BET比表面積，更佳爲在自約6.5至約 8.5 m2/g範圍內。更有其他較佳實施例中，經由本發明所產 生之乾式硏磨ATH粒子具有自約9至約15m2/g範圍內之 ® BET比表面積，更佳在自約10.5至約12.5m2/g範圍內。 經由本發明所產生之乾式硏磨ATH粒子亦可述其特徵 爲具有自約0.5至2.5 μιη範圍內之d5〇。較佳實施例中，經 由本發明所產生之乾式硏磨ATH粒子具有自約1.5至約 2.5 μ m範圍內之d 5 〇，更佳在自約1. 8至約2 · 2 μ m範圍內。 其他較佳實施例中，經由本發明所產生之乾式硏磨ATH粒 子具有自約1.3至約2.Ομιη範圍內之d5G，更佳爲在自約1.4 至約1.8 μιη的範圍內。更有其他較佳實施例，經由本發明 17- 200811047 所產生之乾式硏磨ATH粒子具有自約0.9至約1.8 μιη範圍 內之d5〇，更佳爲在自約1.1至約1.5 μιη之範圍內。 請注意：本文中所揭示之所有粒子直徑量測，即d50 係由使用來自Quantachrome公司之Cilas 1064 L雷射分光 計之雷射繞射予以量測。通常，爲了量測d5G本文中所使 用之步驟可經由首先將適當水-分散劑溶液（製備見下文）導 入入裝置的樣品製備容器中予以實施。然後選擇稱爲「粒 子專家」之標準量測，亦選擇量測模式「範圍1」，然後選 # 擇裝置-內部參數（其適用預期之粒子大小分佈）。請注意， 在量測期間，在分散期間和量測期間，通常將樣品暴露至 超音波歷約60秒。在背景量測已舉行之後，將自約75至 約1 OOmg之欲分析樣品連同水/分散劑溶液置入樣品容器 中並開始量測。該水/分散劑溶液可經由首先使用自BASF 可供應之3升的CAL Polysalt及自KMF Laborchemie可供 應之500g Calgon製備之一種濃縮物而予以製備。將此溶液 用去離子水組成至1 0升。自此1 0升原液中取出1 00毫升 ® ，依次用去離子水進一步稀釋至1 0升，並使用此最後溶液 作爲上述之水-分散劑溶液。 上述係關於本發明的數個實施例。精於該技藝之人士 應確認：可能設計同等有效之其他方法用來實行本發明的 要旨。亦請注意，本發明的較佳實施例考慮本文中所論述 之所有範圍包括自任何較低量至任何較高量之範圍。舉例 而言，當論述乾式硏磨ATH的Vmax時，該Vmax可能包括 範圔自約450至約490mm3/g，範圍自約5 50至約700mm3/g -18- 200811047 ，範圍自約3 90至約410mm3/g等之數値。下列實例將舉例 曰兌明本發明’但是並非思ί曰4人以任何方式限制本發明。 實例 如上文所述，下列實例中所敘述之r5Q和Vmax自使用 孔隙計2 0 0 0進行之水銀孔隙度測定法予以衍生出。除非在 其他情況下指示，所有d5G、BET、油吸收等係根據上述之 各種技術來量測。又，如實例中所使用之術語「發明創造 之氫氧化鋁級」，「發明創造」，和「發明創造之塡料」意指 ® 述及根據本發明所產生之ATH，而「比較性氫氧化鋁級」 ，「競爭性」，和「比較性」意指述及商業上可供應且並非 根據本發明所產生之ATH。 實例1 爲了形成漿體，將自汽巴（Cib a)®公司商業上可供售之 適當數量的分散劑Antiprex ®A40加至ATH濾餅，其具有 55wt%的固體含量，因此形成具有約150cPoise黏度之漿體 。該漿體中，即，在噴霧乾燥之前，氫氧化鋁具有2.3m2/g 的BET比表面積和2·48μιη之d5G。然後將漿體利用Niro F 1 00噴霧乾燥器予以噴霧乾燥，然後將經噴霧乾燥之氫氧 化鋁進給入 SJ50-ER100型之噴射磨機中，此噴射磨機自 Austria之PMT-Jetmill公司商業上可供應，並予以乾式硏 磨。爲了此目的，將組合之類析器轉子速率設定至5200rpm ，將硏磨壓力設定至6.6巴。此等硏磨參數導致每小時1066 仟克的氫氧化鋁之產量，且所生成之硏磨溫度是161°C。在 乾式硏磨之後，將經乾式硏磨之ATH粒子經由空氣過濾器 -19- 200811047 系統自SJ50-ER 100出口之熱空氣流中收集。所回收之乾式 硏磨ATH粒子（發明創造）的產物性質列入下列表1中。 經由馬丁股份有限公司（Martinswerk GmbH)所製造之 比較性氫氧化鋁級，Martinal®OL-104 LE的產物性質及另 外競爭性氫氧化鋁級「競爭性」的產物性質亦顯示於表1 中。 表 1 中値孔隙半徑 最大比孔隙體積 中値粒子大小 BET比表面積 (「r5〇」Χμιη) Vrnax(mm3/g) d5〇(pm) m2/g 比較性ATH 0.419 529 1.83 3.2 OL-104 LE 競爭性 0.353 504 1.52 3.2 本發明 0.33 440 1.93 3.7 如自表1中可見，發明創造之氫氧化鋁級（根據本發明 φ 所產生之ATH)具有最低之中値孔隙半徑和最低之最大比 孔隙體積。 實例2 分別使用比較性氫氧化鋁粒子Martinal® OL-104 LE 和實例1的本發明之氫氧化鋁級來形成阻燃樹脂配方。所 使用之合成樹脂是來自 Exxon Mobile之 EVA Escorene® Ultra UL0 0328 連同來自 ExxonMobile 之 LLDPE 級 LL1001XV ，自Albemarle®公司商業上可供應之Ethanox® 310抗氧化 劑和來自Degussa之胺基矽烷Dynasylan AMEO的混合物 -20- 200811047 。使用以精於該項技藝人士熟悉之通常方式所選擇之溫度 設定和螺桿速率，將該等成分在46mm Buss Κο捏合機（L/D 比=1 1)上混合，產量每小時25仟克。於調配阻燃樹脂配方 時所使用之各成分的數量詳列於下列表2中。 表 2 Phr(每一百份總樹脂 中的份數） Escorene Ultra UL00328 80 LL1001XV 20 氫氧化鋁 150 AMEO矽烷 1.6 Ethanox 310 0.6 在形成阻燃之樹脂配方時，在Buss捏合機配合之前， 首先將AMEO矽烷和Ethanox®310與總數量的合成樹脂在 # 圓桶中摻合。依靠重量進料器之減少，將樹脂/矽烷/抗 氧化劑摻合物連同50%的ATH總量進給Buss捏合機的第一 入口，並將其餘50 %的ATH進給入Buss捏合機的第二進料 口中。將卸料擠壓機安裝凸緣垂直於Buss Ko捏合機並具 有7 0mm的螺桿尺寸。第4圖顯示本發明氫氧化鋁之卸料 擠壓機的電動機上之輸出功率。第5圖顯示由馬丁股份有 限公司（Martinswerk GmbH)所製造之比較性氫氧化鋁級 OL-1 04 LE之卸料擠壓機的電動機上之輸出功率。 -21- 200811047 如第4圖和第5圖中所顯示，當使用根據本發明之ΑΤΗ 粒子在阻燃之樹脂配方中時，顯著減少卸料擠壓機的能量（ 功率）吸進的變動。如上文所述，能階之較小變動容許較大 之產量及/或更均勻（勻相）之阻燃樹脂配方。 【圖式簡單說明】 第1圖顯示與標準等級比較，關於第二注入試驗操作 和根據本發明（「發明創造」）之ΑΤΗ，比孔隙體積V係所 施加壓力之函數。 ^ 第2圖顯示與標準等級比較，關於第二注入試驗操作 和根據本發明（「發明創造」）之ΑΤΗ，比孔隙體積V對孔 隙半徑r之繪圖。 第3圖顯示與標準等級比較，根據本發明（「發明創造」） 之ATH之常態化比孔隙體積，該圖係以將各ATH級之最大 比孔隙體積設定在1 00%，並將相對應ATH等級的其他比容 除以此最大値所產生。 $ 第4圖顯示關於實例1中所產生及實例中所使用之本 發明氫氧化鋁級之卸料擠壓機的電動機上之輸出功率。 第5圖顯示關於比較性氫氧化鋁級〇L-104 LE之卸料 擠壓機的電動機上之輸出功率。 【主要元件符號說明】 4τττ 撒0 -22-By dry honing means means that the spray dried ATH is subjected to further processing wherein the ATH is deagglomerated by slightly reducing the particle size of the spray dried ATH. By "slightly reducing the particle size" is meant that the d5Q of the dry honed ATH is in the range of from about 40% to about 90% of the ATH in the slurry or filter cake prior to spray drying. In a preferred embodiment, the d5Q of the dry honed ATH-11-200811047 is in the range of from about 60% to about 80% of the ath in the slurry or pancake prior to spray drying, more preferably before spray drying. The crucible or filter cake has a range of from about 70% to about 75%. The mill used in the dry honing of the spray dried crucible may be selected from any of the dry honing machines known in the art. Non-limiting examples of suitable dry honing machines include ball or media mills, cone and rotary crushers, disc wear mills, colloid and roll mills, screen mills and coarse crushers, hammers and cage mills. , needle and general purpose mills, impact mills and crushers, crushers, jet and fluid energy Φ honing machines, roller crushers, disc mills, vertical and dry disc mills, vibrating mills. Since the dry mill may produce agglomerates during dry honing based on the mill used, the dry honing of the dry honed spray dried mash may be classified by any known classification technique. Non-limiting examples of suitable classification techniques include air grading. Please note that some mills have a built-in air classifier, and if this is not the case, a separate air classifier can be used. If a pin mill is not used during dry honing, the dry honing ® can be further processed in more than one pin mill. Dry honing spray-dried lanthanum is carried out under conditions effective to produce dry honing with improved morphology, as discussed below. Improved Morphology Dry Honing In general, the method of the present invention can be used to make dry honing particles having many different properties. In general, the method can be used to produce an oil absorption having a range of from about 1 to about 35 % as determined by IS 0 7 7 - 5 : 1 890; as determined by DIN-66 1 32 The BET specific surface area from about 1 to 15 m2/g -12 to 200811047 and dry honed ATH particles ranging from about 0.5 to 2.5 μηη d5G. However, the method of the present invention is particularly well suited for the manufacture of dry-honed ATH particles having an improved morphology when compared to currently available ATH. Again, although not wishing to be bound by the doctrine, the inventors believe that this modified form can be attributed to the total specific pore volume of the dry-honed ATH particles and/or the median pore radius (median). Pore vadius) "r5〇"). In this regard, the inventors are convinced that with respect to the specified poly Φ molecule, ATH with a higher structured aggregate contains more and larger pores and appears to be more difficult to wet, resulting in various difficulties during compounding in the kneader. (The variation in output power on the motor is large), a kneading machine such as a Buss Κο kneader or a twin-screw extruder or other machine known in the art and used for this purpose. Accordingly, in this regard, the inventors have discovered that the dry honing particles produced by the method of the present invention are characterized by a smaller inter- 値 pore size and/or a lower total pore volume, which is an improvement over the use of polymeric materials. Wetting is interrelated and thus results in an improved blending property, i.e., the engine (motor) used in the machine with the dry-honed ATH material is less variable in output power. The r5Q and Vmax of the dry honed ATH particles produced by the present invention can be derived from mercury porosimetry. The theory of mercury porosimetry is based on the physical principle: no reactivity, non-wetting liquid does not penetrate the pores until sufficient pressure is applied to force it into. Therefore, the higher the pressure necessary to bring the liquid into the pores, the smaller the pore size. It has been found that a smaller pore size and/or a lower total specific pore volume correlates with the preferred wettability of the dry-honed ATH particles produced by the present invention -13-200811047. The pore size of the dry honing particles produced by the present invention can be derived from the mercury porosimetry using the pores from Italy, C ar 1 ο E rba S trumentazi ο ne The data is calculated. According to the manual of the Pore Meter 2000, the following equation is used to calculate the pore radius r from the measured pressure: p : r = - 2 τ cos(0 ) /p where 0 is the wetting angle and r is the surface tension. The measurements taken in this paper use 0 = 141.3° and set τ to 480 dyn/cm. Φ In order to improve the reproducibility of the measurement, the pore size of the ruthenium particles is calculated from the second ruthenium test operation, as described in the manual of the porosimeter 2000. The second test operation was used because the inventors noticed that after the extrusion, i.e., after the release pressure to the ambient pressure, a large amount of mercury having a volume V〇 remained in the sample of the ATH particles. Thus, r5Q can be derived from this data, as explained below with reference to Figures 1, 2 and 3. In a first test operation, a sample of dry honed ATH particles produced by the present invention was prepared as described in the manual of Porosimeter 2000, and the pore volume was measured as a maximum pressure of about 1000 bar. A function of the applied injection pressure P. Upon completion of the first test operation, the pressure is released and the ambient pressure is allowed to reach. A second injection test operation (according to the manual of the porosimeter 2000) was carried out using the same ATH sample from the first test operation without doping, in which case the measurement of the specific pore volume V(p) of the second test operation was carried out by volume V〇 is taken as the new starting volume and then set to zero for the second test operation. In the second injection test operation, a maximum pressure of about 1000 bar is used, and then 14-200811047 is used to perform a function of the injection pressure applied to the specific pore volume V(P) of the ATH sample. Figure 1 shows a function of the pressure applied by the second injection test operation and the ATH grade produced in accordance with the present invention over the pore volume V system as compared to the currently commercially available ATH product. The pore volume at about 1 Torr, i.e., the maximum pressure used in the measurement, is referred to herein as Vmax 〇 from the second ATH injection test operation, and the pore radius r is calculated by the porosity meter 2000 according to the following formula: _ r = -2r cos(0 )/ρ where 0 is the wetting angle, r is the surface tension and ρ is the injection pressure. For all r measurements recorded in this paper, use 0 = 1 4 1 · 3 ° and set r to 4 8 0dyn/Cm. Therefore, the specific pore volume can be plotted against the pore radius r. Figure 2 shows the specific pore volume V of the second injection test operation (using the same sample) plotted against the pore radius r. Figure 3 shows the normalization ratio of the second injection test operation to the pore volume versus the pore radius r, i.e., in this curve, the maximum specific pore volume Vmax at 1 000 bar is set to the second injection test operation. 100%, and the other ratio of special ATH is divided by this maximum. By definition, the pore radius at 50% relative pore volume is referred to herein as the median pore radius r50. For example, according to Fig. 3, the ATH according to the present invention, i.e., the intermediate aperture radius r5 of the inventive ATH. It is 〇.33μπι. The above procedure was repeated using a sample of the ruthenium particles produced according to the present invention, and it was found that the dry honing ruthenium particles produced by the present invention have r5() ranging from about 〇·〇9 to about 0·33 μηη, that is, 50% of the maximum specific pores -15- 200811047 The pore radius at the gap volume. In a preferred embodiment of the invention, the r5G of the dry honing ATH particles produced by the present invention is in the range of from about 〇20 to about 0.33 μηη, more preferably from about 〇·2 to about 〇·3 μπι. Within the scope. In other preferred embodiments, this is in the range from about 185 185 to about 0. 325 μηη, more preferably in the range from about 0.185 to about 0. 25 μηη. In other preferred embodiments, the Bo is in the range of from about 〇.〇9 to about 〇·21μηη, more preferably in the range of from about 0.09 to about 0.165 μηη. The dry honing particles produced by the present invention may also be characterized as having a Vmax in the range of from about 300 to about 700 mm 3 /g, i.e., a maximum specific pore volume at 1 bar. In a preferred embodiment of the invention, the Vmax of the dry honing ATH particles produced by the present invention is in the range of from about 390 to about 480 mm 3 /g, more preferably from about 410 to about 450 mm 3 /g. . In other preferred embodiments, the V^ax is in the range of from about 400 to about 600 mm3/g, more preferably from about 450 to about 550 mm3/g. In other preferred embodiments, the Vmax is in the range of from about 300 to about 700 mm3/g, more preferably from about 350 to about 550 mm3/g. Dry honing ATH particles produced by the present invention may also be characterized as having oil absorption in the range of from about 1 to about 35% as determined by ISO 7 87-5:1 980. In certain preferred embodiments, the dry honing ATH particles produced by the present invention are characterized by having an oil absorption in the range of from about 23 to about 30%, more preferably from about 25% to about 28%. The oil inside is absorbed. In other preferred embodiments, the dry honing ATH particles produced by the present invention are characterized by having an oil absorption in the range of from about 25% to about 32%, more preferably from -26% to about 110% from about 26% to about Oil absorption in the range of 30%. In other preferred embodiments, the dry honing ATH particles produced by the present invention are characterized by having an oil absorption in the range of from about 25 to about 35 %, more preferably from about 27% to about 32. Within the range of %. In other embodiments, the oil absorbing of the dry honed A TH particles produced by the present invention is in the range of from about 1 9 % to about 23 %, and in other embodiments, the dry honing produced by the present invention The oil absorption of the ATH particles is in the range of from about 21% to about 25%. Dry honing ATH particles produced by the present invention may also be characterized by having a BET specific surface area ranging from about 1 to 15 m2/g as determined by DIN-66 131. In a preferred embodiment, the dry honing ATH particles produced by the present invention have a BET specific surface area of from about 3 to about 6 m2/g, more preferably from about 3.5 to about 5.5 m2/g. In other preferred embodiments, the dry honing ATH particles produced by the present invention have a BET specific surface area ranging from about 6 to about 9 m2/g, more preferably from about 6.5 to about 8.5 m2/g. . In still other preferred embodiments, the dry honing ATH particles produced by the present invention have a BET specific surface area ranging from about 9 to about 15 m2/g, more preferably from about 10.5 to about 12.5 m2/g. Inside. The dry honing ATH particles produced by the present invention may also be characterized as having d5 自 in the range of from about 0.5 to 2.5 μηη. In a preferred embodiment, the dry honing ATH particles produced by the present invention have a d 5 〇 ranging from about 1.5 to about 2.5 μm, more preferably from about 1.8 to about 2 · 2 μm. . In other preferred embodiments, the dry honing ATH particles produced by the present invention have a d5G ranging from about 1.3 to about 2. Ομηη, more preferably in the range of from about 1.4 to about 1.8 μηη. In still other preferred embodiments, the dry honing ATH particles produced by the present invention 17-200811047 have d5〇 ranging from about 0.9 to about 1.8 μηη, more preferably from about 1.1 to about 1.5 μηη. . Please note that all particle diameter measurements disclosed herein, i.e., d50, were measured by laser diffraction using a Cilas 1064 L laser spectrometer from Quantachrome. In general, the steps used herein for measuring d5G can be carried out by first introducing a suitable water-dispersant solution (prepared as described below) into the sample preparation vessel of the apparatus. Then select the standard measurement called “particle expert”, also select the measurement mode “Range 1”, and then select the device-internal parameter (which applies the expected particle size distribution). Note that during the measurement, the sample is typically exposed to ultrasound for approximately 60 seconds during the dispersion and during the measurement. After the background measurement has been taken, about 75 to about 100 mg of the sample to be analyzed is placed in the sample container along with the water/dispersant solution and measurement is started. The water/dispersant solution can be prepared by first using a concentrate prepared from 3 liters of CAL Polysalt available from BASF and 500 g of Calgon available from KMF Laborchemie. This solution was made up to 10 liters with deionized water. From this 10 liter stock solution, 100 ml of ® was taken out, and further diluted to 10 liters with deionized water in that order, and this final solution was used as the above water-dispersant solution. The foregoing is a few examples of the invention. Those skilled in the art should clarify that other methods that may be equally effective may be used to practice the gist of the present invention. It is also noted that the preferred embodiments of the present invention contemplate all ranges discussed herein including from any lower amount to any higher amount. For example, when discussing the Vmax of dry honing ATH, the Vmax may include from about 450 to about 490 mm 3 /g, ranging from about 5 50 to about 700 mm 3 /g -18 - 200811047, ranging from about 3 90 to Approximately 410mm3/g, etc. The following examples are intended to illustrate the invention, but are not intended to limit the invention in any way. EXAMPLES As described above, r5Q and Vmax described in the following examples were derived from mercury porosimetry using a porosimeter 2000. All d5G, BET, oil absorption, etc. are measured according to the various techniques described above, unless otherwise indicated. Moreover, the terms "aluminum hydride grade invented", "invention", and "invention of invention" as used in the examples mean that ATH refers to the ATH produced according to the present invention, and "comparative hydrogen" "Alumina grade", "competitive", and "comparative" are meant to mean ATH that is commercially available and not produced in accordance with the present invention. Example 1 To form a slurry, an appropriate amount of dispersant Antiprex® A40 commercially available from Ciba® was added to the ATH filter cake, which had a solids content of 55 wt% and thus formed to have about 150 cPoise Viscosity of the slurry. In the slurry, that is, prior to spray drying, the aluminum hydroxide had a BET specific surface area of 2.3 m 2 /g and a d5G of 2.48 μm. The slurry was then spray dried using a Niro F 1 00 spray dryer, and the spray dried aluminum hydroxide was then fed into a jet mill of the type SJ50-ER100, which was commercial from PMT-Jetmill, Austria. It can be supplied and dryly honed. For this purpose, the combined resolver rotor speed was set to 5200 rpm and the honing pressure was set to 6.6 bar. These honing parameters resulted in a yield of 1066 gram of aluminum hydroxide per hour and the resulting honing temperature was 161 °C. After dry honing, the dry honed ATH particles are collected via a hot air stream from the SJ50-ER 100 outlet via an air filter -19-200811047 system. The product properties of the recovered dry honing ATH particles (inventives) are listed in Table 1 below. The product properties of Martinal® OL-104 LE and the "competitive" product properties of the otherwise competitive aluminum hydroxide grade are also shown in Table 1 by comparative alumina grades manufactured by Martinswerk GmbH. Table 1 The maximum pore radius of the crucible in the pore volume BET specific surface area ("r5〇"Χμιη) Vrnax(mm3/g) d5〇(pm) m2/g Comparative ATH 0.419 529 1.83 3.2 OL-104 LE Competition Properties 0.353 504 1.52 3.2 The present invention 0.33 440 1.93 3.7 As can be seen from Table 1, the inventive aluminum hydroxide grade (ATH produced by φ according to the invention) has the lowest intermediate pore radius and the lowest maximum specific pore volume. Example 2 A flame retardant resin formulation was formed using the comparative aluminum hydroxide particles Martinal® OL-104 LE and the aluminum hydroxide grade of the present invention of Example 1, respectively. The synthetic resin used was EVA Escorene® Ultra UL0 0328 from Exxon Mobile together with LLDPE grade LL1001XV from ExxonMobile, a mixture of commercially available Ethanox® 310 antioxidant from Albemarle® and Dynasylan AMEO from Degussa - 20-200811047. The ingredients were mixed on a 46 mm Buss Κο kneader (L/D ratio = 1 1) using a temperature setting and screw speed selected in a manner conventional to those skilled in the art, yielding 25 gram per hour. The quantities of ingredients used in formulating the flame retardant resin formulation are detailed in Table 2 below. Table 2 Phr (parts per hundred parts of total resin) Escorene Ultra UL00328 80 LL1001XV 20 Aluminium hydroxide 150 AMEO decane 1.6 Ethanox 310 0.6 When forming a flame retardant resin formulation, the AMEO will be used first before the Buss kneader is combined. The decane and Ethanox® 310 were blended with the total amount of synthetic resin in a #drum. Relying on the reduction of the weight feeder, the resin/decane/antioxidant blend was fed to the first inlet of the Buss kneader along with a total of 50% ATH, and the remaining 50% of the ATH was fed into the first of the Buss kneader. In the two feed ports. The discharge extruder mounting flange was perpendicular to the Buss Ko kneader and had a screw size of 70 mm. Fig. 4 is a view showing the output power on the motor of the aluminum hydroxide discharge extruder of the present invention. Figure 5 shows the output power of the motor of a comparative aluminum hydroxide grade OL-1 04 LE discharge extruder manufactured by Martinswerk GmbH. -21- 200811047 As shown in Figures 4 and 5, when the ruthenium particles according to the present invention are used in a flame retardant resin formulation, the variation in energy (power) suction of the discharge extruder is significantly reduced. As noted above, small variations in energy levels allow for greater yield and/or more uniform (homogeneous) flame retardant resin formulations. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a graph showing the relationship between the second injection test operation and the pressure applied by the pore volume V system according to the present invention ("invention") as compared with the standard level. ^ Figure 2 shows a comparison of the pore volume V versus the aperture radius r for the second injection test operation and according to the present invention ("Invention") compared to the standard grade. Figure 3 shows the normalized specific pore volume of ATH according to the invention ("Invention") compared to the standard grade, which is set to a maximum specific pore volume of each ATH grade of 100%, and will correspond The other specific volume of the ATH grade is generated by this maximum enthalpy. $ Figure 4 shows the output power on the motor of the inventive aluminum hydroxide grade discharge extruder used in the example 1 and used in the examples. Figure 5 shows the output power on the motor of the unloading extruder of the comparative aluminum hydroxide grade 〇L-104 LE. [Main component symbol description] 4τττ scatter 0 -22-