201034966 六、發明說明： 【發明所屬之技術領域】 本發明大體係關於一種聚集金屬氧化物顆粒之方法，及 更特定而言為一種製備金屬氧仡物顏料顆粒之聚集物的方 法。 【先前技術】 金屬氧化物顆粒（諸如顏料顆粒）常用於化妝品、清潔 劑、油漆、塑料及其他產業中以為產品添加顏色及/或使201034966 VI. INSTRUCTIONS OF THE INVENTION: TECHNICAL FIELD OF THE INVENTION The present invention relates to a method of aggregating metal oxide particles, and more particularly to a method of preparing aggregates of metal oxon pigment particles. [Prior Art] Metal oxide particles, such as pigment particles, are commonly used in cosmetics, detergents, paints, plastics, and other industries to add color and/or
〇 產品不透明。為使產品不透明，該等金屬氧化物顆粒必須 為次微米大小之精細粉末。該等精細粉末具有黏性並傾向 具有較差之流動特徵。在任何連續製程（諸如，例如塑性 複合）中準確控制顆粒流動模式需較佳流動特徵。 提高精細粉末流動性之常用方法包括將金屬氧化物顆粒 聚集成較大顆粒。用於聚集金屬氧化物顆粒之方法可使用 、。口劑，其4聚集體提供黏著力及亦增加聚集顆粒之安定 '=。然而’結合劑一般保留於聚合體内並對最終使用者而 。構成產时之巧染物。一般結合劑係選自水、蠟及/或油 類。蠟及油類可能具有有害作用，而水可能不適合用於塑 性複合中之高溫環境中。 用於聚集金屬氧化物顆#夕0I ^ . a *化物顆粒之已知方法的另-問題係其可 生八有高於所需黏性之堅 ^ 聚集金屬氧化物顆粒。通常 施用於塑性複合中 n 斂剪刀係不足以分解該等堅固聚集 顆拉，且該等顆粒顯示較差之可分散性。 需要製備聚集金屬氧化物顆粒之改良方法，其克服以上 145392.doc 201034966 問題並保持優良可分散性特徵。 【發明内容】 本發明係一種製備金屬氧化物顆粒聚集體之改良方法， 其包括將金屬氧化物顆粒與實質上非水性液體混合以形成 漿液’及隨後乾燥該漿液以形成聚集冑。本發明尤其適於 製備二氧化鈦顆粒聚集體。 【實施方式】 根據-項實施例之本發明包括將金屬氧化物顆粒與實質 上非水性液體混合以形成漿液及隨後乾燥該漿液，藉此形 成聚集體。金屬氧化物顆粒一般具有小於5微米之平均一 次顆粒直徑，而顏料一般具有小於丨微米之平均一次顆粒 直徑。然而對於非顏料應用（例如，所謂奈米物質，諸如 紫外線阻斷劑及觸媒），該平均一次顆粒直徑可小於1〇〇奈 米。根據本發明製得之金屬氧化物顆粒聚集體顯示實質上 等同於聚集前之金屬氧化物顆粒之可分散性的可分散性。 此意味粉末能均一分佈於最終聚合物或塗層中而無保持未 分散之過量聚集體。 本發明之方法尤其可應用於為疏水性或親水性顏料之金 屬氧化物顆粒’其巾其主要作帛係使併入其之物體不透 明。為顏料之金屬氧化物的實例包括（但不限於）二氧化鈦 及氧化鐵。顏料（諸如二氧化鈦）可經一種有機化合物或兩 或更多種有機化合物之混合物被覆以提高其與主體物質之 可相容性。用於提高顏料可相容性之有機化合物的實例包 括有機矽烷及有機磷化合物。顏料顆粒之平均粒徑係在 145392.doc 201034966 0·1至0.5微米之範圍内β 文中所用之術語「實質上非水性液體」係指— 疏水性粉末並顯示實質上比水小之表面張 液體之另-性質為低、、弗=體。該實質上非水性 合此等標準。 …、 3有乂 I水以作為易混溶液體（諸 乙醇或丙酮)之組分係在本發明之範圍及精神 内。為達實踐目的及最佳結果，「 Ο 〇 包含不多㈣重量％之水t 非水性液體」應 重之水’巾即其可包含至多20重量％之 1不具有對製程有害之作用。用於進行本發明製程之最 佳實質上非水性液體為燒’諸如己烧。然而，適宜非水性 液體可選自脂肪族化合物、芳香族化合物及其混合物，諸 如（例如）選自燒、稀、炔、酿、趟、嗣、酸、醇、虐化 物、胺及醯胺。己院、庚烧及丙_為適用於進行本發明方 法之實質上非水性液體。該非水性液體較佳具有在抓至 80 C之範圍内的沸點以便於乾燥。 金屬氧化物與非水性液體之混合可方便地在高速分散器 (諸如C〇WleS分散器）中完成，或混合可以連續方式藉由複 合操作’諸如利用雙螺桿擠壓機完成，其中將金屬氧化物 與非水性液體混合以形成稍漿液或糊料，及將該糊料擠壓 成預成型體’例如分離小球。控制液體與固體之比例以確 保漿液之所需—致性’其可從稀薄漿液變化至稠糊料。液 體之所需量亦可能受諸如金屬氧化物顆粒之多孔性及大小 等口素汾響，但一般在所得漿液總重量之30%至7〇%之範 145392.doc 201034966 圍内。擠壓之金屬氧化物預成型體將具有一在2至3 mm之 範圍内之平均直徑，但該直徑可達至10 mm或甚至更大。 除非對最終應用而言係實用的，否則對大小無限制。隨後 乾燥預成型體並回收乾燥聚集體。 乾燥可藉由在周圍條件下自然蒸發非水性液體而完成， 或乾垛可藉由會加速乾燥過程之強制通風乾燥蒸發非水性 液體完成。預成型體亦可藉由加熱（諸如對流加熱、傳導 加熱或輻射加熱）乾燥。實例包括令該等預成型體與熱惰 性氣體（諸如氮氣）接觸，或於熱表面上（諸如（例如）用於隧 式乾燥器類型之熱金屬片）加熱該等預成型體。該等預成 型體可藉由施用真空有或無其他熱量存在下接受強制乾燥 或其可浸沒於另-具有高於該非水性液體之沸點之溫度的 液體(諸如熱水)下。舉例而言，利用己烷作為非水性液體 所形成之金屬氧化物職型冑可浸沒於已經加熱至至少 饥之溫度之水中。閃蒸出具有65t之彿點的己炫且自水 回收聚木產物並進-步乾燥之。用於進行本發明方法之乾 燥設備可包括噴霧乾燥器、隨道型乾燥器及旋轉爐。較佳 "亥蒸發之非水性液體係藉由濃縮回收並再用於製備新 鮮漿液或糊料。儘管根據本發明製得之聚集體經實質乾 燥’但可保留—些殘餘量之非水性液體’-般小於5重量 對易揮發性化合物，諸如院（例如己幻及酮（例如丙酮） 而δ，殘餘含量較佳係小於1重量％。乾燥後可進-步分 ，，集體以達到提供可接受流動性質之所需大小以用於預 疋最、、用途應用中。聚集體之可接受流動性包括「自由流 145392.doc 201034966 動」’其中流動係穩定且連續的。 可將添加劑加入根據本發明方法之步驟一中所形成之漿 液中以輔助聚集體之處理。適宜添加劑包括多元醇、有機 矽化合物、有機磷化合物、脂肪酸、蠟、金屬硬脂酸鹽、 纖維素、脂肪酸、脂肪酯、躐酯、甘油酯、二醇酯、脂肪 醇Sa、脂肪醇、脂肪酿胺、烯烴聚合物、聚稀烴壤及其混 合物。 〇 金屬氧化物聚集體係用於為大量消費產品’諸如油漆、 塗層、塑料、紙品、墨水、食品、呈藥片及錠劑形式之藥 物以及大多數牙膏提供白度及不透明性。在化妝品及護膚 產品中，金屬氧化物可用於著色及稠化。金屬氧化物亦可 用於紋身顏料及止血筆中及陶竟釉中，其中該金屬氧化物 係用於不透明劑及晶種形成。金屬氧化物聚集體另外用於 塑性複合中以製造塑料物體。除了顯示獲改良之流動特徵 外’根據本發明製得之金屬氧化物聚集體因其較少灰塵亦 促成較佳衛生條件。 測量顏料分散之試驗法 測量並比較非聚集及聚集金屬氧化物之分散，及分散之 ==藉:不同方法製得’其包括滾磨，以及自根 據本發明之貫質上非水性 之方法如下： 作而t集。用於測量分散 金屬氧化物於有機聚合物内之 擠《置藉由記_機網包之網篩上所 ==驗； 物微粒的相對量而測得。 集之金屬軋化 145392.doc 201034966 一種75重量％之金屬氧化物濃縮物及低密度聚乙烯之混 合物係利用Haake 3000 Rheomix混合器藉由337.7 g微米化 之 Ti02與 112.6 g NA209 LDPE(由 Equistar 製造）混合而製 得。該混合器係利用Haake 9000 Rheocord Torque Rheometer控制並監測。首先乾摻合混合物並隨後在75°C 下將其添加至以50 rpm操作之轉子的混合器中。該混合器 溫度係經程序化以在添加乾摻合混合物後一分鐘增加至 120°C。當混合操作達到穩定狀態時，一般需要約3至4分 鐘，另攪拌該混合物3分鐘。從混合器中移除該混合物並 利用Cumberland礙碎機造粒。 分散係利用裝配有長度與直徑比為20 : 1之螺旋的 Killion型KL-100單螺旋擠壓機測得，其中該螺旋從區1至 鑄模分別經預熱至330°F、350°F、390°F及380°F並以70 rpm進行操作。使1000 g由Equistar製造之NA952 LDPE之 掃氣通過該系統並安裝一個新網包。該網包由鑄模往擠壓 機喉口方向係由40/500/200/1 00網篩組成。在溫度穩定 後，將133.33 g粒化之75% Ti02濃縮物饋入擠壓機中。隨 著進料漏斗變空，繼以饋入1500 g NA952掃氣。在擠壓 ；LDPL·掃氣後，移除、分離並利用來自X射線螢光分光計之 測量值以相對計數法測試網篩。獲得網包中1 〇〇、200及 5 00網篩之每秒鐘Ti02的計數值並記算總和以獲得分散結 果。較低之每秒鐘Ti02計數係符合需要。將小於5000之計 數結果視為優良分散，以低於1000為極佳。 分散標準 145392.doc 201034966〇 The product is opaque. In order to make the product opaque, the metal oxide particles must be fine powders of submicron size. These fine powders are viscous and tend to have poor flow characteristics. Accurate control of the particle flow pattern in any continuous process, such as, for example, plastic compounding, requires better flow characteristics. A common method of increasing the flowability of fine powders involves the aggregation of metal oxide particles into larger particles. A method for aggregating metal oxide particles can be used. Oral agent, its 4 aggregates provide adhesion and also increase the stability of aggregated particles '=. However, the binder typically remains in the polymer body and is intended for the end user. It constitutes the coincidence of birth. Typical binders are selected from the group consisting of water, waxes and/or oils. Waxes and oils may have deleterious effects, and water may not be suitable for use in high temperature environments in plastic composites. Another problem with known methods for agglomerating metal oxide particles is that they have a higher concentration of aggregated metal oxide particles than the desired viscosity. Often applied to plastic composites, n-scissors are not sufficient to break down such strong aggregates, and the particles exhibit poor dispersibility. There is a need for an improved process for preparing aggregated metal oxide particles that overcomes the above problems of 145392.doc 201034966 and maintains excellent dispersibility characteristics. SUMMARY OF THE INVENTION The present invention is an improved method of preparing aggregates of metal oxide particles comprising mixing metal oxide particles with a substantially non-aqueous liquid to form a slurry' and subsequently drying the slurry to form aggregated mash. The invention is particularly suitable for the preparation of aggregates of titanium dioxide particles. [Embodiment] The invention according to the embodiment includes mixing metal oxide particles with a substantially non-aqueous liquid to form a slurry and then drying the slurry, thereby forming aggregates. The metal oxide particles generally have an average primary particle diameter of less than 5 microns, while the pigment generally has an average primary particle diameter of less than 丨 microns. For non-pigment applications (e. g., so-called nanomaterials, such as UV blockers and catalysts), the average primary particle diameter can be less than 1 nanometer. The aggregate of metal oxide particles prepared according to the present invention exhibits dispersibility which is substantially equivalent to the dispersibility of the metal oxide particles before aggregation. This means that the powder can be uniformly distributed in the final polymer or coating without excess aggregates remaining undispersed. The method of the present invention is particularly applicable to metal oxide particles which are hydrophobic or hydrophilic pigments, the main purpose of which is that the object incorporated therein is opaque. Examples of metal oxides which are pigments include, but are not limited to, titanium dioxide and iron oxide. The pigment (such as titanium dioxide) may be coated with an organic compound or a mixture of two or more organic compounds to improve compatibility with the host material. Examples of the organic compound for improving the compatibility of the pigment include an organic decane and an organic phosphorus compound. The average particle size of the pigment particles is in the range of 145392.doc 201034966 0·1 to 0.5 μm. The term "substantially non-aqueous liquid" as used herein refers to a hydrophobic powder and exhibits a surface liquid that is substantially smaller than water. The other - the nature is low, and the body = body. This is essentially non-aqueous standard. It is within the scope and spirit of the present invention to use water as a component of a miscible solution (such as ethanol or acetone). For practical purposes and best results, " Ο 包含 contains not more than (4)% by weight of water t non-aqueous liquids" should be heavy water's towel, which can contain up to 20% by weight of one without harmful effects on the process. The most preferred substantially non-aqueous liquid for carrying out the process of the present invention is a fire such as hexane. However, suitable non-aqueous liquids may be selected from the group consisting of aliphatic compounds, aromatic compounds, and mixtures thereof, such as, for example, those selected from the group consisting of burnt, dilute, alkyne, brew, hydrazine, hydrazine, acid, alcohol, acaricide, amine, and decylamine. Hexa, Geng, and C are substantially non-aqueous liquids suitable for carrying out the process of the present invention. The non-aqueous liquid preferably has a boiling point in the range of 80 C to facilitate drying. The mixing of the metal oxide with the non-aqueous liquid can conveniently be accomplished in a high speed disperser, such as a C〇WleS disperser, or the mixing can be accomplished in a continuous manner by a compounding operation, such as by a twin screw extruder, in which the metal is oxidized. The material is mixed with a non-aqueous liquid to form a slight slurry or paste, and the paste is extruded into a preform, such as a separation pellet. The ratio of liquid to solid is controlled to ensure that the desired consistency of the slurry can vary from a thin slurry to a thick paste. The required amount of the liquid may also be affected by a porosity such as the porosity and size of the metal oxide particles, but it is generally within the range of 30% to 7〇% of the total weight of the obtained slurry 145392.doc 201034966. The extruded metal oxide preform will have an average diameter in the range of 2 to 3 mm, but the diameter can be up to 10 mm or even larger. There is no limit to size unless it is practical for the final application. The preform is then dried and the dried aggregates are recovered. Drying can be accomplished by naturally evaporating the non-aqueous liquid under ambient conditions, or the drying can be accomplished by forced drying of the non-aqueous liquid by accelerated drying of the drying process. The preform may also be dried by heating, such as convection heating, conduction heating or radiant heating. Examples include contacting the preforms with a thermally inert gas such as nitrogen, or heating the preforms on a hot surface such as, for example, a hot metal sheet for a tunnel dryer type. The preforms may be subjected to forced drying by application of vacuum with or without other heat or they may be immersed in another liquid having a temperature higher than the boiling point of the non-aqueous liquid, such as hot water. For example, a metal oxide form formed using hexane as a non-aqueous liquid can be immersed in water that has been heated to at least the temperature of hunger. The sleek and self-recovery poly-wood product with 65t of the Buddha's point is flashed off and dried step by step. Drying equipment for carrying out the process of the invention may include a spray dryer, a via dryer, and a rotary furnace. Preferably, the non-aqueous liquid system of the evaporation is recovered by concentration and reused to prepare a fresh slurry or paste. Although the aggregates made in accordance with the present invention are substantially dried 'but may retain some residual amount of non-aqueous liquid', generally less than 5 weights of volatile compounds, such as a hospital (eg, illusion and ketone (eg, acetone) and δ Preferably, the residual content is less than 1% by weight. After drying, it can be further divided into groups to achieve the desired size for acceptable flow properties for use in pre-extraction applications, acceptable flow of aggregates. The properties include "free flow 145392.doc 201034966" "where the flow system is stable and continuous. Additives may be added to the slurry formed in step one of the process according to the invention to aid in the treatment of the aggregates. Suitable additives include polyols, Organic germanium compounds, organophosphorus compounds, fatty acids, waxes, metal stearates, celluloses, fatty acids, fatty esters, oxime esters, glycerides, glycol esters, fatty alcohols Sa, fatty alcohols, fatty amines, olefin polymers Polycarbonaceous soils and mixtures thereof. Base metal oxide aggregation systems are used for a large number of consumer products such as paints, coatings, plastics, paper products, inks, foods. Medications in the form of tablets and lozenges and most toothpastes provide whiteness and opacity. In cosmetics and skin care products, metal oxides can be used for coloring and thickening. Metal oxides can also be used in tattoo pigments and hemostatic pens and ceramics. In the glaze, wherein the metal oxide is used for the formation of an opacifier and a seed crystal. The metal oxide aggregate is additionally used in plastic compounding to produce a plastic object. In addition to showing improved flow characteristics, the invention is made in accordance with the present invention. Metal oxide aggregates contribute to better hygienic conditions due to their less dust. The test method for measuring pigment dispersion measures and compares the dispersion of non-aggregated and aggregated metal oxides, and the dispersion == by: different methods to make 'its include The barreling, and the method of the non-aqueous quality according to the present invention are as follows: a set of t and a set of used for measuring the dispersion of the dispersed metal oxide in the organic polymer. == test; measured by the relative amount of particles. Metallization of the set 145392.doc 201034966 A 75 wt% metal oxide concentrate and low density polyethylene The compound was prepared by mixing 337.7 g of micronized Ti02 with 112.6 g of NA209 LDPE (manufactured by Equistar) using a Haake 3000 Rheomix mixer. The mixer was controlled and monitored using a Haake 9000 Rheocord Torque Rheometer. The mixture was then added to the mixer of the rotor operating at 50 rpm at 75 ° C. The mixer temperature was programmed to increase to 120 ° C one minute after the addition of the dry blending mixture. When the steady state is reached, it usually takes about 3 to 4 minutes and the mixture is stirred for another 3 minutes. The mixture is removed from the mixer and granulated using a Cumberland disrupter. The dispersion was measured using a Killion KL-100 single screw extruder equipped with a 20:1 length to diameter ratio screw, wherein the spiral was preheated from Zone 1 to the mold to 330 °F, 350 °F, 390 °F and 380 °F and operated at 70 rpm. A 1000 g of NA952 LDPE manufactured by Equistar was purged through the system and a new network package was installed. The net bag consists of a 40/500/200/1 00 mesh screen from the mold to the throat of the extruder. After the temperature was stabilized, 133.33 g of the granulated 75% Ti02 concentrate was fed into the extruder. As the feed funnel becomes empty, it is followed by a 1500 g NA952 scavenging gas. After squeezing; LDPL·scavenging, the screen was removed, separated and measured using a measurement from an X-ray fluorescence spectrometer in relative counting. Obtain the count value of Ti02 per second for the 1 〇〇, 200, and 500 mesh screens in the net bag and calculate the sum to obtain the dispersion result. The lower Ti02 count per second is in line with the need. A result of less than 5,000 is considered to be excellent dispersion, and is preferably less than 1,000. Decentralized standard 145392.doc 201034966
Tiona 188(—種由 Millennium Inorganic Chemicals製造之 精細分散的二氧化鈦商品）係用作分散標準品。Tiona 1 88 係經疏水性有機矽表面處理並已在塑性複合應用中顯示極 佳分散性能。Tiona 1 88係以上述試驗法進行四（4)次以建 立試驗可再現性。結果係顯示於下： 平均分散609計數 標準偏差2 1 7計數。 下列實例說明二氧化鈦聚集之前及之後之可分散值，及 ΟTiona 188 (a finely divided titanium dioxide product manufactured by Millennium Inorganic Chemicals) is used as a dispersion standard. Tiona 1 88 is surface treated with hydrophobic organic germanium and has shown excellent dispersion properties in plastic composite applications. Tiona 1 88 was subjected to the above test method four (4) times to establish test reproducibility. The results are shown below: Average dispersion 609 counts Standard deviation 2 1 7 counts. The following examples illustrate the dispersible values before and after the aggregation of titanium dioxide, and
其亦提供一藉由不同方法聚集之二氧化鈦聚集體之可分散 值的指示。 實例1-滚磨 4〇〇 g與分散標準品之材料相同的Ti〇na 188係於1夸脫塑 料缸中以50 rPm軋製1.5小時或18小時。 在滾磨後，顏料開始聚集成大至數毫米之球體，但該聚 集體顯示-從精細粉末至數毫米球體之大小範圍内。可觀 察到滾磨更長時間之產品的大小更均―。根據上述程序測 試所得產品之分散並將結果顯示於下表4 : 表1It also provides an indication of the dispersible value of the titanium dioxide aggregates that are aggregated by different methods. Example 1 - Rolling 4〇〇 g The Ti〇na 188, which is the same material as the dispersion standard, was rolled in a 1 quart plastic cylinder at 50 rPm for 1.5 hours or 18 hours. After barreling, the pigment begins to aggregate into spheres as large as a few millimeters, but the aggregate shows - ranging from fine powder to a few millimeters of sphere size. It can be observed that the size of the product that is rolled for a longer period of time is more uniform. The dispersion of the obtained product was tested according to the above procedure and the results are shown in Table 4 below: Table 1
滾磨1 · 5小時 〜— 滾磨18小時 分散(XRF計數) 1127 4107 可見滾磨導 末流動及聚集 實例2-壓實 較長滾磨時間有利於粉 J45392.doc 201034966 將50磅與實例1所用相同之顏料（Tiona 188)通過 Fitzpatrick Company L-83壓實機之壓力軋報。圓柱體在壓 力下軋製，令Tiona 1 88粉末通過軋輥之間並藉由所施用之 壓力壓實之。該等軋輥係以5 rpm操作並具有400 psi之升 壓機壓力。將產品製成在許多篩子中所集得具有不同聚集 大小之小片。每一篩分粒級進行分散測試並將結果顯示於 下表2中： 表2 樣本 分散 14篩分粒級 5148 20篩分粒級 4344 30篩分粒級 2769 3 5篩分粒級 3140 40篩分粒級 3912 5 0篩分粒級 4281 7 0篩分粒級 6577 盤（殘留精細粉末） 4213 可見到不管所測試之篩分粒級，令顏料通過壓力軋輥以 壓實之已導致顏料之可分散性實質上降低。 實例3-從非水性液體乾燥 將171 g如實例}所用之Ti〇na 188與（a)231 g庚烷或（bp% g丙酮於1夸脫容器中利用c〇wles分散器以3〇〇〇 rpm混合。 令所得混合物隔夜靜置，且非水性液體（庚烷或丙酮）易於 瘵發。以最小力藉使通過4 mm篩子以粗略分解已形成之所 145392.doc -10· 201034966 得乾塊體。包含顯著量之大聚集體之所得產Ο 4 / Μ π肚〜^丨π厓σο進行分散測 試。結果係顯示於下表3中： 表3 樣本 分散 在丙酮中乾燥之Tiona 188 436 在庚烧中乾燥之Tiona 188 丨•丨 ______ 485~— 可見從非水性液體乾燥Tiona 1 88，即使已形成大聚集體 時亦分解產生等同於非聚集之Tiona 188粉末的分散值。兩 〇 個結果係在實例中所用作為分散標準品之非聚集之Tiona 188粉末的1標準偏差内。 實例4-從非水性液體乾燥 如先前實例所用相同之Tiona 188係在（a)己烷或（b)丙酮 中以50〇/〇固體製成漿液並隨後於噴霧乾燥器中利用熱氮氣 作為乾燥方式乾燥之。收集產品並測試其分散，且結果係 顯示於下表4中： 〇 表4 樣本 分散 _^_丙_中噴霧乾燥之Tiona 188 719 在己烧中噴霧乾燥之Tiona 188 749 利用喷霧乾燥器從非水性液體（丙酮/己烷）乾燥之產品顯 不在非聚集之Tiona 188之1標準偏差内並可視為統計上相 當之分散值。 實例5-從非水性液體乾燥 網1如先前實例中所用之Tiona 188製成己烷中含有73%固 145392.doc 201034966 體之糊料，並令其擠壓通過填料槍，使_壓製品直徑在 至1/2"之範圍内變化。令所得產品在通風櫥中 集之並進行分散測試。結果係顯示於下表5中.' 、 表5 樣本 1/8"擠壓製品 1/4”擠壓製品 1/2”擠壓製品Barreling 1 · 5 hours ~ - barreling for 18 hours dispersion (XRF count) 1127 4107 Visible barrel flow and aggregation example 2 - compaction longer barreling time favors powder J45392.doc 201034966 50 pounds with example 1 The same pigment used (Tiona 188) was rolled through the pressure of a Fitzpatrick Company L-83 compactor. The cylinder is rolled under pressure to allow the Tiona 1 88 powder to pass between the rolls and compacted by the applied pressure. The rolls were operated at 5 rpm and had a press pressure of 400 psi. The product is made into small pieces of different aggregate sizes gathered in many sieves. The dispersion test was carried out for each sieve fraction and the results are shown in Table 2 below: Table 2 Sample dispersion 14 sieve fraction 5148 20 sieve fraction 4344 30 sieve fraction 2769 3 5 sieve fraction 3140 40 sieve Fractionation grade 3912 5 0 sieve fraction grade 4281 7 0 sieve fraction grade 6577 disc (residual fine powder) 4213 It can be seen that regardless of the sieve fraction to be tested, the pigment is passed through the pressure roller to compact the pigment. The dispersion is substantially reduced. Example 3 - Drying from a non-aqueous liquid 171 g of Ti〇na 188 as used in Example} and (a) 231 g of heptane or (bp% g of acetone in a 1 quart container using a c〇wles disperser at 3〇〇 Mix 〇 rpm. Allow the resulting mixture to stand overnight, and the non-aqueous liquid (heptane or acetone) is easy to burst. Use a 4 mm sieve to roughly decompose the formed 145392.doc -10· 201034966 Bulk. The resulting calves containing a significant amount of large aggregates were subjected to a dispersion test. The results are shown in Table 3 below: Table 3 Samples dispersed in acetone to dry Tiona 188 436 Tiona 188 干燥•丨______ 485~ dried in g-burning. It can be seen that Tiona 1 88 is dried from a non-aqueous liquid, and even if large aggregates have formed, it decomposes to produce a dispersion value equivalent to non-aggregated Tiona 188 powder. The results are within 1 standard deviation of the non-aggregated Tiona 188 powder used as a dispersion standard in the examples. Example 4 - Drying from a non-aqueous liquid The same Tiona 188 system used in the previous examples was in (a) hexane or (b) a slurry of 50 〇/〇 solid in acetone It was then dried in a spray dryer using hot nitrogen as a dry method. The product was collected and tested for dispersion, and the results are shown in Table 4 below: 〇 Table 4 Sample Dispersion _^_C_ Medium Spray Drying Tiona 188 719 Spray drying of Tiona 188 749 in a dry run The product dried from a non-aqueous liquid (acetone/hexane) using a spray dryer is not within 1 standard deviation of the non-aggregated Tiona 188 and can be considered as a statistically equivalent dispersion value. Example 5 - From a non-aqueous liquid drying web 1 Tiona 188 as used in the previous examples was prepared as a paste containing 73% solid 145392.doc 201034966 in hexane and extruded through a filler gun to make the diameter of the compact Within the range of 1/2", the resulting product was collected in a fume hood and subjected to dispersion testing. The results are shown in Table 5 below. ', Table 5 Sample 1/8"Extrusion 1/4" Extruded product 1/2" extruded product
從非水性液體乾燥之產品顯示TIT'一~ 、，死冲上與非聚集之精細分 散顏料不可區別之分散值。即使 、 车兹》…t 使顏枓恳合物聚集成直徑如 +央吋般大，未觀察到可分散性降低。 以上實例證明從非水性液體之八 m ^ m ., iA 、、’刀散顏料形成糊料或 衆液並繼以乾⑭之以形成根據本發明之 磨及壓實之先前技術㈣方法相 /會產生與滚 品。 匕日寻分散&降低之聚集虞 前述本發明實施例係基於 限制本發⑽㈣提出^欲詳述或 性時’可考慮各種等效物。 Η境暗以賦予適具 H5392.doc -12-Products that are dried from non-aqueous liquids exhibit a dispersive value that is indistinguishable from the non-aggregated finely divided pigments of TIT's. Even if the car is...t, the aggregation of the pigments is as large as the diameter, and no dispersibility is observed. The above examples demonstrate the formation of a paste or a liquid from a non-aqueous liquid of eight m ^ m . , iA , , and a dry powder to form a prior art (4) method according to the present invention. Will produce and roll. The following is an embodiment of the present invention which is based on the limitation of the present invention (10) (4). The dilemma is dark to give the appropriate H5392.doc -12-