TW386101B - Flaky aluminum oxide and pearlescent pigment, and productioon thereof - Google Patents
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A7 B7 五、發明説明（1 ) 本發明係關於一種由氧化鋁和二氧化鈦組成的新等級 片狀氧化鋁及其製法。包含二氧化欽的片狀氧化鋁的特徵 爲其大的外觀比（aspect ratio)(粒徑/厚度）和非常· 小的傾向形成結晶和聚集（ aggregation)。本發明也關 於一種將金屬氧化物塗在片狀氧化鋁而形成具有珍珠光澤 的顏料。具有珍珠光澤的顏料係當做油漆，塑膠，墨水， 化妝品和釉的原料 。 - 〔先前技術〕 已知具有珍珠光澤的顏料係藉由將具有高折射率的金 屬氧化物（例如二氧化鈦）塗在片狀基材（例如雲母薄片 )而形成。這類顔料想要用的基材係爲品質穩定的合成物 質，例如片狀氧化鐵，片狀二氧化鈦，和鋁，塗以明膠的 (doped)片狀氧化鐵，已經發展而出來而且最近已上市 〇 經濟部中央標準局員工消費合作社印製 (請先閲讀背面之注意事項再填寫本頁) 對於有更好的珍珠光澤，基材必需是均勻薄度具有大 外觀比（或相對厚度有大的直徑）的薄片，極無色和透明 而且片狀抗熱性好和片狀機械強度高。 具有高硬度的氧化鋁係當做耐磨性材料，陶器材料， 油漆顏料，研磨劑等來使用。已經努力嘗試製造已經改良 特徵性質的簡單片狀氧化鋁。到現在爲止，實行的典型例 子如下。 •六角形薄片形狀的α —氧化鋁，具有比1 0 大 的粒徑以k外觀比（粒徑/厚度）5_10。（日本專利 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） ~~ -4 - 經濟部中央標率局員工消費合作社印製 A7 B7 五、發明説明（2 ) 公開案第111239號/1982) •片狀α-氧化鋁，具有平均粒徑〇.5-3vm。 (日本專利公告第72527號/1991) •六角形小板單一結晶形狀的α —氧化鋁，厚〇 . 1 一 2#m而直徑2 — 20mm，外觀比5 — 40。（日本 專利公開案第1 3 1 5 1 7號/ 1 9 9 1 ) •六角形結·晶系統細平（fine platy)粒子形-狀的氧 化鋁，具有與發展進入板.內之c軸垂直的平面。（日本專 利公開案第39362號/1992) 然而，結果變成，這些種類氧化鋁不適合當做具有珍 珠光澤顏料用的片狀基材，因爲粒徑過小，外觀比小，強 烈傾向於形成結晶和聚集和水中分散性差。除此之外，因 爲其在水中的分散性差而且是獨自由氧化鋁組成，如此的 氧化鋁粒子很難將金屬氧化物塗上。即使塗覆是可能的， 所產生經塗覆的粒子係爲不均匀的金屬氧化物直徑的粒子 而且容易聚集，並且只認爲是暗珍珠色。結果，它們不適 合當做具有珍珠光澤顔料用的基材來使用。而且，上述氧 化鋁粒子的缺點爲其通常利用需要昂貴高壓反應器的水熱 法（hydrothermal process)(如日本專利公開案第 39362號/1992所揭示）而得。 本發明意圖要克服上述先前技術有關的問題。本發明 目的係提供片狀氧化鋁（當做基材使用），其特徵爲具有 比傳統片狀氧化鋁大的外觀比，均句小的厚度，平滑的表 面，幾乎完全無色和非常小的傾向形成結晶和聚集。本發 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） (請，先鬩讀背面之注意事項再填寫本頁) 釘 -5 ~ A7 ____B7_ 五、發明説明（3 ) 明另一目的係提供將金屬氧化物塗在片狀氧化鋁而形成具 有珍珠光澤的顔料。本發明另一目的係提供製.造該片狀氧 化鋁的簡單方法。 〔發明內容〕 本發明揭示一種新等級的片狀氧化鋁，該片狀氧化鋁 具有珍珠光澤顏料用基材所需的傑出特質。片狀氧·化鋁係 由氧化鋁（作爲主要的成份）和二氧化鈦（當做次要成份 )所組成。其係藉由將水溶性鋁鹽和鈦鹽的均勻水溶液與 鹼式碳酸鹽水溶液在含有鹼金屬硫酸鹽和磷酸（或磷酸鹽 )的水溶液共存之下水解，藉由蒸發（加熱脫水）乾燥， 以及熔鹽處理（molten-salt treatment)而製得。 本發明的第一部份係在於包括含有二氧化鈦在其中的 片狀氧化鋁。 經濟部中央標準局員工消費合作社印製 (請先閣讀背面之注意事項再填寫本頁) 本發明的第二部份係在於製造片狀氧化鋁的方法，該 方法包括製備步驟如下：（a .)水溶性鋁鹽和鈦鹽的水溶 液和（b )與該水溶液（a )裡之該水溶性鋁鹽和鈦鹽大 約等量的驗式碳酸鹽水溶液，將鹼金屬硫酸鹽和磷酸或_磷 酸鹽均勻地溶解在不是水溶液（a )裡就是水溶液（b ) 裡，將該水溶液（a )和（b )混合以得到懸浮液或含有 水解產物（hydrolyzates)的膠體，藉由蒸發將懸浮液或 膠體乾燥以及將經乾燥的產法藉由在9 0 〇 — 14 0 〇。(： 加熱作熔鹽處理而得到固體的產物’將該產物用水清洗， 過濾及乾^而完成。 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） " ~~ —6 - 經濟部中央標準局員工.消費合作社印製 A7 B7 五、發明説明（4 ) 本發明的第三部份係在於製造片狀氧化鋁的方法，該 方法包括以下步驟：逐滴地將水溶性鋁鹽溶液和鹼式碳酸 鹽溶液同時地以前者化學當量約等於後者化學當量的方式 加入水中，藉此形成經水解的氫氧化鋁懸浮液，將該懸浮 液（或將該懸浮液過濾掉所得的固體）加入鹼金屬硫酸鹽 水溶液裡，將鈦鹽和磷酸或磷酸鹽加到所得的溶液裡以得 到懸浮液或含有水解產物的膠體，藉由蒸發將懸浮·液或膠 體乾燥，以及將經乾燥的產法藉由在9 0 0 — 1 4 0 0°C •加熱作熔鹽處理而得到固體的產物，將該產物用水清.洗， 過濾及乾燥而完成》 本發明的第四部份係在於具有珍珠光澤的顏料包括該 片狀氧化鋁的粒子以及形成在該粒子表面上的金屬氧化物 塗層。 本發明的第五部份係在於油漆，塑膠，墨水，化妝品 ，或釉組.合物包括其中含有該片狀氧化銘或該具有珍珠光 澤的顏料。 本發明係具體說明包含二氧化鈦的片狀氧化鋁。與單 獨由氧化鋁組成的傳統氧化鋁作比較，其具有比’較大的粒 徑，均匀比較小的厚度，和比較大的外觀比。除此，還具 有平滑的表面以及非常小的傾向形成結晶和聚集，是基材 所需的傑出特質。其可取用高折射率的金屬氧化物來塗覆 以得到散發很好珍珠色澤的具有珍珠光澤之顏料。該具有 珍珠光澤的顏料係適合用來作爲塑膠，油漆，墨水，化妝 品和袖。 _ 本紙張尺度適用中國國家標準（CNS ) A4規格（21〇X297公釐） —I— I — - I ^ n I (請先聞讀背面之注意事項再填寫本頁)A7 B7 V. Description of the invention (1) The present invention relates to a new grade of flaky alumina composed of alumina and titania and a method for producing the same. The flaky alumina containing dioxin is characterized by its large aspect ratio (particle size / thickness) and its very small tendency to form crystals and aggregation. The present invention also relates to a pigment having a pearly luster by applying a metal oxide to flaky aluminum oxide. Pearlescent pigments are used as raw materials for paints, plastics, inks, cosmetics and glazes. -[Prior Art] It is known that a pigment having a pearly luster is formed by applying a metal oxide (such as titanium dioxide) having a high refractive index to a sheet-like substrate (such as a mica flake). The substrates for which these pigments are intended are synthetic materials of stable quality, such as flake iron oxide, flake titanium dioxide, and aluminum, and doped flake iron oxide coated with gelatin have been developed and recently marketed 〇 Printed by the Consumer Cooperatives of the Central Bureau of Standards of the Ministry of Economic Affairs (please read the precautions on the back before filling this page) For better pearl luster, the substrate must be uniformly thin and have a large appearance ratio (or relatively thick Diameter) sheet, is extremely colorless and transparent, and has good heat resistance and high mechanical strength. Alumina with high hardness is used as abrasion-resistant materials, pottery materials, paints, and abrasives. Efforts have been made to make simple flaky aluminum oxides with improved characteristic properties. The typical examples so far are as follows. • Alpha-alumina in the shape of hexagonal flakes with a particle size larger than 10 and an appearance ratio (particle size / thickness) of 5-10. (Japanese paper size of this paper applies Chinese National Standard (CNS) A4 specification (210X297 mm) ~~ -4-Printed by the Consumer Standards Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs A7 B7 V. Invention Description (2) Publication No. 111239 / 1982) • Flaky α-alumina with an average particle size of 0.5-3 vm. (Japanese Patent Bulletin No. 72527/1991) • Hexagonal small plate of α-alumina in a single crystal shape, with a thickness of 0.1 to 2 #m and a diameter of 2 to 20 mm, and an appearance ratio of 5 to 40. (Japanese Patent Laid-Open No. 1 3 1 5 1 7/1 9 9 1) • Hexagonal junction and crystal system fine platy particle-shaped alumina, which has developed into the c-axis of the plate. Vertical plane. (Japanese Patent Laid-Open No. 39362/1992) However, as a result, these types of aluminas are not suitable as flaky substrates with pearlescent pigments, because the particle size is too small, the appearance ratio is small, and there is a strong tendency to form crystals and aggregates. Poor dispersion in water. In addition, it is difficult to coat metal oxides with such alumina particles because of its poor dispersibility in water and because it is composed of alumina alone. Even if coating is possible, the resulting coated particles are particles of non-uniform metal oxide diameter and are easily aggregated, and are considered only dark pearly. As a result, they are not suitable for use as a substrate for a pearly pigment. Moreover, the above-mentioned aluminum oxide particles have a disadvantage that they are generally obtained by a hydrothermal process that requires an expensive high-pressure reactor (as disclosed in Japanese Patent Laid-Open No. 39362/1992). The present invention is intended to overcome the problems associated with the foregoing prior art. The object of the present invention is to provide flaky alumina (used as a substrate), which is characterized by a larger appearance ratio than traditional flaky alumina, a small thickness, a smooth surface, almost completely colorless and a very small tendency to form. Crystallize and aggregate. The paper size of this issue applies to the Chinese National Standard (CNS) A4 specification (210X297 mm) (please read the precautions on the back before filling this page) Nail -5 ~ A7 ____B7_ V. Description of the invention (3) Specify another The object is to provide a pigment with pearl luster by coating a metal oxide on flake aluminum oxide. Another object of the present invention is to provide a simple method for making and manufacturing the flake aluminum oxide. [Summary of the Invention] The present invention discloses a new class of flaky alumina having excellent characteristics required for a base material for a pearl gloss pigment. The flake oxygen and aluminum oxide system is composed of alumina (as a main component) and titanium dioxide (as a secondary component). It is prepared by hydrolyzing a homogeneous aqueous solution of water-soluble aluminum and titanium salts and an aqueous solution of a basic carbonate in the coexistence of an aqueous solution containing an alkali metal sulfate and phosphoric acid (or phosphate), and drying by evaporation (heating dehydration), And molten salt treatment (molten-salt treatment). The first aspect of the present invention consists in including a flake alumina containing titanium dioxide therein. Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs (please read the notes on the back before filling out this page) The second part of the present invention is a method for manufacturing flake alumina, which includes the following steps: (a .) The aqueous solution of water-soluble aluminum and titanium salts and (b) an aqueous carbonate solution of approximately the same amount as the water-soluble aluminum and titanium salts in the aqueous solution (a), the alkali metal sulfate and phosphoric acid or _ The phosphate is uniformly dissolved in either the aqueous solution (a) or the aqueous solution (b), and the aqueous solutions (a) and (b) are mixed to obtain a suspension or a colloid containing hydrolyzates, and the suspension is evaporated by evaporation Or colloid drying and drying the production method by 900-1400. (: Solid product obtained by heating for molten salt treatment 'This product is washed with water, filtered and dried ^. This paper size applies Chinese National Standard (CNS) A4 specification (210X297 mm) " ~~ --6- Employees of the Central Standards Bureau of the Ministry of Economic Affairs. Printed by the Consumer Cooperative A7 B7. 5. Description of the Invention (4) The third part of the present invention is a method for manufacturing flake alumina. The method includes the following steps: dropwise water-soluble aluminum The salt solution and the basic carbonate solution are simultaneously added to water in such a manner that the former chemical equivalent is approximately equal to the latter chemical equivalent, thereby forming a hydrolyzed aluminum hydroxide suspension, and the suspension (or the resulting suspension is filtered off Solid) is added to the aqueous alkali metal sulfate solution, titanium salt and phosphoric acid or phosphate are added to the resulting solution to obtain a suspension or a hydrolysate-containing colloid, the suspension or the colloid is dried by evaporation, and the dried The production method is completed by heating at 900-1400 ° C. • The product is obtained as a molten salt by heating. The product is washed with water, filtered, and dried. The fourth part is that the pigment with pearl luster includes the particles of the flake alumina and the metal oxide coating formed on the surface of the particles. The fifth part of the present invention is paint, plastic, ink, cosmetics, Or the glaze composition includes the flake oxide or the pigment with pearl luster therein. The present invention specifically describes the flake alumina containing titanium dioxide. Compared with the traditional alumina composed of alumina alone, it has Larger particle size, uniform and smaller thickness, and larger appearance ratio. In addition, it has a smooth surface and a very small tendency to form crystals and aggregates, which is an outstanding characteristic required for substrates. It is desirable Coated with high-refractive metal oxides to obtain pearlescent pigments with good pearl luster. The pearlescent pigments are suitable for use in plastics, paints, inks, cosmetics and sleeves. _ This paper size Applicable to China National Standard (CNS) A4 specification (21 × 297 mm) —I— I —-I ^ n I (Please read the precautions on the back before filling in this page)
-、tT ./k.. -7 - A7 B7 _ 五、發明説明（5) 本發明的片狀氧化鋁係由下列詳細地說明的方法來製 造。 第一個方法係如申請專利範圍第4項所定義。 該方法一開始先製備二個水溶液（a)和（b)。水 溶液（a )係由水溶性鋁鹽和鈦鹽來製備。前者可以選自 各種鋁鹽，其中因取得性和操作性質之故所以硫酸鋁和硝 酸鋁是令人想要。鈦鹽可以選自四氯化鈦，三氯化鈦，過 硫酸欽（_ti tan ium oxy sill fate)，和硫i 酸欽酸（titan yl sulfate)。鈦鹽的用量係因所需產物的形狀（粒徑，厚 度，和外觀比）而不同。通常是氧化鋁用量的0.1— . 經濟部中央橾準局員工消費合作社印製 (請先聞讀背面之注意事項再填寫本頁) 4 · 0重量％，最好是0 . 5 — 3 . 0重量％ (以氧化物 作計算）。鈦鹽在熔鹽處理法的結晶生長期間會防止結晶 形成和聚集。除此，鈦在藉由將金屬氧化物塗到基材上來 '製備具有珍珠光澤顏料的方法裡會幫助金屬氧化物附著到 片狀氧化鋁（當做基材）。少於0 . 1重量％的鈦鹽不足 以防止結晶形成和聚集》相反地，超過4 . 0重量％的鈦 鹽會避免片狀氧化鋁的形成。在製備溶液（a )方面，加 熱將會促進組份的溶解。 ： 水溶液（b )係由從鹼式碳酸鹽以中和用和水解成水 溶性（a )裡水溶性鋁鹽及鈦鹽用的大約相等化學當量來 製備。令人想要的鹼式碳酸鹽係爲碳酸鈉和碳酸鉀。 將鹼金屬硫酸鹽（當做礦化劑（mineralize.r))和 磷酸或磷酸鹽（以下統稱爲磷系化合物）加到水溶液（a ) 或（ιΓ)裡》可能將二個組份一起加到不是（a ) 就 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） '~ — -8 一 經濟部中央標準局員工消費合作社印製 A7 ____B7 ___ 五、發明説明（6 ) 是（b)裡或將其每一個分別加入（a) 和（b)裡。 重要的是要確定在那些溶液 （a )和（b )裡完全地溶 解。 鹼金屬硫酸鹽（當做礦化劑）的例子包括硫酸鈉，硫 酸鉀和硫酸鋰。由於取得性，故前二個是最令人想要的。 他們可以彼此組合來使用。礦化劑的用量（莫耳）應該是 水溶性鋁鹽用量的1到5倍。如果小於上述用量的.話，礦 化劑將不會完全發揮熔鹽加熱處理和製成片狀（flaking )的效果。用量比上述多的話，將浪費礦化劑而沒有增 加效果，並且再接著的步驟裡需要大量的水來沖掉。 磷系化合物可以是選自下列化合物的任何水溶性化合 物：磷酸，.磷酸鹽，濃縮磷酸及濃縮磷酸鹽。例子包括磷 酸’一級碟酸納（sodium secondary隣.酸鹽）’ 一級隣酸 鈉，二級磷酸鉀，一級磷酸鉀，磷酸銨，焦磷酸鈉（pyro-, TT ./k .. -7-A7 B7 _ 5. Explanation of the invention (5) The flake alumina of the present invention is produced by the method described in detail below. The first method is defined in item 4 of the scope of patent application. The method begins by preparing two aqueous solutions (a) and (b). The aqueous solution (a) is prepared from water-soluble aluminum and titanium salts. The former can be selected from a variety of aluminum salts, of which aluminum sulfate and aluminum nitrate are desirable due to availability and operational properties. The titanium salt may be selected from titanium tetrachloride, titanium trichloride, ti tan ium oxy sill fate, and titanyl sulfate. The amount of titanium salt varies depending on the shape (particle size, thickness, and appearance ratio) of the desired product. It is usually 0.1% of the amount of alumina.. Printed by the Consumer Cooperatives of the Central Bureau of Standards, Ministry of Economic Affairs (please read the precautions on the back before filling out this page) 4 · 0% by weight, preferably 0.5-3. 0 % By weight (calculated as oxide). Titanium salts prevent crystal formation and aggregation during the crystal growth of the molten salt process. In addition, titanium will help the metal oxide to adhere to the flake alumina (as the substrate) in the method of preparing a pearlescent pigment by applying a metal oxide to the substrate. Less than 0.1% by weight of titanium salt is not sufficient to prevent crystal formation and aggregation. Conversely, more than 4.0% by weight of titanium salt will prevent the formation of flaky aluminum oxide. In preparing solution (a), heating will promote dissolution of the components. : The aqueous solution (b) is prepared from approximately equal chemical equivalents of basic carbonates for neutralization and hydrolysis to water-soluble aluminum and titanium salts in water-soluble (a). Desirable basic carbonates are sodium carbonate and potassium carbonate. Adding alkali metal sulfate (as mineralizer.r) and phosphoric acid or phosphate (hereinafter collectively referred to as phosphorus compounds) to the aqueous solution (a) or (ιΓ) may add the two components together No (a) Applicable Chinese National Standard (CNS) A4 specification (210X297 mm) for this paper size '~ — -8 Printed by A7 Consumer Cooperatives of the Central Bureau of Standards of the Ministry of Economic Affairs A7 ____B7 ___ V. Invention Description (6) Yes ( b) or add each of them separately to (a) and (b). It is important to determine that those solutions (a) and (b) are completely dissolved. Examples of alkali metal sulfates (as mineralizers) include sodium sulfate, potassium sulfate and lithium sulfate. The first two are the most desirable because of their accessibility. They can be used in combination with each other. The amount of mineralizer (mol) should be 1 to 5 times the amount of water-soluble aluminum salt. If it is less than the above amount, the mineralizer will not fully exert the effects of heat treatment of molten salt and flake formation. If the amount is more than the above, the mineralizer will be wasted without increasing the effect, and a large amount of water will be needed in the next step to flush it away. The phosphorus-based compound may be any water-soluble compound selected from the group consisting of phosphoric acid, phosphate, concentrated phosphoric acid, and concentrated phosphate. Examples include phosphoric acid ’sodium secondary orthophosphate.’ Sodium orthophosphate, potassium secondary phosphate, potassium primary phosphate, ammonium phosphate, sodium pyrophosphate (pyro
Phosphate)，焦磷酸鉀，三聚磷酸鈉，三聚磷酸鉀，和 三聚磷酸銨。磷系化合物藉由加熱使熔鹽處理期間的結晶 變成片狀。使用比〇.1重量％少的用量，將不會產生所 需的薄片狀氧化鋁。使用超過2 . 0重量％的用量，將不 會得到減少片狀氧化鋁的厚度方面的加成效果β在製備溶 液（b )方面，加熱將會促進組份的溶解。 將上述製得的水溶液（a )和（b ) —起攪拌混合以 其水解。混合操作可以利用下列（1 )或（2 )方式完成 〇 (1)同時滴入。該方法係同時將水溶液（a )和（ 本紙張尺度適用中國國家標隼（CNS > A4規格（210、x 297公釐） ： ~ -9 - ---------衣-----一 I 訂 (請先閔讀背面之注意事項再填寫本頁) A7 B7 五、發明説明（7) b )逐滴地加入水中，而前者大約相等於後者。 (2)簡單地加入。該方法係將溶液（a )攪拌加入 溶液（b )所組成’反之亦然。所產生的產物係爲懸浮液 或含有水解產物的膠體。 藉著方法（1 )或（2)會導致懸浮液或膠體包含物 均勻地分散在水性介質裡的水合氧化鋁（細微粒子的形狀 )’礦化劑，水合二氧化鈦和磷系化合。接著將懸-浮液或 膠體藉由蒸發脫水並乾燥。爲了要節省乾燥用的熱量，想 要用足以使溶液成爲幾乎飽和的最小水量來製備水溶液（ a)和（b) »達成這個目的另外的方法係爲藉由加熱那 些水溶液（a)和（b)，藉此在開始上述方法 （1.) 經濟部中央標準局員工消費合作社印製 (請先閲讀背面之注意事項再填寫本頁) 或（2)之前將鹽類濃縮。無論任何方式，水溶液（a )和（b ) 應該包含特定量的水比確定完全溶解。如果 二個溶液之一或二個溶液全部包含未溶解的物質時，其混 合結果會造成由於形成結晶和聚集而導致不是片狀且不均 勻產物的不完全水解。換句話說，水溶液（a )和（b ) 應該均勻地溶解的溶液。接著將徹底地脫水的產物在 9 0 0 _ 1 4 0 0 °C熱處理》將所-生的產物用水清洗以 除去黏在上面的自由態化合物（主要是硫酸鹽）。最後將 洗過的產物乾燥。這樣獲得了所需的片狀氧化鋁。 第二個方法係如申請專利範圍第 5項所定義者。 該方法採用如上述第一個方法所用由相同材料預先已 經製備的原料氫氧化鋁。氫氧化鋁係藉由將水溶性鋁鹽的 溶液和鹼式碳酸鹽溶液同時地逐滴加入水中，使鹼式碳酸 本紙張又度適用中國國家標準（CNS ) A4規格（210X297公釐） -10 - A7 B7 五、發明説明（8 ). 鹽大約等於鋁鹽而製得。將所產生含有水合氧化鋁（或藉 由清洗和過濾從懸浮液分離出來的固體）的懸浮液加入當 做礦化劑的鹼金屬硫酸鹽水溶液》(鹼金屬硫酸鹽應最好 是水溶性鋁鹽數量的1到5倍（莫耳）。）此外將鈦鹽和 磷酸鹽加入所產生的溶液裡。（鈦鹽的數量應最好以二氧 化鈦作計算，是氧化鋁數量的0 . 1 - 4 . 0重量％。.礙 酸鹽的用量應該最好以P2 05作計算，是氧化鋁用-量的 0· 1 — 2.0重量％。）將所產生的懸浮液以上述第一 .個方法所用相同，的蒸發方式徹底地脫水。在脫水步驟期間 ，將仍未水解的鈦鹽熱水解。將已脫水的產物在9 0 0 -1 4 0 0°C熔鹽加熱處理。將所產生的產物用水清洗以除 去黏在上面的自由態化合物（主要是硫酸鹽）。最後將洗 過的產物乾燥。這樣獲得了所需的片狀氧化鋁。附帶一提 地，該方法所用的水合氧化鋁可以用市售可得的氧化鋁溶 膠（alumina sol)或細微粒子形狀的氧化銘來替代。 經濟部中央標準局員工消費合作社印製 (請先閱讀背面之注意事項再填寫本頁) 爲了調査其物理性質，將上述根據本發明製得的片狀 氧化銀樣品以掃描式電子顯微鏡來檢查。發現平均粒徑5 —6 0 # m ’厚度比1 μ m小以及外觀比小於2 〇。也發 現沒有任何結晶的形成和聚集並且可到水裡迅速地分散；。 將可以由將片狀氧化銀樣品分散在水裡並攪拌時得到 流線型結果（streamline)的這個事實來.證明分散性佳。 (流線型結果係爲光線在液體懸浮並流動的片狀粒子表面 反射而產生的薄層條紋圖案。） 由片k氧化鋁的化學分析得知，其包含幾乎與起始材 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -11 經濟部中央標準局負工消費合作社印製 A7 B7 ___ 五、發明説明（9〉 料包含一樣多的欽以及得知其只包含痕量（trace amount )的磷。因而推測本發明方法所用的磷化合物會產生使氧 化鋁成爲片狀的效果，但是最後會從系統釋放並且去除。 磷系化合物在後來的步驟裡會鼙助金屬氧化物附著到那些 氧化鋁粒子。可能的理由係爲痕量的磷在熱處理的步驟裡 改良了氧化鋁粒子表面的性質。 因此，本發明所定義的片狀氧化鋁係由氧化銘·（當做 主要的組份）和二氧化鈦（當做次要的組份）而組成。 本發明具有珍珠光澤的顏料係藉由將高折射率的金屬 氧化物（例如二氧化鈦和氧化锆）塗到該片狀氧化鋁（ 當做基材）而製得。塗層產生銀色調或視塗層厚度而定產 生干涉顏色（interference color)。如果塗層材料被著 色的金屬氧化物，例如氧化鐵替換的話，則所產生具有珍 珠光澤的顏料將會呈現微紅的或帶黑色的顏色。 有金屬氧化物的塗層可以利用任何已知的方法來完成 ，例如藉由加熱或鹼將金屬鹽水解，使水合的金屬氧化物 沉積，接著鍛燒。如果該鍛燒步驟係在減少大氣壓下進行 的話，所產生具有珍珠光澤的顏料混會因爲低氧化狀態的 二氧化鈦或氧化鐵而呈現帶黑色的顏色。 要將具有金屬氧化物塗在單獨由氧化鋁組成之片狀氧 化鋁的傳統基材上是困難的。相反地，本發明的片狀氧化 鋁非常善於接納金屬氧化物。所產生的金屬氧化物塗層是 非常薄而且均匀，因此產生極佳珍珠光澤的色澤。 本發_的具有珍珠光澤顏料或由其衍生的片狀氧化鋁 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） (請先閱讀背面之注意事項再填寫本頁)Phosphate), potassium pyrophosphate, sodium tripolyphosphate, potassium tripolyphosphate, and ammonium tripolyphosphate. The phosphorus-based compound is heated to cause the crystals during the molten salt treatment to become flaky. Using less than 0.1% by weight will not produce the desired flaky aluminum oxide. If the amount exceeds 2.0% by weight, the addition effect of reducing the thickness of the flake alumina will not be obtained. In the preparation of the solution (b), heating will promote the dissolution of the components. The aqueous solutions (a) and (b) prepared above were stirred and mixed together for hydrolysis. The mixing operation can be completed by the following (1) or (2) methods: (1) Simultaneous dripping. This method uses both the aqueous solution (a) and (this paper size applies the Chinese national standard (CNS > A4 size (210, x 297 mm)): ~ -9---------- clothing- --- Order I (please read the notes on the back before filling this page) A7 B7 V. Description of the invention (7) b) Add water dropwise, and the former is approximately equal to the latter. (2) Simply add This method involves adding solution (a) with stirring to solution (b) and vice versa. The product produced is a suspension or a hydrocolloid-containing colloid. Suspension can be caused by method (1) or (2) Liquid or colloidal inclusions are hydrated alumina (fine particle shape) 'mineralizing agent, hydrated titanium dioxide and phosphorus-based compounds uniformly dispersed in an aqueous medium. Then the suspension-float or colloid is dehydrated by evaporation and dried. To save heat for drying, it is desirable to prepare aqueous solutions (a) and (b) with a minimum amount of water sufficient to make the solution almost saturated. Another way to achieve this is by heating those aqueous solutions (a) and (b). To start the above method (1.) Member of the Central Standards Bureau of the Ministry of Economic Affairs Printed by a consumer cooperative (please read the notes on the back before filling out this page) or (2) concentrate the salts before. In any case, the aqueous solutions (a) and (b) should contain a specific amount of water ratio to determine complete dissolution. If one or both of the two solutions contain undissolved substances, the result of their mixing will result in incomplete hydrolysis of non-flaky and heterogeneous products due to crystal formation and aggregation. In other words, the aqueous solution (a) And (b) a solution that should dissolve uniformly. Then the thoroughly dehydrated product is heat-treated at 900 0 -1 400 ° C. The resulting product is washed with water to remove free-state compounds (mainly Is the sulfate salt). Finally, the washed product is dried. In this way, the desired flaky alumina is obtained. The second method is as defined in item 5 of the scope of patent application. This method uses the first method described above. The raw material aluminum hydroxide which has been prepared in advance from the same material. Aluminum hydroxide is a solution in which a water-soluble aluminum salt solution and a basic carbonate solution are simultaneously added dropwise to water to make basic carbonate Zhang Youdu applies the Chinese National Standard (CNS) A4 specification (210X297 mm) -10-A7 B7 V. Description of the invention (8). The salt is approximately equal to the aluminum salt. It is produced by containing hydrated alumina (or by Wash and filter the solids separated from the suspension) The suspension is added to the aqueous alkali metal sulfate solution as a mineralizer (the alkali metal sulfate should preferably be 1 to 5 times (mole) the amount of water-soluble aluminum salt. ) In addition, the titanium salt and phosphate are added to the resulting solution. (The amount of titanium salt should preferably be calculated based on titanium dioxide, which is 0.1 to 4.0% by weight of the amount of alumina. It is preferably calculated based on P205, which is 0.1 to 2.0% by weight of the amount of alumina used. ) The resulting suspension is completely dehydrated by evaporation in the same manner as in the first method above. During the dehydration step, the still unhydrolyzed titanium salt is thermally hydrolyzed. The dehydrated product is heat-treated at 900-400 ° C molten salt. The resulting product is washed with water to remove free-state compounds (mainly sulfates) that stick to it. The washed product is finally dried. This gives the desired flaky alumina. Incidentally, the hydrated alumina used in this method can be replaced with a commercially available alumina sol or fine particle-shaped oxide inscription. Printed by the Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs (please read the notes on the back before filling this page). In order to investigate its physical properties, the flake silver oxide samples prepared according to the present invention were examined with a scanning electron microscope. It was found that the average particle diameter was 5-6 0 # m 'having a thickness smaller than 1 µm and an appearance ratio of less than 20. It was also found that there was no formation and aggregation of any crystals and that it could disperse into water quickly; The fact that the flake silver oxide sample is dispersed in water and stirred to obtain a streamlined result will prove that the dispersion is good. (The streamlined result is a thin layered stripe pattern caused by the reflection of light on the surface of the flake particles in which the liquid is suspended and flowing.) According to the chemical analysis of flake alumina, it contains almost the same size as the starting material. Standard (CNS) A4 specification (210X297 mm) -11 Printed by the Central Standards Bureau of the Ministry of Economic Affairs and Consumer Cooperatives printed A7 B7 ___ V. Description of the invention (9) The material contains the same amount of Chin and it is known that it contains only trace amounts (trace amount) of phosphorus. Therefore, it is speculated that the phosphorus compound used in the method of the present invention will have the effect of making alumina into a flake, but it will eventually be released and removed from the system. The phosphorus-based compound will assist metal oxides to adhere to Those alumina particles. The possible reason is that trace amounts of phosphorus improve the surface properties of the alumina particles during the heat treatment step. Therefore, the flaky alumina defined by the present invention is defined by the oxide name (as the main component) ) And titanium dioxide (as a minor component). The pearlescent pigments of the present invention are obtained by combining high-refractive index metal oxides (for example, Titanium dioxide and zirconia) are applied to the flake alumina (used as a substrate). The coating produces a silver tone or an interference color depending on the thickness of the coating. If the coating material is oxidized by the colored metal If a substance such as iron oxide is replaced, the resulting pearlescent pigment will appear reddish or blackish. Coatings with metal oxides can be done by any known method, such as by heating or Alkali hydrolyzes metal salt, deposits hydrated metal oxides, and then calcined. If this calcination step is performed under reduced atmospheric pressure, the pearlescent pigment mixture will be caused by titanium dioxide or iron oxide in a low oxidation state. It has a black color. It is difficult to apply a metal oxide to a conventional substrate of flaky alumina composed of alumina alone. On the contrary, the flaky alumina of the present invention is very good at receiving metal oxides. The resulting metal oxide coating is very thin and uniform, thus producing an excellent pearly luster. Luster pigments or derived from this paper sheet alumina scale applicable Chinese National Standard (CNS) A4 size (210X297 mm) (Please read the notes and then fill in the back of this page)
-12 - A7 _________B7_ 五、發明説明（lQ) 可能當做爲陶瓷原料或當做油漆，塑膠，墨水，化妝品和 釉的顏料。因其用途而定，將進行使其具有抗水性，耐氣 候性’化學抗性，抗退色性，或高分散力（dispersibili_ ty )的處理。 下列實施例係用來進一步地說明本發明，卻不會因此 限制本發明內容。 (實施例） , (片狀氧化鋁的製備方法） 實施例1 將2 2 3 . 8克硫酸銘1 8—水合物（aluminum su- .............* lfate 18-hydrate) ，1 1 4 . 5 克無水ϋ增及 9 3 · 7克_^酸鉀，藉由加熱到約7 5 °C的方式溶解在 450毫升去離子水裡。將2·0克34.4%硫酸鈦醯 、-------- 溶液加入所得的溶液裡。所得的溶液係稱爲水溶液（a ) 〇 在 250毫升的去離子水裡溶解0.9克三級磷酸 經濟部中央標隼局員工消費合作社印製 (請先閱讀背面之注意事項再填寫本頁) _銷1 2 —水合物和1 〇 7 .9克碳-鈉。產生的溶液係稱 ......——-...........-..............·· 爲水溶液（b )。 將水溶液（a )和（b )同時地以固定速率攪拌加入 200毫升去離子水，加入過程約經15分鐘，在如此方 式裡溶液（a )的溶質大約等於溶液（b)裡的溶質。再 繼續攪拌15 分鐘。將所產生的溶液蒸發到乾。將所產 生的固體茬大_1 2 0 0°C加熱5小時'。將水加入經熱處 --- - ·- _ 本紙張尺度適用中國國家標準（ciMS ) A4規格（;210 乂 297公釐）一 -13 - 經濟部中央標準局員工消費合作社印製 A7 B7 五、發明説明（u) 理過的產物以溶解自由態硫酸鹽。將不能溶解的固體過濾 掉’用水清洗’最後乾燥。如此獲得了所需的片狀氧化鋁 0 將如此獲得的片狀氧化鋁以X光衍射計（dif fractom-etry)檢查。繞射圖型僅有可歸於氧化.銘（剛玉）的波峰 。由化學分析發現片狀氧化鋁包含0 . 9 %二氧化鈦。由 光學顯微鏡和電子顯微鏡觀察，顯示片狀氧化鋁有.3 -1 6 的粒徑及約〇 . 2 的厚度而且沒有結晶的形 成。將片狀氧化鋁攪拌分散進水中時，片狀氧化鋁會產生 表示分散力佳的平滑流線型結果。 實施例2 將1 1 1 . 9克硫酸鋁18 —水合物，57 · 3克無 水硫酸鈉及4 6 · 9克硫酸鉀，藉由加熱到6 0 °C以上的 方式溶解在300毫升去離子水裡。將1 . 〇克34 . 4 %硫酸鈦醯溶液加入所得的溶液裡。所得的溶液係稱爲水 溶液（a )。 在1 5 0毫升的去離子水裡溶解0 . 4 5克三級磷酸 鈉1 2 -水合物和5 4 . 0克碳酸鈉。產生的溶液係稱爲 水溶液（b )。 將水溶液（b )攪拌加入已經加熱到約6 0 °C的水溶 液（a )。再繼續攪拌1 5分鐘。該兩種溶液的混合物係 爲膠體。將所產生的溶液蒸發到乾V將所產生的固體在大 約1 2 0 Ϊ) °C加熱5小時。將水加入經熱處理過的產物以 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） ' —~~ -14 - (請先閲讀背面之注意事項再填窝本頁) 0.-12-A7 _________B7_ 5. Description of the Invention (lQ) May be used as a ceramic material or as a pigment for paints, plastics, inks, cosmetics and glazes. Depending on its use, it will be treated to make it water-resistant, weather-resistant 'chemical resistance, fade resistance, or high dispersibility. The following examples are provided to further illustrate the present invention, but not to limit the present invention. (Example), (Preparation method of flaky alumina) Example 1 2 33.8 g of sulfate sulfate 18-hydrate (aluminum su -......... * lffate 18-hydrate), 1 14.5 g of anhydrous sodium hydroxide and 9 3 · 7 g of potassium phosphate were dissolved in 450 ml of deionized water by heating to about 75 ° C. Add 2.0 grams of a 34.4% titanium sulfate rhenium, -------- solution to the resulting solution. The obtained solution is called aqueous solution (a). 0.9 g of tertiary phosphoric acid is dissolved in 250 ml of deionized water. It is printed by the Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs (please read the precautions on the back before filling this page) _ Pin 12-hydrate and 107.9 g of carbon-sodium. The resulting solution is called ......——-...........-.............. It is an aqueous solution (b). The aqueous solutions (a) and (b) are simultaneously stirred at a fixed rate into 200 ml of deionized water. The addition process takes about 15 minutes. In this manner, the solute of the solution (a) is approximately equal to the solute in the solution (b). Continue stirring for another 15 minutes. The resulting solution was evaporated to dryness. Heat the resulting solid stubble _1 2 0 0 ° C for 5 hours'. Add water to the hot place ----·-_ This paper size applies to the Chinese National Standard (ciMS) A4 specification (; 210 乂 297 mm) 1-13-Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs A7 B7 5 2. Description of the invention (u) The treated product is used to dissolve free state sulfate. The insoluble solid was filtered off and 'washed with water' and finally dried. The desired flake alumina was thus obtained. The flake alumina thus obtained was examined with a dif fractom-etry. The diffraction pattern has only the peaks attributable to oxidation. Ming (corundum). Chemical analysis found that the flaky alumina contained 0.9% titanium dioxide. Observation with an optical microscope and an electron microscope revealed that the flaky aluminum oxide had a particle size of .3 to 16 and a thickness of about 0.2 and no crystal formation. When the flake alumina is stirred and dispersed in water, the flake alumina produces a smooth and streamlined result indicating good dispersing power. Example 2 1 1.1 g of aluminum sulfate 18-hydrate, 57.3 g of anhydrous sodium sulfate and 46.9 g of potassium sulfate were dissolved in 300 ml of deionized water by heating to 60 ° C or higher. In the water. 1.0 g of a 34.4% titanium rhenium sulfate solution was added to the resulting solution. The resulting solution is referred to as an aqueous solution (a). In 150 ml of deionized water, 0.45 g of sodium tertiary phosphate 12-hydrate and 54.0 g of sodium carbonate were dissolved. The resulting solution is called the aqueous solution (b). The aqueous solution (b) is stirred into the aqueous solution (a) which has been heated to about 60 ° C. Stirring was continued for another 15 minutes. The mixture of the two solutions is colloid. The resulting solution was evaporated to dryness and the resulting solid was heated at approximately 120 ° C for 5 hours. Water is added to the heat-treated product to the Chinese paper standard (CNS) A4 (210X297 mm) at this paper size. '~~~ -14-(Please read the precautions on the back before filling this page) 0.
tF 1, A7 B7 五、發明説明（12 ) 溶解自由態硫酸鹽。將不能溶解的固體過濾掉，用水清洗 ，最後乾燥。如此獲得了所需的片狀氧化鋁。 將如此獲得的片狀氧化鋁以X光衍射計撿查。繞射圖 型僅有可歸於氧化鋁（剛玉）的波峰。由化學分析發現片 狀氧化鋁包含0 . 9%二氧化鈦。由光學顯微鏡和電子 顯微鏡觀察，顯示片狀氧化鋁有4 - 2 1 的粒徑及約 0. 2 的厚度而且沒有結晶的形成。將片狀氧.化鋁攪 拌分散進水中時，片狀氧化鋁會產生表示分散力佳的平滑 流線型結果。 實施例3 將1 1 1 . 9克硫酸鋁18 -水合物，57 · 3克無 水硫酸鈉及4 6 . 9克硫酸鉀，藉由加熱到約6 0 °C的方 式溶解在3 0 0毫升去離子水裡。將3. . 0克34 . 4% .硫酸鈦醯溶液加入所得的溶液裡。所得的溶液係稱爲水溶 液（a )。 經濟部中央標準局員工消費合作社印製 (請先閲讀背面之注意事項再填寫本頁) 在150毫升的去離子水裡溶解◦.45克三級磷酸 鈉1 2 _水'合物和5 5 . 0克碳酸_。產生的溶液係稱爲 水溶液（b )。 將水溶液（b )攪拌加入已經加熱到約6 0 °C的水溶 液（a)。再繼續攪拌15分鐘。該兩種溶液的混合物係 爲膠體。將所產生的溶液蒸發到乾。將所產生的固體在大 約1 2 0 〇 °C加熱5小時。將水加入經熱處理過的產物以 溶解自由態硫酸鹽。將不能溶解的固體過濾掉，用水清洗 本紙張尺度適用中國國家標準（CNS ) Μ規格（210X297公釐） -15 - 經濟部中央標準局員工消費合作社印製 Α7 Β7 五、發明説明（13) ’最後乾燥。如此獲得了所需的片狀氧化銘。 將如此獲得的片狀氧化鋁以X光衍射計檢査。繞射圖 型僅有可歸於氧化鋁（剛玉）的波峰。由化學分析發現片 狀氧化鋁包含2 . 6 %二氧化鈦。由光學顯微鏡和電子顯 微鏡觀察’顯示片狀氧化銘有5 - 2 2 Am的粒徑及約 0.2#m的厚度而且沒有結晶的形成。將片狀氧化鋁攪 拌分散進水中時，片狀氧化鋁會產生表示分散力佳_的平滑 流線型結果。 實施例4 將111 . 9克硫酸鋁18 —水合物，57 . 3克無 水硫酸鈉及4 6 .9克硫酸鉀’藉由加熱到約6 〇°c的方 式溶解在300毫升去離子水裡。將3. 0克34 .4% 硫酸鈦醯溶液加入所得的溶液裡。所得的溶液係稱爲水溶 液 ( a ).。 在1 5 0毫升的去離子水裡溶解1 . 3 5克三級磷酸 鈉1 2 —水合物和5 4 · 0克碳酸鈉。產生的溶液係稱爲 水溶液（b )。 ' 將水溶液（b )攪拌加入已經加熱到約6 〇。(：的水溶 液（a )。再繼續攪拌1 5分鐘。該兩種溶液的混合物係 爲膠體。將所產生的溶液蒸發到乾。將所產生的固體在大 約1 2 0 0 °C加熱5小時。將水加入經熱處理過的產物以 溶解自由態硫酸鹽。將不能溶解的固體過濾掉，用水清洗 ，最後乾Μ。如此獲得了所需的片狀氧化鋁。 本紙張尺度適用中國國家標準（CNS ) Α4規格（210Χ：297公釐） -----------— (請先閲讀背面之注意事項再填寫本頁) 訂 -16 - A7 B7 五、發明説明（14 ) 將如此獲得的片狀氧化鋁以X光衍射計檢査》繞射圖 型僅有可歸於氧化鋁（剛玉）的波峰。由化學分析發現片 狀氧化鋁包含0.8%二氧化鈦。由光學顯微鏡和電子顯 微鏡觀察，顯示片狀氧化鋁有5 - 2 0 /zm的粒徑及約 0 . 的厚度而且沒有結晶的形成。將片狀氧化鋁攪 拌分散進水中時，片狀氧化鋁會產生表示分散力佳的平滑 流線型結果。 - 實施例5 將111 . 9克硫酸鋁18 —水合物，57 · 3克無 水硫酸鈉及4 6 · 9克硫酸鉀，藉由加熱到6 0 °C以上的 方式溶解在30 0毫升去離子水裡。將0 . 5克34 . 4 %硫酸鈦醯溶液加入所得的溶液裡。所得的溶液係稱爲水 溶液（a )。 在1.5 0毫升的去離子水裡溶解〇 · 4 5克三級磷酸 鈉1 2 -水合物和5 3 . 7克碳酸鈉。產生的溶液係稱爲 水溶液（b )。 經濟部中央標準局員工消費合作社印製 (請先閱讀背面之注意事項再填寫本頁) 將水溶液（b )攪拌加入已經i/卩熱到約6 〇 °c的水溶 液（a)。再繼續攪拌15分鐘》該兩種溶液的混合物係 爲膠體。將所產生的溶液蒸發到乾。將所產生的固體在大 約1 2 0 0 °C加熱5小時。將水加入經熱處理過的產物以 溶解自由態硫酸鹽。將不能溶解的固體過濾掉，用水清洗 ，最後乾燥。如此獲得了所需的片狀氧化鋁。 將如獲得的片狀氧化鋁以X光衍射計檢査。繞射圖 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -17 - A7 B7 五、發明説明（15 ) 型僅有可歸於氧化鋁（剛玉）的波峰。由化學分析發現片 狀氧化鋁包含0·4%二氧化鈦。由光學顯微鏡和電子顯 微鏡觀察，顯示片狀氧化鋁有4 - 1 8 #ιη的粒徑及約 0 . 的厚度而且沒有結晶的形成。將片狀氧化鉬攪 拌分散進水中時，片狀氧化銘會產生表示分散力佳的平滑 流線型結果。tF 1, A7 B7 V. Description of the invention (12) Dissolve free state sulfate. The insoluble solids were filtered off, washed with water, and finally dried. Thus, a desired flaky alumina was obtained. The flaky alumina thus obtained was checked with an X-ray diffractometer. The diffraction pattern has only peaks attributable to alumina (corundum). Chemical analysis revealed that the flaky alumina contained 0.9% titanium dioxide. Observation by an optical microscope and an electron microscope revealed that the flaky aluminum oxide had a particle size of 4-2 1 and a thickness of about 0.2 and no crystals were formed. When the flaky aluminum oxide is stirred and dispersed in water, the flaky aluminum oxide produces a smooth and streamlined result indicating good dispersing power. Example 3 1 1.1 g of aluminum sulfate 18-hydrate, 57.3 g of anhydrous sodium sulfate and 46.9 g of potassium sulfate were dissolved in 300 ml by heating to about 60 ° C. In deionized water. 3.0 grams of 34.4% titanium hafnium sulfate solution was added to the resulting solution. The resulting solution is referred to as an aqueous solution (a). Printed by the Consumers 'Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs (please read the precautions on the back before filling this page) Dissolved in 150 ml of deionized water. 45 g of sodium tertiary phosphate 1 2 _ water' compound and 5 5 0 g of carbonic acid. The resulting solution is called the aqueous solution (b). The aqueous solution (b) is stirred into the aqueous solution (a) which has been heated to about 60 ° C. Stirring was continued for another 15 minutes. The mixture of the two solutions is colloid. The resulting solution was evaporated to dryness. The resulting solid was heated at approximately 12 ° C. for 5 hours. Water was added to the heat-treated product to dissolve the free-state sulfate. Filter out insoluble solids, and wash the paper with water. This paper applies the Chinese National Standard (CNS) M specification (210X297 mm). -15-Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs. Finally dry. In this way, the desired plate-shaped oxide inscription was obtained. The flaky alumina thus obtained was examined with an X-ray diffractometer. The diffraction pattern has only peaks attributable to alumina (corundum). Chemical analysis revealed that the flaky aluminum oxide contained 2.6% titanium dioxide. Observation by an optical microscope and an electron microscope showed that the flaky oxide had a particle size of 5-2 2 Am and a thickness of about 0.2 #m, and no crystals were formed. When the flaky alumina is stirred and dispersed in water, the flaky alumina produces a smooth streamlined result indicating good dispersion. Example 4 111.9 g of aluminum sulfate 18-hydrate, 57.3 g of anhydrous sodium sulfate, and 46.9 g of potassium sulfate were dissolved in 300 ml of deionized water by heating to about 60 ° C. . 3.0 grams of a 34.4% titanium rhenium sulfate solution was added to the resulting solution. The resulting solution is called an aqueous solution (a). In 150 ml of deionized water, 1.3 g of sodium tertiary phosphate 12-hydrate and 54.0 g of sodium carbonate were dissolved. The resulting solution is called the aqueous solution (b). 'The aqueous solution (b) is added with stirring to about 60. (: Aqueous solution (a). Stirring is continued for another 15 minutes. The mixture of the two solutions is a colloid. The resulting solution is evaporated to dryness. The resulting solid is heated at approximately 12 0 ° C for 5 hours Water is added to the heat-treated product to dissolve the free-state sulfate. The insoluble solids are filtered off, washed with water, and finally dried. In this way, the required flake alumina is obtained. This paper size applies Chinese national standards ( CNS) A4 specification (210 ×: 297 mm) ------------- (Please read the notes on the back before filling out this page) Order -16-A7 B7 V. Description of the invention (14) will The flaky alumina thus obtained was examined by an X-ray diffractometer. The diffraction pattern had only the peaks attributable to alumina (corundum). It was found by chemical analysis that the flaky alumina contained 0.8% titanium dioxide. Observed by an optical microscope and an electron microscope It shows that the flaky alumina has a particle diameter of 5-2 0 / zm and a thickness of about 0. There is no crystal formation. When the flaky alumina is stirred and dispersed in water, the flaky alumina will produce a good dispersion power. Smooth Streamlined Results-Real Example 5 111.9 g of aluminum sulfate 18-hydrate, 57.3 g of anhydrous sodium sulfate and 4 6 · 9 g of potassium sulfate were dissolved in 300 ml of deionized water by heating above 60 ° C. 0.5 g of a 34.4% titanium rhenium sulfate solution was added to the resulting solution. The resulting solution was referred to as the aqueous solution (a). 0.45 g of sodium tertiary phosphate was dissolved in 1.50 ml of deionized water. 1 2-Hydrate and 53.7 grams of sodium carbonate. The resulting solution is called aqueous solution (b). Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs (please read the precautions on the back before filling this page). (B) Add the aqueous solution (a) which has been heated to about 60 ° C with stirring. Continue stirring for 15 minutes. The mixture of the two solutions is a colloid. The resulting solution is evaporated to dryness. The resulting solution The solid was heated at approximately 12 ° C for 5 hours. Water was added to the heat-treated product to dissolve the free-state sulfate. The insoluble solid was filtered off, washed with water, and finally dried. The desired tablet was thus obtained Alumina was obtained in the form of flakes as obtained Check. Diffraction chart This paper size is in accordance with Chinese National Standard (CNS) A4 specification (210X297 mm) -17-A7 B7 V. Description of invention (15) Only the peaks attributable to alumina (corundum). Chemical analysis The flaky alumina was found to contain 0.4% titanium dioxide. Observation by optical and electron microscopy showed that the flaky alumina had a particle size of 4-1 8 # ιη and a thickness of about 0. When molybdenum oxide is dispersed in water with stirring, the flaky oxide will produce a smooth and streamlined result indicating good dispersion.
實施例R 將2 2 3 . 8克硫酸鋁1 8 —水合物加熱溶解在 5 0 0毫升去離子水裡。在2 5 0毫升的去離子水裡溶解 106 . 8克碳酸鈉。將兩種水溶液同時地以固定速率攪 拌加入2 0 0毫升去離子水，加入過程約經1 5分鐘，在 如此方式裡第一溶液的溶質大約等於第二溶液裡的溶質。 再繼續攪拌1 5分鐘。獲得一分散液。將分散液過濾掉並 將固體用水清洗。.因而獲得了水合氧化鋁。 經濟部中央標準局員工消費合作社印製 (請先聞讀背面之注意事項再填寫本頁) 在5 0 0毫升的去離子水裡加熱溶解5 3 . 7克碳酸 鈉和4 6 . 9克硫酸鉀。將上述水合氧化鋁然後將2 . 0 克3 4 . 4%硫酸鈦醯溶液和〇 _ 9克三級磷酸鈉12 — 水合物加入所得的溶液裡。將所得的溶液攪拌1 〇分鐘〃 將所產生的溶液蒸發到乾。將所產生的固體在大約 1 2 0 0 X：加熱5小時。將水加入經熱處理過的產物以溶 解自由態硫酸鹽。將不能溶解的固體過濾掉，用水清洗， 最後乾燥。如此獲得了所需的片狀氧化鋁。 將如&獲得的片狀氧化鋁以X光衍射計檢查。繞射圖 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐) " 18 經濟部中央標準局貝工消費合作社印製 A7 B7 五、發明説明（16 ) 型僅有可歸於氧化鋁（剛玉）的波峰。由化學分析發現片 狀氧化鋁包含0 .· 9 %二氧化鈦》由光學顯微鏡和電子顯 微鏡觀察，顯示片狀氧化鋁有3 - 1 6mm的粒徑及約 0.2mm的厚度而且沒有結晶的形成。將片狀氧化鋁攪 拌分散進水中時，片狀氧化鋁會產生表示分散力佳的平滑 流線型結果。 比較實施例1 粉末混合物係藉由將111.9克硫酸鋁18-水合 物，7 1 . 6克無水硫酸鈉及5 3 . 4克硫酸鉀以機械磨 細3 0分鐘而得。將粉末混合物在1 〇 〇 〇 °C加熱1小時 。將水加入經熱處理過的產物以溶解自由態硫酸鹽。將不 能溶解的固體過濾掉，用水清洗，最後乾燥。如此獲得了 氧化tg粉末。 將如此獲得的氧化鋁粉末以X光衍射計檢查。繞射圖 型僅有可歸於氧化鋁（剛玉）的波峰。由光學顯微鏡和電 子顯微鏡觀察，顯示氧化鋁有小於5 的粒徑及約 0 . 3^111的厚度，外觀比小。將氧化鋁粉末攪拌分散進 水中時，氧化鋁粉末不會產生任何平滑流線型結果。除此 之外，由光學顯微鏡和電子顯微鏡明顯觀察到結晶的形成 和聚集》 比較實施例2 粉末）昆合物係藉由將1 1 1 . 9克硫酸鋁1 8 -水合 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） (請先閲讀背面之注意事項再填寫本頁) 、?Example R 23.8 g of aluminum sulfate 18-hydrate was dissolved by heating in 500 ml of deionized water. Dissolve 106.8 g of sodium carbonate in 250 ml of deionized water. 200 ml of deionized water were added to the two aqueous solutions simultaneously at a fixed rate. The addition process took about 15 minutes. In this way, the solute in the first solution was approximately equal to the solute in the second solution. Stirring was continued for another 15 minutes. A dispersion was obtained. The dispersion was filtered off and the solid was washed with water. Thus, hydrated alumina was obtained. Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs (please read the precautions on the back before filling this page). Heat and dissolve 53.7 g of sodium carbonate and 46.9g of sulfuric acid in 500ml of deionized water. Potassium. The above-mentioned hydrated alumina was then added with 2.0 g of a 34.4% titanium rhenium sulfate solution and 0-9 g of sodium tertiary phosphate 12-hydrate into the resulting solution. The resulting solution was stirred for 10 minutes. The resulting solution was evaporated to dryness. The resulting solid was heated at approximately 12 0 X: for 5 hours. Water was added to the heat-treated product to dissolve the free-state sulfate. The insoluble solids were filtered off, washed with water, and finally dried. Thus, a desired flaky alumina was obtained. The flaky alumina obtained as & was examined with an X-ray diffractometer. Diffraction map This paper size applies Chinese National Standard (CNS) A4 specification (210X297mm) " 18 Printed by A7 B7, Shellfish Consumer Cooperative, Central Bureau of Standards, Ministry of Economic Affairs 5. Description of invention (16) type can only be attributed to alumina (Corundum) crest. The chemical analysis revealed that the flaky alumina contained 0.9% titanium dioxide. Observation by optical microscope and electron microscope showed that the flaky alumina had a particle diameter of 3-16 mm and a thickness of about 0.2 mm and no crystals were formed. When the flaky alumina is stirred and dispersed in water, the flaky alumina produces a smooth and streamlined result indicating good dispersing power. Comparative Example 1 The powder mixture was obtained by mechanically pulverizing 111.9 g of aluminum sulfate 18-hydrate, 7 1.6 g of anhydrous sodium sulfate and 5 3.4 g of potassium sulfate for 30 minutes. The powder mixture was heated at 1000 ° C for 1 hour. Water was added to the heat-treated product to dissolve the free-state sulfate. The insoluble solids were filtered off, washed with water and finally dried. Thus, an oxidized tg powder was obtained. The alumina powder thus obtained was examined with an X-ray diffractometer. The diffraction pattern has only peaks attributable to alumina (corundum). Observation by an optical microscope and an electron microscope showed that the alumina had a particle size of less than 5 and a thickness of about 0.31111, and the appearance ratio was small. When the alumina powder is dispersed into the water under stirring, the alumina powder does not produce any smooth streamlined results. In addition, the formation and aggregation of crystals were clearly observed by the light microscope and the electron microscope. Comparative Example 2 Powder) The compound was prepared by hydration of 1 1 .9 g of aluminum sulfate 1 8-hydrated paper scale applicable to China National Standard (CNS) A4 specification (210X297 mm) (Please read the precautions on the back before filling this page),?
-19 - 經濟部中央標準局員工消費合作社印製 A7 B7 _ 五、發明説明（17 ) 物，5 7 . 3克無水硫酸鈉，4 6 . 9克硫酸鉀，五水過 硫酸鈦(titanium oxysulfate pentahydrate)， 0 . 4 5克三級磷酸鈉1 2 —水合物及5 3 . 4克碳酸鈉 以機械磨細3 0分鐘而得。將粉末混合物在1 2 0 0 °C加 熱5小時。將水加入經熱處理過的產物以溶解自由態硫酸 鹽。將不能溶解的固體過濾掉，用水清洗，最後乾燥。如 此獲得了氧化鋁粉末。 . 將如此獲得的氧化鋁粉末以X光衍射.計檢查。繞射圖 型僅有可歸於氧化鋁（剛玉）的波峰。由光學顯微鏡和電 子顯微鏡觀察，顯示氧化鋁在直徑及厚度方面波動很大並 含有許多的聚集體（aggragates)。除此之外，其分散力 很差。 . 比較實施例3 將111 . 9克硫酸鋁18 —水合物，5 7. 3克無 水硫酸鈉及4 6 . 9克硫酸鉀，藉由加熱到，6 0 °C以上的 方式溶解在300 毫升去離子水裡。所得的溶液係稱爲 水溶液（a / )。 ’ 在1 5 0.毫升的去離子水裡溶解5 3 . 4克碳酸鈉。 產生的溶液係稱爲水溶液（b > )。 將水溶液（b > )攪拌加入保持約6 〇 °C的水溶液（ a >)裡。再繼續攪拌1 5分鐘。該兩種溶液的混合物係 爲膠體。將所產生的膠體蒸發到乾，並將經乾燥的固體在 大約1 2 _0 〇 °C加熱5小時。將水加入經熱處理過的產物 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） (請先閲讀背面之注意事項再填寫本頁) Φ. tr -20 - 經濟部中央標準局員工消費合作社印製 A7 B7 五、發明説明（18 ) 以溶解自由態硫酸鹽。將不能溶解的固體過濾掉，用水清 洗，最後乾燥。如此獲得了氧化鋁粉末。 將如此獲得的氧化鋁以X光衍射計檢査。繞射圖型僅 有可歸於氧化鋁（剛玉）的波峰。由化學分析發現片狀氧 化鋁包含0.4%二氧化鈦。由光學顯微鏡和電子顯微 鏡觀察，顯示片狀氧化鋁係爲粒徑5 — 3 0 及厚約 0 .1 Mm的板狀（platy)粒子而且含有結晶的形成和 聚集。將氧化鋁粉末攪拌分散進水中時，因爲分散力差所 以氧化鋁粉末不會產生任何的流線型結果。 比鉸實施例4 將111 . 9克硫酸鋁18 —水合物，57 . 3克無 水硫酸鈉及4 6 . 9克硫酸鉀，藉由加熱到6 0 °C以上的 方式溶解在3 0 0毫升去離子水裡。所得的溶液係稱爲水 溶液（a/ )。 在1 5 0毫升的去離子水裡溶解0 · 4 5克三級磷酸 鈉1 2 _水合物及5 3 . 4克碳酸鈉。產生的溶液係稱爲 水溶液（b > )。 ’ 將水溶液（b / )攪拌加入保持約6 0 °C的水溶液（ a >)裡。再繼續攪拌15 分鐘。該兩種溶液的混合物 係爲膠體。將所產生的膠體蒸發到乾，並將經乾燥的固體 在大約1 2 0 0 °C加熱5小時。將水加入經熱處理過的產 物以溶解自由態硫酸鹽。將不能溶解的固體過濾掉，用水 清洗，最备乾燥。如此獲得了氧化鋁粉末。 本紙張尺度適用中國國家標準（CNS〉A4規格（210 X 297公釐） (請先閱讀背面之注意事項再填寫本頁) •Φ. 訂 -21 - A7 __._________B7 _._ 五、發明説明（I9〉 將如此獲得的氧化鋁以X光衍射計檢査。繞射圖型僅 有可歸於氧化鋁（剛玉）的波峰。由化學分析發現氧化鋁 包含0 · 9%二氧化鈦。由光學顯微鏡和電子顯微鏡觀察 ，顯示氧化鋁係具有5 — 2 0μιη的粒徑及約1 . Oem 的厚度。該厚度遠大於加入磷系化合物而製得之氧化鋁的 厚度。 比較實施例5 將111 . 9克硫酸鋁18 —水合物，57 · 3克無 水硫酸鈉及4 6 . 9竞硫酸鉀，藉由加熱到6 0 °C以上的 方式溶解在3 0 〇毫升去離子水裡。所得的溶液係稱爲水 溶液（a 一）。 在1 5 0毫升的去離子水裡溶解〇 . 4 5克三級磷酸 '鈉1 2 —水合物及5 3 · 4克碳酸鈉。產生的溶液係稱爲 水溶液（b / )。 經濟部中央標準局員工消費合作社印製 .(請先閲讀背面之注意事項再填寫本頁) 將水溶液（b / )攪拌加入保持約6 0 °C的水溶液（ a /)裡。再繼續攪拌1 5分鐘。該兩種溶液的混合物係 爲膠體。將所產生的膠體蒸發到乾‘，並將經乾燥的固體在 大約1 2 0 0 °C加熱5小時。將水加入經熱處理過的產物 以溶解自由態硫酸鹽。將不能溶解的固體過濾掉，用水清 洗，最後乾燥。如此獲得了氧化鋁粉末。’ 將如此獲得的氧化鋁以X光衍射計檢查。繞射圖型僅 有可歸於氧化鋁（剛玉）的波峰。由化學分析發現片狀氧 化鋁包含ΐ.4%二氧化鈦。由光學顯微鏡和電子顯微鏡 本紙張尺度適用中國國家標隼（CNS ) Α4規格（210'乂297公釐） ' -22 - 經濟部中央標準局員工消費合作社印裝 A7 B7 五、發明説明（2〇) 觀察’顯τκ片狀氧化銘係爲5 - 2 0 ；tz.rn的粒徑及約 0 . 2/zm的厚度並且明顯地有結晶的形成和聚集。將氧 化錫粉末攪拌分散進水中時，因爲分散力差所以氧化鋁粉 末不會產生任何的流線型結果。 比較實施例 將111 . 9克硫酸鋁18 -水合物，57 ._3克無 水硫酸鈉及4 6 · 9克硫酸鉀，藉由加熱到6 0 °C以上的 方式溶解在300毫升去離子水裡。將2.25克 3 4 . 4 %硫酸鈦醯溶液加入所得的溶液。所得的溶液係 稱爲水溶液（a > )。 在1 5 0毫升的去離子水裡溶解4 . 5克三級磷酸鈉 1 2 —水合物及5 3 . 7克碳酸鈉。產生的溶液係稱爲水 溶液（b —)。 將水溶液（b V )攪拌加入保持約6 0 °C的水溶液（ a / )裡。再繼續攪拌1 5 分鐘》該兩種溶液的混合物 係爲膠體。將所產生的膠體蒸發到乾，並將經乾燥的固體 在大約1 2 0 〇°C加熱5小時。將永加入經熱處理過的產 物以溶解自由態硫酸鹽。將不能溶解的固體過濾掉，用水 清洗’最後乾燥。如此獲得了氧化鋁粉末。 由化學分析發現因而獲得的氧化鋁包含4 . 5 %二氧 化鈦。由光學顯微鏡和電子顯微鏡觀察，顯示氧化鋁沒有 包含任何的片狀粒子。 本紙張尺度適用中國'國家標準（CNS ) A4規格（210X297公釐） (請先閲讀背面之注意事項再填寫本頁) -- --訂— -23 - ·Α7 _Β7 _ 五、發明説明（21) 〔表係顯示製備的條件〕 表1顯示實施例1到6及比較實施例1到6製備方法 件 條 的 (請先閣讀背面之注意事項再填寫本頁) 、w 經濟部中央標準局員工消費合作社印製 本紙張尺度適用中國國家標準_ ( CNS ) A4規格（210 X 297公釐） -24 --19-A7 B7 printed by the Consumer Cooperatives of the Central Bureau of Standards of the Ministry of Economic Affairs _ V. Description of the Invention (17), 57.3 grams of anhydrous sodium sulfate, 46.9 grams of potassium sulfate, titanium oxysulfate pentahydrate pentahydrate), 0.45 grams of tertiary sodium phosphate 12-hydrate and 5 3.4 grams of sodium carbonate were obtained by mechanically pulverizing for 30 minutes. The powder mixture was heated at 12 0 ° C for 5 hours. Water was added to the heat-treated product to dissolve the free-state sulfate. The insoluble solids were filtered off, washed with water, and finally dried. Thus, alumina powder was obtained. The alumina powder thus obtained was examined with an X-ray diffraction meter. The diffraction pattern has only peaks attributable to alumina (corundum). Observation by optical microscope and electron microscope showed that alumina fluctuates greatly in diameter and thickness and contains many aggragates. In addition, its dispersive power is poor. Comparative Example 3 111.9 g of aluminum sulfate 18-hydrate, 57.3 g of anhydrous sodium sulfate and 46.9 g of potassium sulfate were dissolved in 300 ml by heating to 60 ° C or more. In deionized water. The resulting solution is called an aqueous solution (a /). ′ Dissolve 5 3.4 g of sodium carbonate in 15.0 ml of deionized water. The resulting solution is called an aqueous solution (b >). The aqueous solution (b >) was stirred into the aqueous solution (a >) maintained at about 60 ° C. Stirring was continued for another 15 minutes. The mixture of the two solutions is colloid. The resulting colloid was evaporated to dryness, and the dried solid was heated at approximately 12 ° C. for 5 hours. Water is added to the heat-treated product. The paper size is in accordance with Chinese National Standard (CNS) A4 (210X297 mm) (please read the precautions on the back before filling this page) Φ. Tr -20-Staff of the Central Bureau of Standards, Ministry of Economic Affairs Printed by Consumer Cooperatives A7 B7 V. Description of Invention (18) To dissolve free-state sulfate. The insoluble solids were filtered off, washed with water and finally dried. Thus, alumina powder was obtained. The alumina thus obtained was examined with an X-ray diffractometer. The diffraction pattern has only the peaks attributable to alumina (corundum). Chemical analysis revealed that the flaky aluminum oxide contained 0.4% titanium dioxide. Observation by an optical microscope and an electron microscope revealed that the flaky aluminum oxide was platy particles having a particle diameter of 5 to 30 and a thickness of about 0.1 Mm, and contained the formation and aggregation of crystals. When alumina powder is dispersed in water with stirring, the alumina powder does not produce any streamlined results because of poor dispersion power. Specific Example 4 Dissolved 111.9 g of aluminum sulfate 18-hydrate, 57.3 g of anhydrous sodium sulfate and 46.9 g of potassium sulfate in 300 ml by heating to 60 ° C or higher. In deionized water. The resulting solution is called an aqueous solution (a /). In 150 ml of deionized water, 0.45 g of sodium tertiary phosphate 12 2 hydrate and 5 3.4 g of sodium carbonate were dissolved. The resulting solution is called an aqueous solution (b >). ’The aqueous solution (b /) is stirred into the aqueous solution (a >) maintained at about 60 ° C. Continue stirring for another 15 minutes. The mixture of the two solutions is colloid. The resulting colloid was evaporated to dryness and the dried solid was heated at approximately 12 0 ° C for 5 hours. Water is added to the heat-treated product to dissolve the free-state sulfate. Filter off insoluble solids, wash with water, and dry the most. Thus, alumina powder was obtained. This paper size applies to Chinese national standards (CNS> A4 size (210 X 297 mm) (Please read the notes on the back before filling out this page) • Φ. Order -21-A7 __._________ B7 _._ V. Description of the invention (I9> The alumina thus obtained was examined with an X-ray diffractometer. The diffraction pattern had only the peaks attributable to alumina (corundum). Chemical analysis revealed that alumina contained 0.9% titanium dioxide. Optical microscope and electron Microscopic observation showed that the alumina system has a particle size of 5-20 μm and a thickness of about 1.0 Oem. This thickness is much larger than the thickness of alumina prepared by adding a phosphorus-based compound. Comparative Example 5 111. 9 grams of sulfuric acid Aluminum 18-hydrate, 57.3 grams of anhydrous sodium sulfate and 46.9% potassium sulfate were dissolved in 300 ml of deionized water by heating above 60 ° C. The resulting solution is called Aqueous solution (a a). Dissolve 0.45 g of tertiary phosphate 'sodium 12-hydrate and 5 3.4 g of sodium carbonate in 150 ml of deionized water. The resulting solution is called an aqueous solution (b /). Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs (Please read the precautions on the back before filling this page) Stir the aqueous solution (b /) into the aqueous solution (a /) maintained at about 60 ° C. Continue stirring for 15 minutes. The mixture of the two solutions is Is a colloid. The resulting colloid is evaporated to dryness, and the dried solid is heated at approximately 12 ° C. for 5 hours. Water is added to the heat-treated product to dissolve the free-state sulfate. The insoluble The solid was filtered off, washed with water, and finally dried. The alumina powder was thus obtained. 'The alumina thus obtained was examined by an X-ray diffractometer. The diffraction pattern had only the peaks attributable to alumina (corundum). By chemical analysis It was found that flaky aluminum oxide contained ΐ.4% titanium dioxide. The paper size was applied to the Chinese National Standard 隼 (CNS) A4 specification (210 '乂 297 mm) by optical microscope and electron microscope' -22-Consumption by employees of the Central Standards Bureau of the Ministry of Economic Affairs Cooperative printed A7 B7 V. Description of the invention (20) Observe that the 'significant τκ flake oxidation inscription is 5-2 0; the particle size of tz.rn and the thickness of about 0.2 / zm and obvious crystal formation And aggregate. Will tin oxide When the powder is stirred and dispersed in water, the alumina powder does not produce any streamlined results because of the poor dispersing power. In the comparative example, 111.9 g of aluminum sulfate 18-hydrate, 57 .3 g of anhydrous sodium sulfate and 4 6 · 9 G of potassium sulfate was dissolved in 300 ml of deionized water by heating to a temperature above 60 ° C. 2.25 g of a 3.4% titanium hafnium sulfate solution was added to the resulting solution. The resulting solution was referred to as an aqueous solution (a >). In 150 ml of deionized water, 4.5 g of sodium tertiary phosphate 12-hydrate and 53.7 g of sodium carbonate were dissolved. The resulting solution is called an aqueous solution (b —). The aqueous solution (b V) was stirred into the aqueous solution (a /) maintained at about 60 ° C. Continue to stir for another 15 minutes. The mixture of the two solutions is a colloid. The resulting colloid was evaporated to dryness, and the dried solid was heated at approximately 12 ° C for 5 hours. The heat-treated product is added to dissolve the free-state sulfate. The insoluble solid was filtered off, washed with water 'and finally dried. Thus, alumina powder was obtained. Chemical analysis revealed that the alumina thus obtained contained 4.5% titanium dioxide. Observation by an optical microscope and an electron microscope revealed that the alumina did not contain any flaky particles. This paper size applies to China's National Standard (CNS) A4 specification (210X297 mm) (Please read the precautions on the back before filling out this page)--Order--23-· Α7 _Β7 _ V. Description of the invention (21 ) [Table shows preparation conditions] Table 1 shows the preparation methods of Examples 1 to 6 and Comparative Examples 1 to 6 (please read the precautions on the back before filling this page), w Central Standards Bureau, Ministry of Economic Affairs The paper size printed by the employee consumer cooperative is applicable to Chinese national standard _ (CNS) A4 specification (210 X 297 mm) -24-
7 7 A B 五、發明説明（22 ) 表丄 經濟部中央標準局員工消費合作社印製 實施例 (比較實施例） 製備方法的條件 方法 礦化劑/鋁鹽 (莫耳比） Ti〇2/Al2〇3 (韋暈%) P2O5/AI2O3 (韋暈%) 反應種類 1 同時加入 4.0 1.0 0.5 濕法 2 簡單加入 4.0 1.0 0.5 濕法 3 簡單加入 4.0 3.0 0.5 濕法 4 簡單加入 4.0 1.0 1.5 濕法 5 簡單加入 4.0 0.5 0.5 濕法 6 水解 2.0 1.0 0.5 濕法 (1) - 3.0 0 0 乾法 (2) - 4.0 0.6 , 0.5 乾法 (3) 加入 4.0 0 0 濕法 (4) 加入 4.0 1.0 0 濕法 (5) 加入 4.0 0 0.5 濕法 (6) 加入 4.0 0.5 2.5 濕法 本紙張尺度適用中國國家標準（CNS ) A4規格（2·1 OX297公釐） (請先閲讀背面之注意事項再填寫本頁) 言 /πτ\」 Γ -25 - A7 B7 五、發明説明（23) •〔形狀與分散力〕 表2係顯示由實施例1 到6及比較實施例1到6製 力 散 分 與 狀 形 的 品 樣 鋁 化 氧 狀 片 之 備 (請先閲讀背面之注意事項再填寫本頁)7 7 AB V. Description of the invention (22) Table 印 Example printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs (Comparative Example) Conditions of preparation method Method Mineralizer / Aluminum salt (Molar ratio) Ti〇2 / Al2 〇3 (Wei hao%) P2O5 / AI2O3 (Wei hao%) Reaction type 1 Simultaneous addition of 4.0 1.0 0.5 Wet method 2 Simple addition 4.0 1.0 0.5 Wet method 3 Simple addition 4.0 3.0 0.5 Wet method 4 Simple addition 4.0 1.0 1.5 Wet method 5 Simply add 4.0 0.5 0.5 wet method 6 hydrolysis 2.0 1.0 0.5 wet method (1)-3.0 0 0 dry method (2)-4.0 0.6, 0.5 dry method (3) add 4.0 0 0 wet method (4) add 4.0 1.0 0 wet Method (5) Add 4.0 0 0.5 Wet method (6) Add 4.0 0.5 2.5 Wet method The paper size applies the Chinese National Standard (CNS) A4 specification (2 · 1 OX297 mm) (Please read the precautions on the back before filling in this (Page) // πτ \ ″ Γ -25-A7 B7 V. Description of the invention (23) • [Shape and Dispersion Force] Table 2 shows the force dispersion and state from Examples 1 to 6 and Comparative Examples 1 to 6. Preparation of Shaped Aluminized Oxide Sheets (Please read the precautions on the back before filling this page)
———iT __A ^___ 經濟部中央標準局員工消費合作社印製 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -26 - A7 B7 經濟部中央標準局員工消費合作社印製 五、發明説明（24) 表2 實施例 (比較實施例） 粒徑 m) 厚度 (# m) 外觀比 結晶的形 成與聚集 流線型結果的 期間（秒π 1 3-16 0.2 45 沒有 85 2 4-21 0.2 60 沒有 80 3 5-22 0.2 65 沒有 71 4 5-20 0.2 60 沒有 75 5 4-18 0.2 55 沒有 70 ' 6 3-16 0. 2 50 沒有 77 (1) 0.3 X 有 0 (2) X X X 有 16 (3) 5-30 1.0 X 有 21 (4) 5-20 1.0 13 有 23 (5) 5-20 0. 2 X 有 25 (6) <4 X X 有 0 -----------Φ.--^----1T------IV (請先閲讀背面之注意事項再填寫本頁) -27 - A7 __B7 ___ 五、發明説明（25) 〔製造具有珍珠光澤之顏料] 實施例7 將實施例1所得的片狀氧化鋁（2 0克）懸浮在 4 0 0毫升的去離子水裡。將含有1 2 5克丁 i C 14的 溶液以每升0 . 6毫升/分鐘的速度加入所得的懸浮液（ 保持.在約6 5 °C )。同時將1 〇 % N a ◦ Η溶液加入以保 持pH值爲2 . 5。當所得的產物呈現銀色時，便-停止將 Ti C 14加入。將懸浮著的固體過濾掉，用水清洗，最 後乾燥。最後，將經乾燥過的固體在8 5 0 °C煆燒成極白 且具有珍珠光澤之顏料。 實施例8 將實施例2所得的片狀氧化鋁（2 0克）懸浮在 4 0 0毫升的去離子水裡。將1 〇%N a OH溶液加入所 得的懸浮液（保持在約7 5 °C)以調節pH值爲9 . 0 » 1 0分鐘之後，將4 0毫升含有3 6克S.n C 1 4的溶液 以每升0 . 6毫升/分鐘的速度加入。同時將1 〇% 經濟部中央標準局頁工消費合作社印裝 (請先閱讀背面之注意事項再填寫本頁) N a Ο Η溶液加入以保持pH值爲1.9 » 15分鐘之後， 將含有1 2 5克T i C 14的溶液以每升〇 . 6毫升/分 鐘的速度加入。當所得的產物呈現銀色時，便停止將 T i C 1 4加入》將懸浮著的固體過濾掉，用水清洗，最 後乾燥。最後，將經乾燥過的固體在8 5 0。(：煆燒成極白 且具有珍珠光澤之顏料。以X光衍射計檢査的結果顯示， 該顏料裡_的所有二氧化鈦都是金紅石（rutiie)類型。 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） ' ~ 28 - 經濟部中央標準局員工消費合作社印製· A7 B7 五、發明説明（26 ) 實施例9 將實施例5所得的片狀氧化鋁（2 0克）懸'浮在 4 0 0毫升的去離子水裡。將2 0 %硝酸鐵9 ~~水合物溶 液以1 . 0毫升/分鐘的速度加入所得的懸浮液（保持在 約75°C)。同時將10%Na〇H溶液加入以保持PH 值爲3. · 0。將懸浮著的固體過濾掉，用水清洗，_最後乾 燥。最後，將經乾燥過的固體在8 5 0 °C煆燒成微紅棕色 •珍珠光澤具有金色干涉顏色的顔料。 下列實施例係舉例說明具有珍珠光澤之顏料在油漆， 塑膠組合物及印刷油墨上的應用。. 實施例1 0 將汽車用的底漆（base coat paint)根據下列配方 製備。 <底漆系統 > 丙烯系-三聚氰胺樹脂系統 "Acrydic 47712"* 70 pbw "Superbekkamine G821-60"** 30 pb w 甲苯 30 pbw 醋酸乙酯 50 pbw η —丁醇 110 pbw Solvesso #150 40 pbw 丹尼朋'(Dai n ippon)油墨與化學品公司的丙嫌系樹脂 本紙張又度適用中國國家標準（CNS ) A4規格（210X297公釐） (請先閎讀背面之注意事項异填寫本頁) ▲ 訂 -29 - A7 B7 五、發明説明（27) ** 丹尼朋油墨與化學品公司的三聚氰胺樹脂 上述丙烯系一三聚氰胺樹脂係統（1 0 0 P bw)係 與實施例1到9獲得的2 0 p b w片狀氧化鋁或具有珍珠 光澤的顏料合併。用稀釋劑將所得的化合物稀釋，使得所 產生的油漆具有油漆用的充分稠度。（12 — 15秒，F-ord杯#4)。將該油漆藉由噴塗方式塗到基材上-以形成 底漆層（base coat layer)。 將該底漆層進一步地用無色頂層清澈的塗漆再塗上一 層，該塗漆係根據下列配方而製得： (請先閲讀背面之注意事項再填寫本頁) 言. 〈頂層清澈的塗漆' > "Acrydic 44-179" 14 pbw "Superbekkaraine L117-60" 6 pbw 甲苯 4 pbw MIBK 4 pbw 丁基賽璐素 3 pbw 經濟部中央標準局員工消費合作社印製 將頂層塗層曝露在4 0°C的空氣中3 0分鐘，然後在 1 3 5 °C固化3 0分鐘。 實施例1 1 汽車用的底漆係根據下列配方而製得： 本紙張尺度適用中國國家標準（CNS ) Α4規格（210X29*7公釐） 五、發明説明（28) <底漆系統> "Dynapol H-700"*l 25. 2克 "Mapranal MF-650"*2 2. 7克 "乙醯基丁酸纖維素酯5 3 1 · 1" $ 3 15· 5克 "Irgarol TZ-6" 1.1克 醋酸.乙酯 . 23· 3克 二甲苯 11. 6 克- Solvesso 150 " 11· 6 克 C. I .顔料紅色1 77 4. 5克 實施例1到9獲得的片狀氧化鋁或 4. 5克 (請先閲讀背面之注意事項I填寫本頁) 經濟部中央標準局員工消費合作社印製 具有珍珠光澤的顏料 * 1 So lvesso 1 5 0裡聚酯樹脂的6 0 %溶液，得自 Dynan i t Nobe 1 0 *2 丁醇裡三聚氰胺的5 5 %溶液，得自Hoechst。 * 3 二甲苯與醋酸丁酯1 : 2混合物裡的2 5%溶液， 得自Eastman化學國際公司。 *4 以礦物油與羧酸鹽爲基礎的觸媒，得自Giba— Geigy——— iT __A ^ ___ Printed by the Central Consumers ’Cooperative of the Ministry of Economic Affairs. The paper is printed in accordance with the Chinese National Standard (CNS) A4 (210X297 mm). -26-A7 B7 Printed by the Central Consumers’ Cooperative of the Ministry of Economic Affairs. Description of the invention (24) Table 2 Examples (comparative examples) Particle size m) Thickness (# m) Appearance ratio Crystal formation and aggregation streamlined result period (sec π 1 3-16 0.2 45 No 85 2 4-21 0.2 60 No 80 3 5-22 0.2 65 No 71 4 5-20 0.2 60 No 75 5 4-18 0.2 55 No 70 '6 3-16 0. 2 50 No 77 (1) 0.3 X Yes 0 (2) XXX Yes 16 (3) 5-30 1.0 X Yes 21 (4) 5-20 1.0 13 Yes 23 (5) 5-20 0. 2 X Yes 25 (6) < 4 XX Yes 0 ------- ---- Φ .-- ^ ---- 1T ------ IV (Please read the notes on the back before filling out this page) -27-A7 __B7 ___ V. Description of the invention (25) [Manufacture with Pearlescent Pigment] Example 7 The flake alumina (20 g) obtained in Example 1 was suspended in 400 ml of deionized water. A solution containing 1.25 g of butyl i C 14 was added per liter. Added at a rate of 0.6 ml / min Suspension (maintained at about 65 ° C). At the same time, a 10% Na Η solution was added to keep the pH at 2.5. When the resulting product appeared silvery, the addition of Ti C 14 was stopped. The suspended solid was filtered off, washed with water, and finally dried. Finally, the dried solid was calcined at 850 ° C into an extremely white pigment with pearl luster. Example 8 The flakes obtained in Example 2 were obtained. Alumina (20 g) was suspended in 400 ml of deionized water. A 10% NaOH solution was added to the resulting suspension (maintained at about 75 ° C) to adjust the pH to 9.0. »After 10 minutes, add 40 ml of a solution containing 36 g of Sn C 1 4 at a rate of 0.6 ml / min per liter. At the same time, print 10% of the pager consumer cooperative of the Central Standards Bureau of the Ministry of Economic Affairs ( Please read the notes on the back before filling this page) N a 〇 Ο solution added to maintain the pH value 1.9 »After 15 minutes, the solution containing 125 grams of T i C 14 at 0.6 ml / min When the obtained product appears silver, stop adding T i C 1 4 "to filter the suspended solids, use Wash, and finally dried. Finally, the dried solid was placed at 850. (: Sintered into an extremely white pigment with pearl luster. The results of inspection by X-ray diffractometer show that all titanium dioxide in the pigment is of the rutile type. This paper size applies to the Chinese National Standard (CNS) A4 specifications (210X 297 mm) '~ 28-Printed by the Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs · A7 B7 V. Description of the invention (26) Example 9 The flake alumina obtained in Example 5 (20 g) Suspended in 400 ml of deionized water. A 20% iron nitrate 9 ~~ hydrate solution was added to the resulting suspension at a rate of 1.0 ml / min (maintained at about 75 ° C). At the same time 10% NaOH solution was added to maintain the pH value of 3. · 0. The suspended solid was filtered off, washed with water, and finally dried. Finally, the dried solid was calcined at 8 50 ° C. Slightly reddish-brown pigments with pearly luster and golden interference color. The following examples are examples of the application of pigments with pearly luster to paints, plastic compositions, and printing inks. Example 1 0 Basecoat for automobiles coat paint) is prepared according to the following formula. Lacquer system> Acrylic-melamine resin system " Acrydic 47712 " * 70 pbw " Superbekkamine G821-60 " ** 30 pb w toluene 30 pbw ethyl acetate 50 pbw η -butanol 110 pbw Solvesso # 150 40 pbw Dan Nippon (Dai n ippon) Ink & Chemicals Co., Ltd.'s acrylic resin This paper is again applicable to the Chinese National Standard (CNS) A4 specification (210X297 mm) (Please read the precautions on the back first and fill out this page) ▲ Order-29-A7 B7 V. Description of the invention (27) ** Melamine resin of Dannibon Ink & Chemicals Co., Ltd. The above-mentioned propylene-melamine resin system (100 P bw) was obtained with Examples 1 to 9 20 pbw flake alumina or pigment with pearl luster is combined. The resulting compound is diluted with a diluent so that the resulting paint has a sufficient consistency for paint. (12-15 seconds, F-ord Cup # 4). The paint is applied to the substrate by spraying to form a base coat layer. The base paint layer is further coated with a clear topless paint, which is based on the following formula And made: ( Please read the notes on the back before filling this page). "Clear paint on top" > " Acrydic 44-179 " 14 pbw " Superbekkaraine L117-60 " 6 pbw toluene 4 pbw MIBK 4 pbw butylcellulose Prime 3 pbw Printed by the Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs. The top coating was exposed to air at 40 ° C for 30 minutes, and then cured at 1 35 ° C for 30 minutes. Example 1 1 The primer for automobiles was prepared according to the following formula: The paper size is in accordance with the Chinese National Standard (CNS) A4 specification (210X29 * 7 mm) V. Description of the invention (28) < Primer system > " Dynapol H-700 " * l 25. 2 grams " Mapranal MF-650 " * 2 2. 7 grams " cellulose acetate ethyl butyrate 5 3 1 · 1 " $ 3 15 · 5 grams " Irgarol TZ-6 " 1.1 g of acetate. Ethyl ester. 23.3 g of xylene 11.6 g-Solvesso 150 " 1 1 g of C. I. Pigment red 1 77 4.5 g obtained in Examples 1 to 9 Flaky alumina or 4.5 g (please read the note on the back first to fill out this page) Printed by the Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs with pearlescent pigments * 1 So lvesso 1 5 0 Polyester resin 6 0% solution from Dynan No No 1 0 * 2 55% solution of melamine in butanol, from Hoechst. * 3 A 2 5% solution in a 1: 2 mixture of xylene and butyl acetate, available from Eastman Chemical International. * 4 Catalyst based on mineral oil and carboxylates, available from Giba—Geigy
I Ο 將上述組份利用球磨機（ba 1 1 m i 1 1 )混合9 6小時 ^使得顏料徹底地分散在蟲漆展色劑（lacquer vehicle )裡。將產生的組合物用醋酸丁酯，二甲苯及solvesso 1 5 0混合過的溶液來稀釋，以得到一根據D I N 4約 1 8秒0 °C )稠度的油漆。將該油漆塗在金屬板上。 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -31 - S86101 A7 B7 五、發明説明（29) 在約4 0°C的空氣裡曝附2分鐘之後，將該底漆層進一步 地用無色頂層塗漆再塗上一層，該塗漆係根據下列配方而 製得： <頂層清澈的塗漆） "V i a c r y 1 VC-373"*1 58. 3克 "M a p r e n a 1 MF-590"*2 2 7 · 3 克 矽酮油〃 3 ' --: 1 · 0克 "Tinuvin 900"*4 1. 0克 二甲苯 1 · 0克 "S o 1 v e s s o 15 0" 5. 4克 醋酸乙二醇酯 3. 0克 * 1 —甲本裡丙稀系樹脂的6 0%溶液，得自Vianora 。 ' 丁醇裡三.聚氰胺的5 5 %溶液，得自Hoechst。 * 3 1 %二甲苯溶液，得自Bayer。 *4 苯駢***衍生物，得自Giba- Geigy。 , 經濟部中央標準局員工消費合作社印製 (請先閱讀背面之注意事項再填寫本頁) 將頂層塗層曝露在4 0 °C的空k中3 0分鐘，然後在 1 3 5 °C固化3 0分鐘。 實施例1 2 該實施例係舉例說明以具有珍珠光澤之顏料在塑膠著 色上的應用》射出成型化合物（彈丸狀）係根據下列配方 藉由乾調初方式而製得》 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -32 - 386101 Δ7 A 7 ____—_Β7 克、發明説明（30) 聚乙烯樹脂（彈丸狀） 100 pbw 實施例1到9獲得的片狀氧化鋁或 1 pb«r 具有珍珠光澤的顏料 硬脂酸鋅 0. 2 pbw 石蠘.液 0.1 pbw 實施例1 3 - 該實施例係舉例說明以具有珍珠光澤之顏料在照相印 刷油墨上的應用，根據下列配方製得。 CCST介質 *1 10 pbw 實施例1到9獲得的片狀氧化鋁或 8 pbw 具有珍珠光澤的顏料 * 1 硝基纖維素樹脂，得自東京油墨公司。 ' . . 將因而獲得的油墨用溶液來稀釋（"NC 10 2〃 ， 經濟部中夹梂準局員工消費合作社印裝 (請先聞讀背面之注意事項再填寫本頁) 得自東乐公司），使得產生_的油墨真有Zahn杯第.3號2 0 秒的稠度。 本紙張尺度適用中國國家標準（CNS )_A4規格（210X297公釐） -33I 0 The above components were mixed using a ball mill (ba 1 1 m i 1 1) for 96 hours ^ so that the pigment was thoroughly dispersed in the lacquer vehicle. The resulting composition was diluted with a mixed solution of butyl acetate, xylene and solvesso 150 to obtain a paint having a consistency of about 18 ° C (0 ° C) according to D I N 4. Apply the paint to a metal plate. This paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm) -31-S86101 A7 B7 V. Description of the invention (29) After exposure to air at about 40 ° C for 2 minutes, the primer layer It is further coated with a colorless top coat, and the paint is prepared according to the following formula: < Clear top coat) " V iacry 1 VC-373 " * 1 58. 3g " M aprena 1 MF-590 " * 2 2 7 · 3 grams of silicone oil 〃 3 '-: 1 · 0 grams " Tinuvin 900 " * 4 1. 0 grams of xylene 1.0 · 0 grams " S o 1 vesso 15 0 & quot 5.4 grams of ethylene glycol acetate 3.0 grams * 1-a 60% solution of a methyl ester acrylic resin, obtained from Vianora. 'Butanol. A 55% solution of melamine in Hoechst. * 3 1% xylene solution from Bayer. * 4 Benzotriazole derivative, available from Giba-Geigy. Printed by the Consumer Cooperatives of the Central Bureau of Standards of the Ministry of Economic Affairs (please read the precautions on the back before filling this page). Expose the top coating to 40 ° C for 30 minutes, and then cure at 1 35 ° C 30 minutes. Example 1 2 This example illustrates the application of pigments with pearl luster to plastic coloring. "Injection molding compounds (pellet-like) are prepared by dry adjustment according to the following formula." This paper size applies to China Standard (CNS) A4 specification (210X297 mm) -32-386101 Δ7 A 7 ____—_ B7 g, description of the invention (30) polyethylene resin (pellet) 100 pbw flake alumina obtained in Examples 1 to 9 or 1 pb «r Pearlescent pigment zinc stearate 0.2 pbw Lichen. Liquid 0.1 pbw Example 1 3-This example illustrates the application of pigments with pearly luster to photographic printing inks, according to the following formula be made of. CCST medium * 1 10 pbw The flake alumina obtained in Examples 1 to 9 or 8 pbw pigment with pearl luster * 1 A nitrocellulose resin obtained from Tokyo Ink Co., Ltd. '.. The ink thus obtained was diluted with a solution (" NC 10 2〃, printed by the Consumer Cooperatives of the Associate Bureau of the Ministry of Economic Affairs (please read the precautions on the back before filling out this page) from Dongle Company), so that the ink produced has a consistency of Zahn Cup No. .3 20 seconds. This paper size applies Chinese National Standard (CNS) _A4 specification (210X297 mm) -33
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Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| TW85109691A TW386101B (en) | 1996-08-09 | 1996-08-09 | Flaky aluminum oxide and pearlescent pigment, and productioon thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| TW85109691A TW386101B (en) | 1996-08-09 | 1996-08-09 | Flaky aluminum oxide and pearlescent pigment, and productioon thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| TW386101B true TW386101B (en) | 2000-04-01 |
Family
ID=21625368
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| TW85109691A TW386101B (en) | 1996-08-09 | 1996-08-09 | Flaky aluminum oxide and pearlescent pigment, and productioon thereof |
Country Status (1)
| Country | Link |
|---|---|
| TW (1) | TW386101B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112479241A (en) * | 2020-12-28 | 2021-03-12 | 济南大学 | Method for preparing flake aluminum oxide by utilizing flake aluminum hydroxide |
-
1996
- 1996-08-09 TW TW85109691A patent/TW386101B/en not_active IP Right Cessation
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112479241A (en) * | 2020-12-28 | 2021-03-12 | 济南大学 | Method for preparing flake aluminum oxide by utilizing flake aluminum hydroxide |
| CN112479241B (en) * | 2020-12-28 | 2022-11-08 | 济南大学 | Method for preparing flake aluminum oxide by utilizing flake aluminum hydroxide |
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