1240699 玖、發明說明： 【發明所屬之技術領域】 本發明是有關於一種製造程序，特別是指一種獲得奈 米級二氧化鈦的奈米粉體製造程序。 5 【先前技術】 二氧化鈦（Ti02)對光具有高折射率，且吸收紫外線後 會產生觸媒效應，因此，應用領域相當廣泛，其中包括顏 料、化妝品、光觸媒、陶瓷釉料、紡織纖維、複合材料... 等。而開發奈米級二氧化鈦的目的在於，該奈米級二氧化 10 鈦會產生量子躍遷(quantum jump)的物理現象，可以大幅提 昇上述特性的使用效果。 目前市面上製造二氧化鈦的方法相當多，以光觸媒粉 體的製造方法為例，主要包含有下列方法： 1. 以水難溶性的有機物皮膜對二氧化鈦微粒作表面包 15 覆，再以高溫燒結而成，而該二氧化鈦微粒的尺寸並不是 奈米級，所以，效能的提昇有限。 2. 以鹵化欽為原料，進彳于氣相反應製成—氧化欽彳鼓粒 子，再以多孔質磷酸鈣包覆於二氧化鈦微粒子表面，惟， 這種方法必須使用陰離子性的界面活性劑，且二氧化鈦微 20 粒子的平均粒徑分存範圍較不集中，為0.001〜0.2微米。 3. 以物理製備方法，用加壓衝撞的方式分散該二氧化 鈦微粒子，但是，這種加壓衝撞的方式，只能分散微粒子 並不具有研磨粉碎的功能，所以，該二氧化鈦微粒子仍然 不能到達奈米級尺寸，且必須以除氣泡裝置除去過程中產 1240699 生的氣泡。 【發明内容】 因此，本發明之目的，即在提供一種能製造奈米級二 氧化鈦的奈米粉體製造程序。 5 於是，本發明的奈米粉體製造程序包含：以二氧化鈦 粉體做為溶質，及以有機液體乙二醇做為溶媒，調製成懸 浮液。攪拌該懸浮液，使溶質與溶媒充份混合。以濕式球（ 珠）磨法粉碎及分散該懸浮液。離心萃取該懸浮液中的粉粒 體，獲得奈米級的粉體成品。 10 本發明的功效是能獲得奈米級的粉體成品。 【實施方式】 有關本發明之前述及其他技術内容、特點與功效，在 以下配合參考圖式之二較佳實施例的詳細說明中，將可清 楚的明白。 15 參閱圖1，本發明的奈米粉體製造程序包含下列步驟 步驟一：以平均粒徑300 nm〜400 nm的微米級二氧化 鈦粉體做為溶質，及以有機液體乙二醇做為溶媒，調製成 懸浮液。該二氧化鈦粉體與乙二醇的重量百分比濃度為4 20 〇/〇 〜12%。 步驟二：以人工或機械攪拌的方式，攪拌該懸浮液， 使二氧化鈦粉體均勻地溶於乙二醇中。而該攪拌的動作要 溫和，不宜太劇烈，建議攪拌速度為40 rpm〜120 rpm。 步驟三：參閱圖2，以一濕式球(珠）磨裝置1粉碎及 1240699 分散該懸浮液。該濕式球(珠）磨裝置1主要包含有一中空 且容置有懸浮液的研磨室11、多數容置在研磨室11内且 0.5腿以下的研磨珠12、一沿一軸線X方向穿置在該研磨 室11内的轉子13，及數彼此相間隔地套固在該轉子13上 5 的迴轉盤14。該等迴轉盤14分別具有數散佈在一上盤面 141與一下盤面142且沿該轴線X方向突出的攪動梢143 。該研磨珠12是以二氧化锆製成，用量約佔研磨室11總 容積的5%〜25% ，粉碎及分散該懸浮液時，溫度是控制在 室溫以下，持續作業2〜8小時。藉此，當轉子13帶動迴 10 轉盤14產生強力渦流時，就能以突出的攪動梢143撞擊 研磨珠12，使研磨珠12產生強力的撞擊力及剪切力分散 及粉碎該懸浮液，使懸浮液中的粉粒體尺寸小至奈米級。 此時，該製造程序可以選擇粉體是否要求以更小的粒徑等 級輸出，如果選擇否，則會輸出平均粒徑120 nm〜170 nm 15 的奈米級二氧化鈦粉體成品。 步驟四：若是要求粉體以更小的粒徑等級輸出，則參 閱圖3，以一離心萃取裝置2萃取該懸浮液中的粉粒體。 該離心萃取裝置2包含一載體21、一可旋動的容置在載體 21内的轉體22,及一固定在載體21上的控制單元23。該 20 載體21可將研磨後的懸浮液導入轉體22内。該控制單元 23可驅動轉體22以23000〜36000 G的相對離心力，高速 轉動3〜30分鐘，分離懸浮液内粒徑不符合要求的粉粒體 ，萃取出平均粒徑40 nm〜80 nm的奈米級二氧化鈦粉體成 品0 7 1240699 步驟五：無論是平均粒徑120 nm〜170 nm或是40 nm〜80 nm的粉體成品，其成品狀態皆為濕式懸浮液，此 時可視需要，經由烘乾的步驟獲得乾式的奈米級二氧化鈦 粉體成品。 5 參閱圖4，值得一提的是，當10 nm〜40 nm的奈米級 二氧化鈦乾燥粉體原料，如果因為長時間存放或其他因素 ，而發生再團聚現象，聚合成微米級二氧化鈦粉體，此時 也可以將該微米級二氧化鈦粉體原料，送經上述調製、攪 拌、粉碎或分散、離心萃取或烘乾等程序，充份的分散還 10 原成奈米級的二氧化鈦粉體成品。 據上所述可知，本發明之奈米粉體製造程序具有下列 優點及功效： 本發明可以將原始平均粒徑為300 nm〜400 nm的微米 級二氧化鈦粉體原料，充份地粉碎並萃取出平均粒徑為30 15 nm〜80 nm的奈米級成品，也可以將原本平均粒徑為10 nm〜40 nm的二氧化鈦乾燥粉體，因團聚現象聚合成微米級 的二氧化鈦粉體原料，充份的分散還原成奈米級的二氧化 鈦粉體。使本發明能確實獲得粒徑平均的奈米級二氧化鈦 粉體。 20 惟以上所述者，僅為本發明之較佳實施例而已，當不 能以此限定本發明實施之範圍，即大凡依本發明申請專利 範圍及發明說明書内容所作之簡單的等效變化與修飾，皆 應仍屬本發明專利涵蓋之範圍内。 【圖式簡單說明】 1240699 圖1是一方塊圖，說明本發明一奈米粉體製造程序的 第一較佳實施例； 圖2是一剖視圖，說明該第一較佳實施例所使用的分 散研磨裝置； 5 圖3是一剖視圖，說明該第一較佳實施例所使用的離 心萃取裝置；及 圖4是一方塊圖，說明本發明一奈米粉體製造程序的 第二較佳實施例。 10 9 1240699 【圖式之主要元件代表符號簡單說明】 ………濕式球磨裝置 142…… ……下盤面 11…… 14 3 ^ V ：：. * ^ ……攪動梢 ……"研磨珠 2,……… ……離心萃取裝置 13…… ^ ：i i * s· 21……… ……載體 1 Λ ^ ^ ……"迴轉盤 22……" ……轉體 14* 1 *+、^ ……“上盤面 22 ……控制單元 101240699 发明 Description of the invention: [Technical field to which the invention belongs] The present invention relates to a manufacturing process, and more particularly, to a manufacturing process of nano-powder to obtain nano-grade titanium dioxide. 5 [Previous technology] Titanium dioxide (Ti02) has a high refractive index for light and will have a catalytic effect after absorbing ultraviolet rays. Therefore, it has a wide range of applications, including pigments, cosmetics, photocatalysts, ceramic glazes, textile fibers, and composite materials. ... Wait. The purpose of developing nanometer titanium dioxide is that the nanometer titanium dioxide will produce a physical phenomenon of quantum jump, which can greatly improve the use effect of the above characteristics. At present, there are many methods for manufacturing titanium dioxide on the market. Taking the manufacturing method of photocatalyst powder as an example, it mainly includes the following methods: 1. The surface of the titanium dioxide particles is coated with 15 water-insoluble organic film, and then sintered at high temperature. The size of the titanium dioxide particles is not nanometer, so the efficiency improvement is limited. 2. The halogenated chitin is used as the raw material, which is made by gas phase reaction-oxidation of chitin drum particles, and then coated with porous calcium phosphate on the surface of titanium dioxide particles. However, this method must use anionic surfactants. In addition, the average particle size distribution range of the titanium dioxide micro-20 particles is less concentrated, and is 0.001 to 0.2 microns. 3. The titanium dioxide microparticles are dispersed by means of pressure impact by a physical preparation method. However, this method of pressure impact can only disperse the microparticles and does not have the function of grinding and pulverizing. Therefore, the titanium dioxide particles still cannot reach nanometers. Class size, and the bubble generation device must be removed in the process of 1240699 bubbles. SUMMARY OF THE INVENTION Therefore, an object of the present invention is to provide a nanometer powder manufacturing process capable of manufacturing nanometer titanium dioxide. 5 Therefore, the nano-powder manufacturing process of the present invention includes: using titanium dioxide powder as a solute, and organic liquid ethylene glycol as a solvent to prepare a suspension. The suspension was stirred to thoroughly mix the solute and the solvent. The suspension was pulverized and dispersed by a wet ball (bead) mill method. The powder and granules in the suspension were extracted by centrifugation to obtain a nano-sized powder product. 10 The effect of the present invention is to obtain a nano-grade powder product. [Embodiment] The foregoing and other technical contents, features, and effects of the present invention will be clearly understood in the following detailed description with reference to the second preferred embodiment of the drawings. 15 Referring to FIG. 1, the nano-powder manufacturing process of the present invention includes the following steps. Step 1: Use micron-sized titanium dioxide powder with an average particle diameter of 300 nm to 400 nm as a solute, and use organic liquid ethylene glycol as a solvent to prepare Into suspension. The weight percentage concentration of the titanium dioxide powder and ethylene glycol is 4 200/0 to 12%. Step 2: Agitate the suspension manually or mechanically to make the titanium dioxide powder evenly dissolve in the ethylene glycol. The stirring action should be gentle and not too violent. The recommended stirring speed is 40 rpm ~ 120 rpm. Step 3: Refer to FIG. 2, use a wet ball (bead) mill device 1 to pulverize and disperse the suspension 1240699. The wet ball (bead) grinding device 1 mainly includes a hollow grinding chamber 11 containing a suspension, a plurality of grinding beads 12 housed in the grinding chamber 11 and below 0.5 legs, and a penetrating device along an axis X. The rotor 13 in the grinding chamber 11 has a plurality of rotating disks 14 fixed to the rotor 13 at intervals. The rotary disks 14 each have a plurality of agitating tips 143 that are scattered on an upper disk surface 141 and a lower disk surface 142 and protrude in the X direction of the axis. The grinding beads 12 are made of zirconia, and the amount is about 5% to 25% of the total volume of the grinding chamber 11. When the suspension is crushed and dispersed, the temperature is controlled below room temperature, and the operation is continued for 2 to 8 hours. Thereby, when the rotor 13 drives back 10 and the turntable 14 generates a strong vortex, it can hit the grinding beads 12 with the protruding stirring tip 143, so that the grinding beads 12 generate a strong impact force and shearing force to disperse and crush the suspension, so that The size of the particles in the suspension is as small as nanometers. At this time, the manufacturing process can choose whether the powder is required to be output at a smaller particle size level. If you choose No, it will output a finished nano-sized titanium dioxide powder with an average particle size of 120 nm ~ 170 nm 15. Step 4: If the powder is required to be output at a smaller particle size level, refer to FIG. 3, and extract the powder and granules in the suspension with a centrifugal extraction device 2. The centrifugal extraction device 2 includes a carrier 21, a swivel body 22 housed in the carrier 21, and a control unit 23 fixed on the carrier 21. The 20 carrier 21 can introduce the ground suspension into the rotor 22. The control unit 23 can drive the swivel body 22 to rotate at a high centrifugal force of 23000 ~ 36000 G for 3 to 30 minutes at high speed to separate the powder and granules whose particle diameter does not meet the requirements, and extract the average particle diameter of 40 nm to 80 nm. Nano-sized titanium dioxide powder finished product 0 7 1240699 Step 5: Whether it is a powder finished product with an average particle size of 120 nm ~ 170 nm or 40 nm ~ 80 nm, its finished product state is a wet suspension, at this time, as needed, The dried nano-sized titanium dioxide powder product is obtained through the drying step. 5 Referring to FIG. 4, it is worth mentioning that when the nanometer titanium dioxide dry powder raw material of 10 nm to 40 nm is re-aggregated due to long-term storage or other factors, it will be polymerized into micron titanium dioxide powder. At this time, the micron-level titanium dioxide powder raw material can also be sent to the above-mentioned procedures for preparation, stirring, pulverization or dispersion, centrifugal extraction or drying, and the dispersion can be reduced to 10 nanometer titanium dioxide powder products. According to the above, it can be known that the nanometer powder manufacturing process of the present invention has the following advantages and effects: The present invention can fully pulverize and extract the average micron-sized titanium dioxide powder raw material with an average particle diameter of 300 nm to 400 nm and extract the average Nano-sized finished products with a particle size of 30 15 nm to 80 nm can also be used to dry titanium dioxide powder with an average particle size of 10 nm to 40 nm to aggregate into micron-sized titanium dioxide powder raw materials due to agglomeration. Disperse and reduce to nanometer titanium dioxide powder. In the present invention, nano-sized titanium dioxide powder having an average particle diameter can be surely obtained. 20 However, the above are only the preferred embodiments of the present invention. When the scope of the present invention cannot be limited by this, that is, the simple equivalent changes and modifications made according to the scope of the patent application and the contents of the invention specification , All should still fall within the scope of the invention patent. [Schematic description] 1240699 FIG. 1 is a block diagram illustrating the first preferred embodiment of the nanometer powder manufacturing process of the present invention; FIG. 2 is a cross-sectional view illustrating the dispersion grinding used in the first preferred embodiment Apparatus; 5 FIG. 3 is a cross-sectional view illustrating a centrifugal extraction apparatus used in the first preferred embodiment; and FIG. 4 is a block diagram illustrating a second preferred embodiment of a nanometer powder manufacturing process of the present invention. 10 9 1240699 [Simplified explanation of the main symbols of the drawings] ............ Wet ball milling device 142 ...... ...... Lower plate surface 11 …… 14 3 ^ V ：: * ^ ...... Stirring tip ...... " Grinding beads 2, …………… Centrifugal extraction device 13 …… ^: ii * s · 21 …………… Carrier 1 Λ ^ ^ …… " Rotary plate 22 …… " …… Rotate 14 * 1 * + , ^… "On the surface 22 ...... control unit 10