TWI291893B - - Google Patents
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- TWI291893B TWI291893B TW93129518A TW93129518A TWI291893B TW I291893 B TWI291893 B TW I291893B TW 93129518 A TW93129518 A TW 93129518A TW 93129518 A TW93129518 A TW 93129518A TW I291893 B TWI291893 B TW I291893B
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1291893 五、發明說明(1) 【發明所屬之技術領域】 本發明係關於一種高固體含量之微粒粉末漿料之製造 方法,特別是指一種將經一次離心所得漿料,置於震動和 攪拌環境中,利用震動和攪拌破壞漿料中的粉體架橋,再 以二次離心等能量使固體及液體得以進一步分離,俾以增 加離心效率,且有助於得到更高固體含量的漿料者。 【先前技術】1291893 V. INSTRUCTION DESCRIPTION OF THE INVENTION (1) Technical Field of the Invention The present invention relates to a method for producing a high solid content particulate powder slurry, and more particularly to a slurry obtained by centrifugation in a vibration and stirring environment. In the vibration and agitation, the powder bridge in the slurry is destroyed, and the solid and liquid are further separated by energy such as secondary centrifugation to increase the centrifugal efficiency and contribute to obtaining a slurry with a higher solid content. [Prior Art]
奈米級材料具有高活性、大表面積、自我組裝、超晶 格特性及特殊光電效應等功能,未來五年我國將投入2 〇 〇 多億元研發,至2 0 1 0年奈米產值將達一千億美元的規模。 透過奈米特性的發揮,帶來科技與產品新突破,使未來的 民生生活方式產生改變。如新世代儲能產品,提供高儲能 密度電池及高效率環保能源,加速低污染、高效能之能源 的開發腳步,減少空氣汙染與石化能源的消耗。Nano-grade materials have high activity, large surface area, self-assembly, superlattice characteristics and special photoelectric effect. In the next five years, China will invest more than 2 billion yuan in research and development, and the output value of nanometer will reach in 2010. The size of a hundred billion dollars. Through the development of nano-characteristics, new breakthroughs in technology and products will be brought about, which will change the future lifestyle of people's livelihood. For example, new generation energy storage products provide high energy storage density batteries and high-efficiency environmentally friendly energy sources, accelerate the development of low-pollution and high-efficiency energy sources, and reduce air pollution and petrochemical energy consumption.
奈米層次所製造的奈米電子元件,在元件密度、速 度、耗能及成本上的效益,將遠遠超過現有的半導體技 術。奈米科技的家電產品如奈米電風扇、除濕機、空氣清 淨機、冷氣空調等;還有清潔衛浴設備等奈米科技應用, 主要著重除臭、殺菌功能。奈米材料與加工可應用在食衣 住行各方面則如藥品,可加速人體吸收;建築物的破璃、 衣服材料具有防火、殺菌的功能;以及汽車上的擋風玻 璃、後視鏡不容易起霧、明亮等。奈米級具有智慧型、舒 適性、保健性及機能性等之紡織品等。纖維本身或其表面 上利用奈米相關技術加以處理,產生保暖、防水透氣、防The nanoelectronic components manufactured at the nano level will far outweigh the existing semiconductor technologies in terms of component density, speed, energy consumption and cost. Nanotechnology's home appliances such as nano-fans, dehumidifiers, air cleaners, air-conditioning, etc.; as well as nano-technology applications such as clean bathroom equipment, mainly focus on deodorization and sterilization. Nano materials and processing can be applied to all aspects of food and clothing such as medicines, which can accelerate the absorption of the body; the glass and clothes of buildings have the function of fire prevention and sterilization; and the windshield and mirrors on the car are not Easy to fog, bright, etc. Nano-grade textiles with intelligence, comfort, health and functionality. The fiber itself or its surface is treated with nano-related technology to produce warm, waterproof, breathable, and resistant
第5頁 1291893 五、發明說明(2) 污、除臭、殺菌、改變光澤等效果。這些林林總總奈米科 技的應用已漸漸進入市場,成為民生必然的需要。 另一方面,粉體漿料的應用日廣,以微粒α - A 1 2 0 3為 例,其潛力無窮。1 9 9 4年以來非冶金鋁用氧化鋁的需求平 均年成長約達2. 4°/。,至2 0 0 6年會達4. 4百萬公噸。但據了 解其成長方向也隨時代改變與以往略異,最明顯的是以往 使用量少的反而增加,同時有新用途的出現;耐火物的用 量僅少量成長,而在合成沸石(Z e ο 1 i t e, 作请潔劑)及 其他鋁矽酸鹽,以及煉油催化材上的用量則增加,其成長 率已超過2 · 4 % /年。另外以精密陶瓷製品及研磨劑型態 用於電子工業的氧化鋁也顯著增加,其成長率更達16〜30 % /年。值得注意的是在合成礦物及研磨作業上所使用的 氧化銘粉末又以微粒粉末為主。由於化學合成的產率與成 本均與合成所使用原料的反應活性有關,而粒徑又為其主 要因素’因此如有易獲付的細粒原料將有助於產品成本的 降低,而造成大量的採用。這點對奈米α - A 1 2 0 3微粉的進 入合成用氧化紹的前途大有幫助。而在研磨作業上所使用 的氧化鋁粉末,除仍發揮傳統的研磨功能外,目前對金屬 及金屬氧化物的拋光作業 ,微粒氧化鋁成為最熱門的耗材對象。 然而,關於如前述之粉體漿料P遺著需求的增加,由於 粉體含量會影響運送成本和後續的製程已經成為問題 ,低粉體含量使運送和儲存的成本大幅提高,而且後續配 合的擠出製程等通常需要高粉體含量。Page 5 1291893 V. Description of invention (2) Effects such as pollution, deodorization, sterilization, and gloss change. The application of these forestry technologies has gradually entered the market and become an inevitable need of people's livelihood. On the other hand, the application of the powder slurry is extensive, and the particle α-A 1 2 0 3 is taken as an example, and its potential is endless. 4°/。 The demand for non-metallurgical aluminum alumina has an average annual growth of about 2. 4 ° /. It will reach 4.4 million metric tons in 2006. However, it is understood that its growth direction is also slightly different from the past. The most obvious is that the amount of use in the past has increased, and there have been new uses; the amount of refractory used has only grown in a small amount, while in the synthesis of zeolite (Z e ο The amount of 1 ite, as a cleaning agent) and other aluminosilicates, as well as refining catalysts, has increased, and its growth rate has exceeded 2 · 4 % / year. In addition, alumina used in the electronics industry in precision ceramics and abrasives has also increased significantly, with a growth rate of 16 to 30% per year. It is worth noting that the oxidized powder used in synthetic minerals and grinding operations is dominated by particulate powder. Since the yield and cost of chemical synthesis are related to the reactivity of the raw materials used in the synthesis, and the particle size is also the main factor', therefore, if there is a readily available fine-grained raw material, it will contribute to the reduction of the product cost, resulting in a large amount. Adoption. This is helpful for the incorporation of nano-α-A 1 2 3 micropowder into the future of oxidation. In addition to the conventional grinding function, the alumina powder used in the grinding operation is currently the most popular consumable object for the polishing of metals and metal oxides. However, with regard to the increase in the demand for the powder slurry P as described above, since the powder content affects the transportation cost and the subsequent process has become a problem, the low powder content greatly increases the cost of transportation and storage, and the subsequent cooperation Extrusion processes and the like generally require high powder content.
1291893 五、發明說明(3)1291893 V. Description of invention (3)
迄今為止,可以用離心沉降的方法來強化顆粒沉降 ,加速顆粒的沉降過程。在離心力場中,人工造成的離心 加速度可比自然界中固有的重力加速度,大幾十倍甚至幾 百倍,因此細粒和密度小的物料在離心力場中沉降比在重 力場中有效得多。離心沉降是一種高效的沉降方法’已經 被採用為粉體漿料之濃縮處理方法,它是利用固態兩相的 密度差,將分散在懸浮液中的固相顆粒在離心立場中快速 沉降分離的過程,離心沉降可根據不同的分離要求而分別 完成濃縮、澄清和分級等作業。在工作方式上有閒歇排料 和連續排料兩種。但面對高固體含量的要求,其處理效果 不理想。 針對上述高固體含量問題,對於濃縮的奈米槳料相當 重要,因為濃縮槳料要有類似電腦檔案之壓縮及解壓縮過 程、便於傳送,運輸及應用的便利性;加上濃縮過程必須 避免破壞粉粒的分散性,在解濃縮時只要簡易處理(例如: 加水)即能恢復原有槳料性能;濃縮槳料經長時間存放也不 會改變性質。過去使用凝絮劑、再壓濾和乾燥製程都不適 用。Up to now, centrifugal sedimentation can be used to enhance particle sedimentation and accelerate the sedimentation process of the particles. In the centrifugal force field, the artificial centrifugal acceleration can be several tens of times or even hundreds of times greater than the inherent gravitational acceleration in nature, so that fine-grained and low-density materials settle much more effectively in the centrifugal field than in the gravity field. Centrifugal sedimentation is a highly efficient sedimentation method 'has been used as a concentrated treatment method for powder slurry. It uses the density difference of solid two phases to rapidly settle the solid phase particles dispersed in the suspension in a centrifugal position. Process, centrifugal sedimentation can be concentrated, clarified and graded according to different separation requirements. There are two types of work methods: idle discharge and continuous discharge. However, in the face of high solid content requirements, the treatment effect is not satisfactory. In view of the above high solid content problem, it is very important for concentrated nano pulp, because the concentrated pulp has a compression and decompression process similar to computer files, convenient for transportation, transportation and application; plus the concentration process must avoid damage The dispersibility of the powder particles can be restored to the original paddle performance by simple treatment (for example, adding water) during decondensation; the concentrated paddle material does not change its properties after long-term storage. In the past, the use of flocculants, re-filtration and drying processes were not suitable.
然而,過去文獻所記載的處理方法並無提及破壞一次 離心漿料後的粉體架橋製程,由於離心製程可提高漿料的 固體含量,但是離心過程使粗粉體或粗凝團因受力大而快 速沈降,細粉體或細凝團則留在漿料上層,如此現象,即 使加大離心轉速和加長工作時間,分離液體後所得漿料固 體含量提局有限。However, the treatment method described in the past literature does not mention the powder bridging process after destroying a centrifugal slurry. Since the centrifugation process can increase the solid content of the slurry, the centrifugation process causes the coarse powder or coarse coagulum to be stressed. Large and rapid sedimentation, fine powder or fine coagulation remains in the upper layer of the slurry. This phenomenon, even if the centrifugal speed is increased and the working time is lengthened, the solid content of the slurry obtained after separating the liquid is limited.
第7頁 1291893 五、發明說明(4) 破壞粉體架橋技術已應用在食品、製藥、陶瓷、化工 -的粉體傳送,但目前並無針對濃縮漿料而設計的離心後破 壞粉體架橋的製程,特別是利用其非添加和非加熱特性, 達到提高固體含量的效果,加上殘餘水分大都留在粉體層 層相疊的顆粒接觸面間,攪拌造成上、下粉體重排,粗細 粉體有效的堆積,使堆積更緻密,一如級配處理可使密度 增加,再續以二次離心處理,在離心管中,離心力作用在 粉體上,因為粉體密度大於液體,水分沿此粒間間隙上 移,將粒間水排出,同時,此法對奈米粉體或一般粉體都 可以處理,其製程方式迥異於傳統,不僅是提高固體含 量,也產生提高漿料的價值,加上攪拌使粉體均勻化,減 _ 少後續製程缺陷,這是過去文獻未提及的新用途,特別適 用於奈米粉體的特殊要求,此為本案之新穎性。 【發明内容】 本發明係有鑑於前述情況而創作一種高固體含量之微 粒粉末漿料之製造方法,特別是指一種將經一次離心所得 漿料,置於震動和攪拌環境中,由於水分含量會影響運送 成本、包裝、儲存和後續的製程,利用震動和攪拌破壞漿 料中的粉體架橋,且攪拌可以使漿料粉體内獲得大幅且長 程的移動,而震動則是提供粉體短程移動的能量,在二次 離心前,先將粗細粉體有序和緻密排列,再以二次離心能 量使固液分離,不需要加熱,故不劣化漿料,如此,可大 ® 幅增加離心效率,且有助於得到更高固體含量的漿料者, 例如,將3 6 %固體含量的奈米氧化鋁,提高至5 4 . 6 %以上。Page 7 1291893 V. INSTRUCTIONS (4) Destruction of powder bridging technology has been applied to powder conveying in food, pharmaceutical, ceramics, and chemical industries, but there is currently no centrifugal crushing powder bridge designed for concentrated slurry. The process, especially the non-added and non-heated properties, achieves the effect of increasing the solid content, and the residual moisture is mostly left between the powder contact surfaces of the powder layers, and the stirring causes the upper and lower powders to be discharged. The effective accumulation of the powder makes the accumulation denser. As the grading treatment can increase the density, the secondary centrifugation is continued. In the centrifuge tube, the centrifugal force acts on the powder because the powder density is greater than the liquid, and the water is along the water. The intergranular gap moves up and the intergranular water is discharged. At the same time, the method can treat the nano powder or the general powder, and the process method is different from the conventional one, which not only improves the solid content, but also increases the value of the slurry. Adding agitation to homogenize the powder, reducing the defects of subsequent processes, which is a new use not mentioned in the literature, especially suitable for the special requirements of nano-powder. Sex. SUMMARY OF THE INVENTION The present invention has been made in view of the foregoing circumstances to create a high solid content particulate powder slurry manufacturing method, in particular, a slurry obtained by centrifugation, placed in a vibrating and stirring environment, due to moisture content Affecting transportation costs, packaging, storage, and subsequent processes, using vibration and agitation to break the powder bridge in the slurry, and stirring can achieve large and long-range movement of the slurry powder, while vibration provides short-range movement of the powder. The energy, before the second centrifugation, first arranges the fine powder in an orderly and dense manner, and then separates the solid and liquid by the secondary centrifugal energy, without heating, so the slurry is not deteriorated, so that the large-width can increase the centrifugal efficiency. And it is helpful to obtain a slurry having a higher solid content, for example, increasing the alumina alumina content of 3 6 % solid content to 54.6% or more.
第8頁 1291893 五、發明說明(5) ^發明可以快速的沈降粉體,有利於量產,具有快速、簡 單和低成本的優點。 【實施方式】 接著’兹列舉一些具體實施例,詳細介紹本發明之内 容及其所能達成之功效: 以粒徑小於1 Ο Ο η Π1的奈米氧化鋁漿料,因由溶液化學 反應法所得’其固體含量小於丨9 ν 〇丨%,圖一為在稜驗值 1 1· 4,轉速6 0 0 0 rpm,時間2〜1〇分鐘内的固含量變化,達5 分鐘後’固含量幾達定值,證實延長工作時間,包括再次 離心,對固含量幫助不大。 本案之實施程序如下: 1. 一次離心:離心條件為轉速1〇〇〇〇rpm,時間丨〇分 鐘,並在一次離心後移除I料上層之澄清水。 2 ·震動和授1 f二·搜拌轉速5rpm,時間10分鐘 後,超音波震動2 〇 /刀鐘。 rpm,時間1 0分 鐘 3·二次離心:離心條件為轉迷1〇〇〇〇 其中的震動和授摔處理,將4κ a 下層粗細粉體兼具長短種混合和^ f叙肢架橋,並此上 緻密。 和有序堆積排列,堆積更為 第二圖為在酸性溶液下,—A 後,氧化鋁之固含量比較表。由^離心及本發明二次離心 量介於39〜48·5vol%,而震動LH,一次離心後固含 含量介於45· 7〜56· 4v〇U,比和祝雷拌處理後二次離心的固 早用震動或超音波效果好,Page 8 1291893 V. INSTRUCTIONS (5) ^ The invention can quickly settle powder, is advantageous for mass production, and has the advantages of fast, simple and low cost. [Embodiment] Next, the specific contents of the present invention and the effects thereof can be exemplified in detail. The nano alumina slurry having a particle diameter of less than 1 Ο Ο η Π1 is obtained by a solution chemical reaction method. 'The solid content is less than 丨9 ν 〇丨%. Figure 1 shows the solid content change in the tempering value of 1 1 · 4, the rotational speed of 600 rpm, and the time is 2~1〇, and the solid content after 5 minutes. A few fixed values confirm the extended working time, including re-centrifugation, which does not help the solids content. The procedure for the implementation of this case is as follows: 1. One-time centrifugation: Centrifugal conditions are 1 rpm, time 丨〇 minutes, and the clarified water of the upper layer of I material is removed after one centrifugation. 2 · Vibration and 1 f 2 · Mixing speed 5 rpm, after 10 minutes, the ultrasonic vibration 2 〇 / knife clock. Rpm, time 10 minutes 3 ·Secondary centrifugation: Centrifugal conditions are the vibration and drop treatment of the 1 转 a 粗 , , , , , , 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 This is dense. And the orderly stacking arrangement, the second stack is the comparison table of the solid content of alumina in the acidic solution, after -A. By centrifugation and the second centrifugation amount of the present invention is between 39 and 48·5 vol%, and the vibration LH, the solid content after one centrifugation is between 45·7~56·4v〇U, and the ratio is twice after the treatment. Centrifugal solid early use vibration or ultrasonic effect is good,
1291893 五、發明說明(6) 所以震動和攪拌 I呂之固含量。 5 0 v ο 1 %固含 的下限,過多水 和攪拌使粉體均 減少應用離心粉 均所致裂紋,這 震動和攪拌環境 原始物性以供高 性亦由此可知。 上述的粉體 放置於攪拌環境 中,可以使用機 混合漿料中上下 上述的粉體 離心濃縮漿料放 動作用過程中, 復式震動和衝擊 的。 而上述攪拌 程序後再依序進 處理後二次離心的方式能有效的提高氧化 量是奈 分會導 勻化, 體所產 是單獨 中完全 價值之 漿料置 中,調 械攪拌 層粉體 漿料置 置於震 可以使 式震動 和震動 行攪拌 行一次離心程序時,同 和授拌破壞漿料中的粉 體進一步分離,以得到1291893 V. INSTRUCTIONS (6) So shake and stir Ilu solid content. 5 0 v ο 1 % of the lower limit of solid content, too much water and agitation to reduce the cracks caused by the application of centrifugal powder. This vibration and agitation environment are also known for their high physical properties. The above powder is placed in a stirred environment, and the above-mentioned powder can be used in the mixed slurry to centrifugally concentrate the slurry during the action of the double shock and impact. After the above-mentioned stirring procedure, the method of secondary centrifugation followed by sequential centrifugation can effectively increase the amount of oxidation, and the homogenization will be homogenized. The body is produced in a separate medium of complete value, and the mixing and stirring layer powder slurry is prepared. When the material is placed in the earthquake, the vibration and the vibration can be stirred and the centrifugal process is performed once, and the powder in the mixed slurry is further separated to obtain the powder.
米氧化鋁直接適用於陶瓷擠出成型 致擠出生坯過軟而變形,加上震動 粗細粒徑粉體能緻密化堆積,大幅 生的成型和燒結缺陷,例如收縮不 使用離心所無法解決的問題,加上 不需加溫和添加藥劑,並保留溶液 利用,此製程改良的實用性和關鍵 入攪拌程序時,係將待疼理之漿料 整功率和時間,在攪拌作用過程 、磁力攪拌和氣泡攪拌之集合達成 之目的。 入震動程序時,係將待處理之一次 動環境中,調整功率和時間,在震 用機械偏心震動、超音波震動、往 之集合達成混合漿料中粉體之目 能量係可於粉體漿料進行一次離心 和震動程序,或亦可於粉體漿料進 時進行震動和攪拌程序,利用震動 體架橋,再以二次離心使固體及液 高固體含量之微粒粉末漿料者。Rice alumina is directly suitable for ceramic extrusion molding, and the extruded green body is too soft and deformed. In addition, the vibration thickness particle size can be densified and accumulated, and the large-scale molding and sintering defects, such as shrinkage cannot be solved without using centrifugation. The problem, plus no need to warm and add the agent, and retain the use of the solution, the practicality of the process improvement and the key into the mixing process, the pulp will be treated with the power and time, during the stirring process, magnetic stirring And the purpose of the collection of bubble agitation. When entering the vibration program, the power and time are adjusted in the first moving environment to be treated. In the seismic eccentric vibration, ultrasonic vibration, and the combination, the powder energy of the powder can be obtained in the powder slurry. The material is subjected to a centrifugation and shaking procedure, or a vibration and agitation procedure may be performed while the powder slurry is being introduced, and the solid body and the liquid high-solid content fine particle powder slurry are used by using a vibrating body bridge.
第10頁 1291893 五、發明說明(7) 另外,各類漿料因材質、來源、製作參數和品管等差 異,需要濃縮製程部分,如污泥脫水、藥物萃取、粉體合 成後去除溶液和礦物分選等,而有進一步固體及液體分離 或乾燥步驟,經過一次離心之半成品,攪拌和震動後可再 施予二次離心,以進一步徹底固體及液體分離,即本案製 程所欲得的產品,包括粉體和澄清液兩部份。 如此,在二次固體及液體分離製程中,若配合濃縮程 序,可續採沈澱、過濾和二次離心至少一種方法作用 。其中過濾可為壓濾或真空過濾之集合。Page 10 1291893 V. Description of the invention (7) In addition, various types of slurry require concentration process parts due to differences in materials, sources, production parameters, and quality control, such as sludge dewatering, drug extraction, and powder synthesis to remove the solution. Mineral sorting, etc., and further solid and liquid separation or drying steps, after a semi-finished product after centrifugation, after stirring and shaking, it can be further centrifuged to further completely separate the solid and liquid, that is, the product desired in the process of the present process. , including powder and clear liquid. Thus, in the secondary solids and liquid separation process, if the concentration process is combined, at least one of the methods of sedimentation, filtration, and secondary centrifugation can be continued. The filtration can be a collection of pressure filtration or vacuum filtration.
前述之粉體漿料材質可包括金屬、陶瓷、高分子和複 合材料之集合等。由於這幾類粉體,皆具有固、液混合 態,所遭遇的濃縮問題皆相同,因此適用於本法。 此外,上述離心時,可同時設計離心機外加攪拌裝 置,或離心機外加震動裝置,或離心機同時具攪拌和震動 裝置,一次離心後,在原位處理攪拌和震動混合,復以二 次離心,如此可節省製程的時間與能源,有利於自動化。The foregoing powder slurry material may include a collection of metals, ceramics, polymers, and composite materials. Since these types of powders have a solid-liquid mixed state and the same concentration problems are encountered, they are applicable to this method. In addition, during the above centrifugation, the centrifuge can be designed with a stirring device at the same time, or the centrifuge can be equipped with a vibrating device, or the centrifuge can be equipped with a stirring and shaking device. After one centrifugation, the mixing and shaking mixing is performed in situ, and the second centrifugation is repeated. This saves time and energy in the process and is conducive to automation.
本發明提供之高固體含量之微粒粉末漿料之製造方 法,適用於污泥脫水、藥物萃取、粉體合成後去除溶液和 礦物分選等,減少運送成本、包裝、儲存和後續的製程問 題,因不需要加熱和添加劑,故不劣化和污染漿料,如 此,可大幅增加分離效率,且有助於得到更高固體含量的 漿料和更高純度澄清液者,加上攪拌及震動將使粉體均勻 化,有利於減少後續製程缺陷,具有快速、簡單和高附加 價值的優點。The invention provides a method for manufacturing a high solid content particulate powder slurry, which is suitable for sludge dewatering, drug extraction, powder removal, solution removal and mineral sorting, etc., and reduces transportation cost, packaging, storage and subsequent process problems. Since heating and additives are not required, the slurry is not deteriorated and contaminated, so that the separation efficiency can be greatly increased, and a slurry having a higher solid content and a higher purity clarified liquid can be obtained, and stirring and vibration will be The homogenization of the powder is beneficial to reduce defects in subsequent processes, and has the advantages of quickness, simplicity, and high added value.
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