1281463 九、發明說明: 【發明所屬之技術領域】 本發明係有關於一種含膠體的擠出塑料之水分調控方 去,其主要係將泥料以微波處理,以去除多餘水分,而濃 縮至適於擠出的含水率,以求快速、均勻濃縮及大量生產 之目的,藉以適合於含化學膠體的擠出塑料之水分調控方 法者。 _ 【先前技術】 按,目前擠出成形係利用潤溼且具有内聚力之塑性陶 瓷配料,以壓力將之擠壓經模具產生截面均勻的述體,擠 出成形分成連續式與半連續式兩種方式,所施之壓力比乾 粉壓製略低,其操作步驟依入料、擠推、擠入模具及通孔、 擠出順序,而模具又分為熱模與冷模雨種,熱模可以改善 陶瓷粉料的流動特性,陶瓷擠出成形之配料所添加之有機 物必需具有良好的流動能力、潤溼性、與脫脂順利性’又 • 操作與機台參數包含·· (1)擠出成形長寬比(AsPect1281463 IX. Description of the invention: [Technical field to which the invention pertains] The present invention relates to a moisture regulating method for a colloid-containing extruded plastic, which mainly uses a microwave treatment to remove excess water and concentrates to a suitable temperature. For the purpose of rapid, uniform concentration and mass production, the moisture content of the extrusion is suitable for the moisture control method of the extruded plastic containing chemical colloid. _ [Prior Art] According to the current extrusion molding system, a plastic ceramic compound which is wet and has cohesive force is used, and the pressure is pressed through the mold to produce a uniform cross-section, and the extrusion molding is divided into continuous and semi-continuous. In the way, the pressure applied is slightly lower than that of dry powder pressing, and the operation steps are based on feeding, pushing, squeezing into the mold and through hole, and extrusion sequence, and the mold is divided into hot mold and cold mold rain, and the hot mold can be improved. The flow characteristics of ceramic powders, the organic substances added by the ceramic extrusion forming ingredients must have good flowability, wettability, and smooth degreasing'. • Operation and machine parameters include · (1) Long extrusion molding Aspect ratio (AsPect
Ratio)、意即模具長度與擠出物件直徑之比值;(2)坯 體厚度的遞減比值;(3)配料的擠出速率;(4)真空度; 、 (5)擠出所施之油壓壓力;(6)模溫;(7)機台潤滑準 備動作。 而擠出成形的機台有旋動鑽頭式與滑桿動式,陶瓷配 料混練後似是一堆麵團,包含陶瓷粉末、溶劑、黏結劑、 增塑劑、分散劑、潤滑劑與表面活性劑等添加物;當配料 1281463 , 進入捏練槽中加以反覆捏練,促其增加塑性,再將配料送 / 入除氣室,抽除配料中的空氣,然後擠入模具,擠出成形 像是麵包師傅用彩色奶油擠經飾花筒,變成可愛的裝飾花 樣於蛋糕上面,因陶瓷擠出成形之配料含達25〜50volG/〇的有 機添加物,生坯進行脫脂必須額外謹慎,加溫速率不能過 高,否則易使坯體龜裂、腫大、或變形;若配料中的陶瓷 粉末的粒徑細小且粒徑分佈範圍小者,將有助於減低燒成 溫度,亦可避免當擠出時所造成配粉成分的不均勻性,擠 _ 出成形的產品包括燒結爐的陶瓷管、蜂窩式陶瓷體、石墨 電極、扁平基板、與電熱隅之陶兗護管等。 擠出成型(extrusion )適合製作截面一致,長寬比高 之產品,廣泛應用於陶莞爐管、而ί火物、蹲塊、磁磚、觸 媒載體、熱交換器等,擠出成型利用濕潤且具有内聚力的 塑性陶瓷配料,以壓力將之擠入模具產生截面均勻的坯 體,對於沒有黏性的陶瓷粉末,可利用添加黏結劑使其產 0 生塑性成型。 為了得到理想中的塑性陶瓷配料,需要了解起始粉末 粒徑分佈與堆積狀況,添加適量的成形助劑,調整黏度與 擠出述料的固體含量和含水量,再進行適當的擠出成形、 脫脂及熱處理,即可得到理想的試片。 本發明暫不討論或評斷生胚成型法、燒結、陶瓷材質 或添加劑成分問題;僅特別針對一般的含膠體泥料的水分 調整處理提出另一作法。 1281463 一般現行較為普遍的粉體混合處理,為了使陶瓷粉末 / 容易成型生胚,通常把黏著劑、填充劑、界面活性劑或潤 滑劑與乾燥的陶瓷粉體混合,唯採用陶瓷粉末與水、黏結 劑混練的方式會產生許多問題,特別是含膠體的陶瓷奈米 粉末所製作的擠出泥料,製作過程因混入膠體而含水量過 高,其水分控制方法,難以兼具快速、均勻和量產性。 膠體製作時須具有相當的配合水量,亦即使用膠體為 成形助劑時,泥料本身含水量可高達40-60%,一般以15-20% _ 為適當範圍,而含水量過多的生胚,容易變形和產生内部 缺陷,造成擠出困難或是具成形缺陷,對成型和燒結都有 相當不利的影響,加上陶兗的機械性質對缺陷敏感,因此 如何解決含膠體的陶瓷泥料的水分控制問題,此為使用膠 體為成形助劑的技術關鍵所在。 針對上述問題,目前大部分採用離心濃縮或壓濾方式 調控泥料含水量,但是離心濃縮方式會因比重的不同,使 φ 氧化鋁粉粒沉降分離,採用壓濾方式則因膠體微細,去水 不易,不適用大量生產,傳統加熱乾燥亦造成泥料表面乾 燥過快而易結成硬膜,以致無法使用。 ’ 【發明内容】 爰此,有鑑於含膠體的擠出塑料具有上述之缺失與問 題,故本發明係在提供一種含膠體的擠出塑料之水分調控 方法,乃藉由應用微波均勻加熱含膠體泥料操控其水量, 利用化學反應合成的膠體溶液與陶瓷粉體混合,經濃縮步 1281463 , 驟調整成坯體所需的水分比,直接與黏著劑、填充劑、界 〆 面活性劑或潤滑劑與潮濕的陶瓷粉體混合,由於顆粒間一 直保有大量液態水,此法可以免除傳統加熱乾燥粉體所導 致的凝聚,粉體一直保持分散狀態,因此無去凝聚問題, 過量的水藉由微波自生坯均勻移除,達到控制含水量的目 的。 本發明係應用微波加熱解決含膠體潮濕泥料之水量控 制,以膠體為成型助劑,關鍵在於含水量的控制,藉由微 B 波快速加熱、均勻濃縮和易於大量生產,可配製適合擠出 成形之泥料,使工業化生產的成本大幅降低。 【實施方法】 本創作係為一種含膠體的擠出塑料之水分調控方法, 如第一圖所示,其方法係為: A. 漿液製備:漿液製作時,利用氨水以及硝酸作為分 散劑,將工業用α-Α1203粉末及boehmite(氫氧化銘),後 φ 者為PH值約3的水溶液中溶膠(sol),分別以氨水和硝酸混 合後成為分散的漿液。 B. 微波濃縮:以微波加熱濃縮法提高A1203的固粒含 ' 量,降低其含水量,將沉降的混合膠體放入微波爐中烘乾 至適當的含水率,含水量與微波時間的關係如第二圖所 示,氧化鋁漿液經一次或多次濃縮後,將分離出之漿料取 出,以獲得高濃度(53vol% )的漿料,含水率約18wt% , 符合擠出泥料所需之含水率。 1281463 (C)混合和成型:將濃縮漿 性的泥料以進行擠出的試驗,這指劑’製作具可塑 播出成形,使用微型擠出機能擠=㈣經捏棟抽真空後 出坏料乾燥後燒結,如附件所示^細乳化崎;最將擠 其特徵在於:對於該含膠二銘裝料燒結後外觀。 題’泥料的濃縮過程採微波加埶 尼料的水分控制問Ratio), meaning the ratio of the length of the mold to the diameter of the extruded object; (2) the decreasing ratio of the thickness of the blank; (3) the extrusion rate of the ingredients; (4) the degree of vacuum; (5) the oil applied by extrusion Pressure; (6) mold temperature; (7) machine lubrication preparation action. The extrusion forming machine has a rotary drill type and a sliding rod type. After mixing the ceramic ingredients, it seems to be a pile of dough, including ceramic powder, solvent, binder, plasticizer, dispersant, lubricant and surfactant. Additives; when the ingredients 1281463, enter the kneading tank to repeatedly knead, to increase the plasticity, then send the ingredients into the degassing chamber, remove the air in the ingredients, and then squeeze into the mold, extrusion molding is like The baker squeezed the decorative tube with colored cream and turned it into a cute decorative pattern on the cake. Since the ceramic extrusion molding ingredients contain organic additives of 25~50 volG/〇, the green body must be degreased with extra caution. The heating rate cannot be increased. If it is too high, it will easily crack, enlarge, or deform the body; if the ceramic powder in the batch has a small particle size and a small particle size distribution, it will help to reduce the firing temperature and avoid extrusion. The non-uniformity of the powder component caused by the extrusion, the extruded product includes a ceramic tube of a sintering furnace, a honeycomb ceramic body, a graphite electrode, a flat substrate, a ceramic tube with an electric heating pot, and the like. Extrusion is suitable for the production of products with uniform cross-section and high aspect ratio. It is widely used in pottery tubes, but also in fireworks, crucibles, tiles, catalyst carriers, heat exchangers, etc. The plastic ceramic compound with cohesive force is squeezed into the mold by pressure to produce a uniform body with a uniform cross section. For the non-sticky ceramic powder, the addition of a binder can be used for plastic forming. In order to obtain the ideal plastic ceramic batch, it is necessary to understand the particle size distribution and accumulation of the starting powder, add an appropriate amount of forming aid, adjust the viscosity and the solid content and water content of the extruded material, and then perform appropriate extrusion molding. Degreasing and heat treatment will give you the ideal test piece. The present invention does not discuss or judge the problems of green mold forming, sintering, ceramic materials or additive components; another method is proposed specifically for the moisture conditioning treatment of general colloidal mud. 1281463 Generally, the current common powder mixing treatment, in order to make the ceramic powder / easy to shape the green embryo, usually mix the adhesive, filler, surfactant or lubricant with the dried ceramic powder, only ceramic powder and water, The method of mixing the adhesive will cause many problems, especially the extruded mud made of colloidal ceramic nano-powder. The water content is too high due to the mixing of the colloid, and the moisture control method is difficult to combine both fast and uniform. Mass production. The colloid should be produced with a considerable amount of water, that is, when the colloid is used as a forming aid, the moisture content of the mud itself can be as high as 40-60%, generally 15-20% _ is the appropriate range, and the raw water with too much water content Easy to deform and produce internal defects, resulting in difficulty in extrusion or forming defects, which have a considerable adverse effect on molding and sintering, and the mechanical properties of ceramics are sensitive to defects, so how to solve the colloid-containing ceramic slurry Moisture control problem, this is the key to the technology of using colloid as a forming aid. In view of the above problems, most of the current centrifugal concentration or pressure filtration method is used to regulate the water content of the mud material. However, the centrifugal concentration method will cause the φ alumina powder particles to settle and separate due to the difference in specific gravity, and the pressure filtration method is adopted because the colloid is fine and dehydrated. It is not easy to use, and it is not suitable for mass production. The traditional heating and drying also causes the surface of the mud to dry too fast and easily form a hard film, which makes it impossible to use. SUMMARY OF THE INVENTION Accordingly, in view of the above-mentioned defects and problems of colloidal extruded plastics, the present invention provides a method for controlling moisture in a colloid-containing extruded plastic by uniformly heating the colloid by application of microwaves. The mud material controls the amount of water, and the colloidal solution synthesized by the chemical reaction is mixed with the ceramic powder, and the concentration ratio of the desired body is adjusted by the concentration step 1281463, directly with the adhesive, the filler, the boundary surfactant or the lubrication. The agent is mixed with the moist ceramic powder. Since a large amount of liquid water is always kept between the particles, the method can eliminate the agglomeration caused by the conventional heating and drying powder, and the powder remains dispersed, so there is no problem of decondensation, excessive water is used. Microwaves are uniformly removed from the green body to achieve the purpose of controlling the water content. The invention adopts microwave heating to solve the water quantity control of the colloid-containing moist mud material, and the key is the control of the water content by using the colloid as the molding aid. The micro B wave is rapidly heated, uniformly concentrated and easy to mass-produce, and can be prepared for extrusion. The formed mud material greatly reduces the cost of industrial production. [Implementation method] This creation is a moisture control method for a colloid-containing extruded plastic. As shown in the first figure, the method is as follows: A. Slurry preparation: when preparing the slurry, using ammonia water and nitric acid as a dispersing agent, For industrial use α-Α1203 powder and boehmite (manganese hydroxide), the latter φ is a sol (sol) in an aqueous solution having a pH of about 3, and is mixed with ammonia water and nitric acid to form a dispersed slurry. B. Microwave concentration: increase the solid content of A1203 by microwave heating concentration method, reduce the water content, and put the precipitated mixed colloid into the microwave oven to dry to the appropriate moisture content. The relationship between water content and microwave time is as follows. As shown in the second figure, after the alumina slurry is concentrated one or more times, the separated slurry is taken out to obtain a high concentration (53 vol%) of the slurry, and the water content is about 18% by weight, which is in accordance with the extrusion mud. Moisture content. 1281463 (C) Mixing and Molding: The slurry is concentrated for the extrusion test. The agent is made of plastically spliced and formed by a micro-extruder. (4) After the vacuum is drawn by the pinch, the material is broken. Sintering after drying, as shown in the attached article, fine emulsified; the most extruded is characterized by: the appearance after sintering of the rubber-containing material. The problem of the concentration process of the mud material is the microwave and the moisture control of the material
均勾、快速和節能完成含水量㈣2其整體加熱特性, 和離心漠料製程。 Μ 非傳統的壓遽 在混合過程中,粉體來源可為 广也人立、功收 粉或部分來自於化學 反應&成後水料,例如在添加第二相材料時,用以強化、 幫助燒結緻密化或參與高溫反應等,亦可藉此技術達到均 勻分散第二相的要U和經過傳―合的半成品製料, 亦可再添加所需的化學反應合成後漿料,配成預設組成等 混合程序之組合,皆可在後續濃縮程序中,達到減少水分 的目的,亦即在擠出成型的粉體來源,可使用反應合成之 粉體漿料或乾燥後粉體,皆可適用。 亦即,本發明乃係應用化學反應粉體於陶瓷擠出成 型,均化擠出成型坯料技術之改良,改良習用混合之方法, 減少凝聚體,增加製程穩定性,達成一種可以均化擠出成 型坯料之目的;適合陶瓷粉末材料與黏著劑、填充劑、界 面活性劑或潤滑劑之混練步驟者。 另外,各類含膠體陶瓷泥料因材質、來源、製作參數 和品管等差異’除需要添加膠體部分,可另與黏著劑、填 1281463 •充劑或潤滑劑之配合者等,而有濃縮步驟,經過一次或多 •次微波乾燥處理之半成品,係可再施予至少黏著劑、填充 劑或潤滑劑中至少-種成分;或者,先予以至少添加黏著 劑、填充劑或满滑劑中一種成分,再續以濃縮步驟等,皆 可適用此法;即微波加熱濃縮可為含膠體潮濕陶竟泥 道製私之其中一部份。 有關將含膠體陶瓷泥料置入微波環境之方式,可為連 •續或半連續將其以輸送帶輸送,其行進持續接收微波,濃 縮完畢時,適被送離微波環境; 此外,上述微波乾燥時,可同時外加氣流將水氣吹除, 如此可節省後續乾燥的時間與能源,兼可透過視窗直接觀 察者。 又,有關將含膠體陶瓷泥料置入微波環境之方式, 為下列方式: 1·批次式:如第三圖所示,其係利用容器(1)盛裝陶瓷 • 泥料(2)分批進出於微波環境(3)中,於一定時間後將其取 出,以完成微波處理。 2·半連續式:如第四圖所示,陶瓷泥料(2)以輪送帶(4) 輸送至微波環境(3)中,其停止行進後開始微波處理,俟微 波處理完畢再由輸送帶(4)送離微波環境; 、一 3·連續式:如第五圖所示,陶瓷泥料(2)以輪送帶(4) 輸送至微波環境(3)中,其持續行進接收微波處理。 另外,凡微波頻率在微波範圍之間,並不小於微波頻 1281463 率範圍者,均可為水分吸收,而具有相同之功效。 適用的陶兗包括氧化物、氮化物、複化物、琉化物或 其化合物之任意比例混合物。 【圖式簡單說明】 第一圖係為本發明之方法步驟示意圖。 第二圖係為本發明微波時間對擠出泥料含水率之關係 不意圖。 第三圖係為本發明實施例之批次式置入示意圖。 第四圖係為本發明實施例之半連續式置入示意圖。 第五圖係為本發明實施例之連續式置入示意圖。 附件:係為本發明實施行中燒結後形成微米氧化鋁管 之相片。 【主要元件符號說明】 (1) 容器 (2) 陶瓷泥料 (3) 微波環境 (4) 輸送帶Hook, fast and energy-saving to complete the water content (4) 2 its overall heating characteristics, and centrifugal desert material process. Μ Non-traditional compression During the mixing process, the source of the powder can be broad, artificial, or partially derived from chemical reactions & after-water, for example, when adding a second phase material, To assist in sintering densification or to participate in high-temperature reaction, etc., it is also possible to achieve uniform dispersion of the second phase of the U phase and the transfer of the semi-finished product, or to add the desired chemical reaction to the synthesized slurry. The combination of the preset composition and the like can all achieve the purpose of reducing the moisture in the subsequent concentration process, that is, in the powder source of the extrusion molding, the reaction synthesis powder slurry or the dried powder can be used. applicable. That is, the present invention is an application of chemical reaction powder in ceramic extrusion molding, homogenization of extrusion molding blank technology, improvement of conventional mixing method, reduction of aggregates, increase process stability, and achieve a uniform extrusion The purpose of molding blanks; suitable for mixing steps of ceramic powder materials with adhesives, fillers, surfactants or lubricants. In addition, all kinds of colloidal ceramic mud materials differ in material, source, production parameters and quality control. In addition to the need to add colloidal parts, they can be combined with adhesives, filled with 1281463 • filler or lubricant, etc. Step, after one or more microwave drying treatments, at least one of at least one of an adhesive, a filler or a lubricant may be applied; or, at least an adhesive, a filler or a slip agent may be added first. One component, which is followed by a concentration step, etc., can be applied to this method; that is, microwave heating and concentration can be part of the manufacture of colloidal wet ceramics. The method for placing the colloidal ceramic mud into the microwave environment can be continuously or semi-continuously conveyed as a conveyor belt, and the traveling continuously receives the microwave, and when concentrated, it is sent away from the microwave environment; When drying, the air can be blown off at the same time, which saves the time and energy of subsequent drying, and can be directly observed through the window. In addition, the way to place the colloidal ceramic mud into the microwave environment is as follows: 1. Batch type: As shown in the third figure, it is made up of containers (1) containing ceramics • mud (2) batch Into the microwave environment (3), after a certain time, it is taken out to complete the microwave treatment. 2. Semi-continuous type: As shown in the fourth figure, the ceramic slurry (2) is transported to the microwave environment (3) by the belt (4). After stopping the travel, the microwave treatment is started, and the microwave treatment is completed and then transported. The belt (4) is sent away from the microwave environment; a continuous flow: as shown in the fifth figure, the ceramic slurry (2) is conveyed to the microwave environment (3) by the belt (4), which continuously travels to receive the microwave. deal with. In addition, where the microwave frequency is between the microwave range and not less than the microwave frequency of 1281463, it can absorb moisture and have the same effect. Suitable ceramics include oxides, nitrides, complexes, tellurides or mixtures thereof in any ratio. BRIEF DESCRIPTION OF THE DRAWINGS The first figure is a schematic diagram of the steps of the method of the present invention. The second figure is the relationship between the microwave time of the present invention and the moisture content of the extruded mud. The third figure is a schematic diagram of batch placement in accordance with an embodiment of the present invention. The fourth figure is a schematic diagram of semi-continuous placement of an embodiment of the present invention. The fifth drawing is a schematic diagram of the continuous placement of the embodiment of the present invention. Attachment: This is a photograph of a micron alumina tube formed after sintering in the practice of the present invention. [Explanation of main component symbols] (1) Container (2) Ceramic clay (3) Microwave environment (4) Conveyor belt