200920481 九、發明說明： 【發明所屬之技術領域】 本發明係有關於一種鍵劑型金屬蛾化物的製造方法。 【先前技術】 以碘化鉀（Potassium iodide)為代表的金屬蛾化物被 廣泛用作極化膜材料、尼龍（Nylon )穩定劑以及醫藥原料 等。該金屬碘化物通常以粉末狀銷售，因而在長期儲藏時 f % 存在以下問題。 金屬硤化物一般吸濕性較高。因此，例如如果使用透 濕性較尚的低进度聚乙烯（Polyethylene )做包裝材料來儲 . 藏金屬蛾化物粉末，則金屬蛾化物吸濕的同時，會因粉末 -自身的重量而壓密固結，因此，儲藏前粉末狀的金屬碘化 物在歲個月後會形成大塊。此外，用透濕性較低的物質代 替包裝材料時，雖能在一定程度上防止固結，但無法達到 1..；完全不固結。當金屬碘化物固結時，必須在使用它之前用 木槌4物理方法敲碎固結部分，從而降低了工作效率。 針對於此，例如在專利文獻所述的方法中提出了 以金屬碘化物為代表的金屬鹵化物（Metal halide)的固結 防止方法。 專利文獻1中公開了一種金屬鹵化物一食鹽（氣化鈉） 的固結防止方法，即對食鹽噴霧磷酸氫二鈉（Dis〇dium hydrogen phosphate )飽和溶液之後’再添加碳酸鎂 (Magnesium carbonate)粉末的方法。 200920481 專利文獻2中公開了一種金屬碘化物的乾燥制粒方 法即為了提供一種高工作效率的金屬碘化物顆粒，向流 動層噴霧造粒乾燥機中連續供給金屬碘化物的水溶液。 專利文獻3中公開了一種金屬碘化物製劑的加工方 法，即為了防止因金屬碘化物的固結和凝集而發生塊狀 化’採用壓塊輥壓（Briquettingr〇11)式的壓縮造粒方法， 將金屬峨化物加工為全體3〇%以上具有粒徑大於3麵的 造粒體。 專利文獻4中以結晶性無機化合物中的蛾化卸為例， =開了-種高溫下處理造粒品的方法。即為了提供高純度 、=固化的且具有均質強度的結晶性無機化合物，在採用 ，式壓縮造粒機對結晶性無機化合物粉末進行造粒時， 在分餘碎、篩分工序中高溫處理造粒品的造粒方法。 料=如上所述，金屬蛾化物被廣泛用作極化膜材 ，、匕龍（Nylon)穩定劑以及醫藥 :時’要求高純度的金屬•物。因此，由 了碑酸4二納及侧等添加劑而增加了雜 μ /不適合用作金屬碘化物的固結防止方法。 伯每 > 利文獻2的方法雖財—定程度㈣結防止效果， 仁只施儲藏試驗後不到—4 結防业效果並不理Γ。個月❹現了固結徵候，因此固 雖然專利文獻3的方法士名 效果，但長期儲藏德甚Γ 度上具有固結防止 & 4後產生固結’固結防止 專利文獻4的方法中，—一 / 不t个攻心 中在尚》里（60〜〗2〇t )下處理結 200920481 1 i丨ν>· 1 ττ 晶性無機化合物是必要條件，而人們知道以峨化鉀為代表 的大部分金屬碘化物會因熱或光分解為游離碘。因此表明 高溫處理會造成金屬碘化物的品質下降，專利文獻4的方 法不適合用作金屬碘化物的固結防止方法。 專利文獻1 :日本專利申請特開平成6 — 24738號公報 專利文獻2:曰本專利申請特開平成9— 156920號公 報 專利文獻3:曰本專利申請特開2004 —217467號公報 ( 專利文獻4:日本專利申請特開平成6 — 285355號公 報。 【發明内容】 ^ 因此，有鑑於此，本發明之目的在於提供一種不會發 生上述狀況，即使長期儲藏也可以充分防止固結的金屬碘 化物的製造方法。 ί 本發明人經過反復鑽研，通過在10〜50°c下將金屬碘 化物粉末壓縮成型，製成壓碎強度大於4kgf並且粒徑為 5〜20mm的錠劑型金屬碘化物的製造方法，達到了上述目 的。 通過本發明可以提供一種即使長期儲藏也可充分防 止固結的金屬碘化物的製造方法。 在本發明的製造方法中，由於錠劑的壓碎強度大於 4kgf，假定製成的錠劑投影面積為lcm2，則計算出其可承 受4kg/cm2以上的壓力。以前，將作為金屬蛾化物代表的 200920481 蛾化鉀粉末填充到35L的紙桶D晒）等中 此時在紙桶底部峨化鉀粉末由於自身重量所受到的最1壓 力約為㈣g—究這些計算結果發現，當使= 法時，由於錠劑的壓碎強度顯著大於旋劑因自 μ的壓力’所以防止了㈣自身破碎形成表面 產生的固結。 及料者吸濕 在本發明的製造方法中，通過在lo〜5(rc壓縮成型金 =:=’防止了游離硪的產生，從而可以防止金屬 破化物的純度下降。 此外二本發明的製造方法中’由於錠劑的粒徑大於 mm，因此可以防止在粒徑小於5_時產生的不良狀兄。 即，當粒控小於5麵時，如果使用打旋機進 π=:τ成反比例增加而導致初期丄 大’會因粒子變細而導致每小時的生 大™防止在總成本(_:=:h因此粒， +產生的問題等傾向。此外’在本發明的製造方:n中dlm: ^錠劑^^、於2Gmm，因此還可以防止在粒徑超過 l=fi 產品。即，當粒捏超過加_時， 使至屬埃化物溶解在溶劑中需要較長的時間，因 於20mm可防止工作效率下降等不良狀況的發生… 在本發明的製造方法中，較佳地是翻ς式壓縮造粒 機進行上㈣㈣型。纽可進—步提高上述固結防土效 果0 200920481 在本發明的製造方法中，上述壓縮成型過程中的打錠 壓力較佳地為1〜20kN。由此可進一步提高上述固結防止效 果。 在本發明的製造方法中，金屬職化物較較佳地是驗金 屬埃化物或者驗土金屬破化物。 本發明提供了一種即使長期儲藏也可以充分防止固 結的金屬碘化物的製造方法。此外由於採用本發明的製造 方法所得到的金屬碘化物是錠劑，因此沒有粉塵飛揚，對 使用者來說跨越性的改善了其操作性，從而可以更容易操 作。 為讓本發明之上述内容能更明顯易懂，下文特舉較佳 之實施例，並配合所附圖式，作詳細說明如下： 【實施方式】 以下對本發明的較佳實施例進行詳細的說明，但本發 明並非僅限於此。 本發明的製造方法，例如可以使用職化經、議化鈉、 礎化鉀、峨化伽、蛾化铯等驗金屬蛾化物，使用雄化|丐、 碘化勰等鹼土金屬碘化物，以及碘化鋁等金屬碘化物。其 中，較佳地可以使用適合本發明製造方法的鹼金屬碘化物 及鹼土金屬碘化物，更佳地是使用更適合本發明製造方法 的蛾化鉀。 在本發明製造方法中使用的金屬碘化物粉末，不包含 基本的水及固結防止劑等雜質，但可以混入少量雜質。此 200920481 外，作為金屬碘化物粉末，較佳地是，可以使用結晶乾燥 品的粉末，由流動乾燥機乾燥，使用粒徑均為1000/im以 下的粉末。 本發明製造方法中壓縮成型時的溫度為10〜50°C，較 佳地是10〜40°C，更較佳地是常溫（15〜25°C )。 在本發明的製造方法中例如可使用幹式壓縮造粒機 進行壓縮成型。幹式壓縮造粒機大體上分為壓縮輥壓式、 壓塊輥壓式以及打錠式三類，其中較佳地是打錠式（打錠 機）。打鍵機大致可分為單髮式離心（eccentric )型和旋轉 (rotary )型，其中較佳地是旋轉型打敍:機。使用旋轉型打 錠機時，操作轉子旋轉數為30〜60rpm，以1〜10KN (千牛 頓、Kilo Newton )的打鍵壓力進行打鍵：。通過這種旋轉型 打錠機每小時可生產100〜500kg的錠劑。 使用打錠式的幹式壓縮造粒機進行上述壓縮成型時 的打錠壓力，較佳地是1〜20kN，更佳地是3〜15kN。 本發明製造方法中的錠劑型金屬碘化物的壓碎強度 為4kgf。此外，沒有特別限定壓碎強度的上限，但例如可 以在30kgf以下。 本發明製造方法中的鍵劑型金屬峨化物的粒徑為 5〜20mm，較佳地是7〜15mm。 本發明的製造方法特徵在於將金屬碘化物粉末在 10〜50°C壓縮成型、加工為壓碎強度大於4kgf並且粒徑為 5〜20mm的錠劑，並且還提供一種金屬碘化物的固結防止 方法。 10 200920481 KHT〜20N。 以下’對本發明的實施例進行進一步的詳細說明，但 本發明並非僅㈣此。科，壓碎強㈣枝賴原㈣ 股份有限公司所製造的木屋式數位（咖 第一實施例 將使用流動乾燥機製造的粒徑1000/zm以下（平均粒 佐250# m)的峨化鉀原料粉末，在常溫下使用旋轉型打鍵 機打鍵成型製成粒;^為9mm岐劑。旋轉型打旋機的打旋 [力為3 5KN ’為了不引起頂裂（）以及粉末在 杵及臼上的黏著，並且考慮了成型速度後，將轉子的旋轉 數的最適條件&定$ 5Qi<pm。得到的錠劑壓碎強度約為 5e〜7kgf。得到的錠劑照片如附圖1所示。此外，“頂裂” 是心鍵劑的一部分黏著在打錠式壓縮造粒機的臼及杵 上，該黏著部分為帽子形狀的剝離現象。 第二實施例 除了打錠壓力為1〜1.7KN以外’製造錠劑的方法與第 實施例相同。得到的錠劑壓碎強度約為6〜lOkgf。此外， 旋劑製造中不引起頂裂以及粉末在杵及臼上的黏著。 第一對比例 將使用流動乾燥機製造的粒徑為小於1000//m的碘化 钟原料粉末’通過壓塊輥壓方式的壓縮式造粒機進行造200920481 IX. Description of the Invention: [Technical Field to Be Invented by the Invention] The present invention relates to a method for producing a key type metal moth compound. [Prior Art] Metal moth compounds typified by Potassium iodide are widely used as a polarizing film material, a nylon (Nylon) stabilizer, and a pharmaceutical raw material. The metal iodide is usually sold in the form of a powder, so that the following problems occur in the case of long-term storage. Metal halides are generally more hygroscopic. Therefore, for example, if a low-permeability polyethylene (Polyethylene) is used as a packaging material to store the metal moth powder, the metal moth compound absorbs moisture and is compacted by the weight of the powder itself. Therefore, the powdered metal iodide will form a large mass after the age of storage. In addition, when the packaging material is replaced by a material having a low moisture permeability, although the consolidation can be prevented to some extent, it cannot be achieved until 1..; it is not consolidated at all. When the metal iodide is consolidated, the consolidated portion must be broken by the raft 4 physical method before using it, thereby reducing work efficiency. In response to this, for example, a method of preventing the consolidation of a metal halide typified by a metal iodide has been proposed in the method described in the patent document. Patent Document 1 discloses a method for preventing consolidation of a metal halide-salt salt (sodium hydride), that is, after adding a saturated solution of Dis dium hydrogen phosphate to a salt, 'addition of magnesium carbonate (Magnesium carbonate) Powder method. 200920481 Patent Document 2 discloses a dry granulation method of metal iodide, that is, in order to provide a metal oxide iodide particle having high work efficiency, an aqueous solution of a metal iodide is continuously supplied to a fluidized layer spray granulation dryer. Patent Document 3 discloses a method for processing a metal iodide preparation, that is, a block granulation method for preventing consolidation and aggregation of metal iodide, and a compression granulation method using a briquetting roll press method. The metal telluride is processed into granules having a particle diameter of more than 3 faces in an overall amount of 3% by mole or more. In Patent Document 4, a method of treating a granulated product at a high temperature is exemplified by moth removal in a crystalline inorganic compound. That is, in order to provide a crystalline inorganic compound having high purity, solidification, and homogeneity, when a crystalline inorganic compound powder is granulated by a compression granulator, it is subjected to high-temperature treatment in a fractionation and sieving process. Granulation method of granules. Material = As described above, metal moth compounds are widely used as polarizing film materials, Nylon stabilizers, and pharmaceuticals: when high-purity metals are required. Therefore, a method of preventing the solidification of the metal iodide by the addition of the impurity μ 4 / the additive such as the side acid is added. The method of Bog > Li Wen 2, although the financial-fixed degree (four) knot prevention effect, the effect of the anti-industry effect of the Ren-only storage test is not ignored. In the case of the consolidation of the patent document 3, the method of the patent document 3 has a solid effect, but the long-term storage has a consolidation prevention & , - a / not t attack in the heart in the "Shang" (60 ~ 〗 2 〇 t) under the treatment of 200920481 1 i丨ν> 1 ττ crystalline inorganic compounds are necessary conditions, and people know that represented by potassium telluride Most of the metal iodide is decomposed into free iodine by heat or light. Therefore, it has been revealed that the high-temperature treatment causes a deterioration in the quality of the metal iodide, and the method of Patent Document 4 is not suitable as a method for preventing the consolidation of the metal iodide. [Patent Document 1] Japanese Patent Application Laid-Open No. Hei. No. Hei. No. Hei. No. Hei. No. Hei. No. Hei. No. Hei. In the light of the above, it is an object of the present invention to provide a metal iodide which can prevent the consolidation from occurring even if it is stored for a long period of time without causing the above-mentioned situation. The present inventors have repeatedly studied to produce a tablet-type metal iodide having a crushing strength of more than 4 kgf and a particle diameter of 5 to 20 mm by compression molding a metal iodide powder at 10 to 50 ° C. According to the present invention, it is possible to provide a method for producing a metal iodide which can sufficiently prevent consolidation even after long-term storage. In the production method of the present invention, since the crushing strength of the tablet is more than 4 kgf, assuming The projected area of the tablet is 1cm2, and it can be calculated to withstand a pressure of 4kg/cm2 or more. Previously, it will be represented as a metal moth compound. 200920481 Potassium moth potassium powder is filled into 35L paper drum D. In this case, the maximum pressure of potassium telluride powder at the bottom of the paper barrel due to its own weight is about (4) g. These calculations show that when the = method is used Since the crushing strength of the tablet is significantly larger than the pressure of the spinner due to the μ, the (4) self-crushing is prevented from forming a surface to form a consolidation. In the manufacturing method of the present invention, the purity of the metal-breaking compound can be prevented from being lowered by preventing the generation of free ruthenium in lo~5 (rc compression molding gold =:='). In the method, 'Because the particle size of the tablet is larger than mm, it can prevent the bad brother produced when the particle size is less than 5_. That is, when the grain control is less than 5 faces, if the swirler is used, the π=:τ is inversely proportional. The increase will cause the initial large size to be caused by the finening of the particles, resulting in the prevention of the total cost per hour (_:=:h, therefore the grain, the problem of production, etc.. In addition, the manufacturer of the invention: n In the dlm: ^ lozenge ^ ^, in 2Gmm, it can also prevent the product in the particle size exceeding l = fi. That is, when the pellet is more than the addition of _, it takes a long time to dissolve the genus into the solvent. In the manufacturing method of the present invention, it is preferable that the turning type compression granulator performs the upper (four) (four) type. The New Zealand can further improve the above-mentioned consolidated soil-proof effect. 0 200920481 In the manufacturing method of the present invention, the above compression molding The tableting pressure in the process is preferably from 1 to 20 kN, whereby the above-mentioned consolidation preventing effect can be further improved. In the manufacturing method of the present invention, the metal compound is preferably a metal oxide or a soil-measuring metal. The present invention provides a method for producing a metal iodide which can sufficiently prevent solidification even after long-term storage. Further, since the metal iodide obtained by the production method of the present invention is a tablet, there is no dust flying to the user. In order to make the above-mentioned contents of the present invention more obvious and easy to understand, the following description of the preferred embodiments and the accompanying drawings are described in detail below: BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, preferred embodiments of the present invention will be described in detail, but the present invention is not limited thereto. For the production method of the present invention, for example, it is possible to use a chemical, a sodium, a chemical, or a potassium hydride. The metal moth compound such as moth and phlegm is used, and an alkaline earth metal iodide such as male, bismuth, or cesium iodide, and a metal iodide such as aluminum iodide are used. An alkali metal iodide and an alkaline earth metal iodide suitable for the production method of the present invention can be used, and it is more preferred to use potassium molybdate which is more suitable for the production method of the present invention. The metal iodide powder used in the production method of the present invention does not contain basic As the metal iodide powder, it is preferable to use a powder of a crystal dried product, which is dried by a flow dryer, and the particle diameter is used. Powder of 1000/im or less. The temperature at the time of compression molding in the production method of the present invention is 10 to 50 ° C, preferably 10 to 40 ° C, and more preferably normal temperature (15 to 25 ° C). In the manufacturing method of the invention, for example, a dry compression granulator can be used for compression molding. The dry compression granulator is generally classified into a compression roll type, a compact roll type, and a tablet type, and among them, preferably Ingot type (ingot machine). The keying machine can be roughly classified into an eccentric type and a rotary type, and preferably a rotary type: a machine. When using a rotary type ingot machine, the number of rotations of the operating rotor is 30 to 60 rpm, and the key is pressed with a keying pressure of 1 to 10 KN (Kilton Newton, Kilo Newton). A tablet of 100 to 500 kg per hour can be produced by this rotary type ingot machine. The tableting pressure at the time of the above compression molding using a bar-type dry compression granulator is preferably 1 to 20 kN, more preferably 3 to 15 kN. The tablet type metal iodide in the production method of the present invention has a crush strength of 4 kgf. Further, the upper limit of the crushing strength is not particularly limited, but may be, for example, 30 kgf or less. The particle type metal halide in the production method of the present invention has a particle diameter of 5 to 20 mm, preferably 7 to 15 mm. The manufacturing method of the present invention is characterized in that the metal iodide powder is compression-molded at 10 to 50 ° C, processed into a tablet having a crushing strength of more than 4 kgf and a particle diameter of 5 to 20 mm, and also provides a metal iodide consolidation prevention. method. 10 200920481 KHT~20N. The embodiments of the present invention are described in further detail below, but the present invention is not limited to only (4). Branch, crushed strong (four) Zhi Laiyuan (four) Co., Ltd. made by the wooden house type digital (the first embodiment of the coffee will use a flow dryer to produce potassium telluride with a particle size of 1000 / zm or less (average grain 250# m) The raw material powder is formed into a pellet by a keying machine at a normal temperature using a rotary type keying machine; ^ is a 9 mm tincture. The spinning of the rotary type rotary machine [force is 3 5KN 'in order not to cause a top crack () and the powder is in the crucible and the crucible After the adhesion, and considering the molding speed, the optimum condition of the number of rotations of the rotor is set to $5Qi < pm. The obtained tablet has a crushing strength of about 5e to 7kgf. The obtained tablet is as shown in Fig. 1. In addition, the "top crack" is a part of the core bond adhered to the crucible and the crucible of the tablet-type compression granulator, and the adhesive portion is a peeling phenomenon of a hat shape. The second embodiment has a pinch pressure of 1~. The method for producing a tablet is the same as that of the first embodiment except for 1.7 KN. The obtained tablet has a crushing strength of about 6 to 10 kgf. Further, the spinner is produced without causing cracking and adhesion of the powder to the crucible and the crucible. The comparative example will be made using a flow dryer with a small particle size Iodide powder raw clock 1000 // m 'of a compression type be made by briquetting roll pelletizer embodiment
II 200920481 粒。在造粒時，壓縮式造粒機的輥壓壓力約為5MPa，同 時旋轉報壓袋（pocket)變為煤球狀、杏仁狀（Almond) 等各種形狀，從而製造各種形狀的造粒體。 但是無論哪種情況得到的造粒體，都易引起分層 (lamination )從而不能形成整齊的塊劑（briquette )型。 • 此外，由於得到的造粒體以薄的部分相連接的形狀被排 出，其薄的部分或是被分割破碎，或是成為粉末混入造粒 體中（推測像這樣不能很好成型的造粒體的比例是 20%〜30%)。因此，不能進行後述儲藏狀態的評價等試驗。 此外，“分層”是指錠劑剝離、分割為層狀的現象。 第二對比例 準備與實施例1中使用的碘化鉀原料粉末相同的、使 用流動乾燥機製造的粒徑小於1000// m (平均粒徑250// m)的埃化鉀粉末。 ί \， 錠劑物理性質的評價 針對實施例1及2的錠劑的表面積、粒子密度、比表 面積、體積密度（Bulk density)以及壓碎強度進行評價。 此外，對作為比較物件的對比例2中粉末的表面積、粒子 密度、比表面積以及體積密度也進行了評價。結果如表1 所示。並且，表1中為了求算表面積，以對比例2的粒子 密度為真密度。此外，表面積、粒子密度、比表面積以及 體積密度按照以下方式求算。 12 200920481 :卜貫施例…成型的鍵劑中取出丨 出其料以及表面積，同時岐重量。比表面積是由^ 面積的值除以重量值計算出的，粒子密度是由重量= 體積值計算出的。 街里里值除μ 此外，由於對比例2的粉末具有粒度分佈的性質 不能用上述方法求算粒子密度等。因此，除了㈣子 粉末的粉末粒度分佈之外，料分麻算粒彳f作為正球形 的表面積、體積，通料些㈣及上述真密度求算比表面 實施例1及2旋劑的體積密度是通過將錠劑放入 250mL量筒内測定重量，再用該重量除以體積求算出的。 此外’對比例2粉末的體積密度通過同樣的操作使用 100mL量筒進行計算。 _ 實施例1 實施例2 對比例2 表面積（cm2) 3.61 3.85 134 粒子密度（g/cm3) 2.76 2.62 3.13 (真密度） 比表面積（cm2/g ) 2.30 2.36 307 體積密度（g/cm3) 2.02 1.95 1.98 壓碎強度（kgf) 約5〜7 約6〜10 - 表1 表1結果顯示，與對比例2的粉末比較，實施例1和 2旋劑的比表面積非常小。因此，可以很容易想像減小了 固結問題的間接原因是吸濕性。此外，實施例1和2紅劑 13 200920481 的體積密度與對比例2粉末的體積密度值幾乎相同。因此 表明可以使用與包裝對比例2粉末的以往包裝材料相同的 包裝材料來包裝實施例1和2的錠劑。 錠劑的防止固結性的評價 針對實施例1的旋劑以及對比例2的粉末，採用以下 方法進行了儲藏狀態的評價。 用塑膠袋包裝實施例1的旋劑，將包裝後的旋 劑在500Φ的l〇〇L柔性集裝袋（Fiec〇n)(注冊商標）中 儲藏一個月，目測觀察固結的發生。儲藏後的錠劑與包裝 前幾乎沒有變化，完全沒有固結。而對比例2的粉末用紙 板箱（Cardboard)包裝一個月後’粉末沿紙板箱的形狀固 έ士。 、、、口 鍵劑溶解特性的評價1 ( 針對實施例1的錠劑，採用以下方法進行了溶解特性 的評價。 準備兩個1L的燒杯（Beaker)，向各燒杯中加入5漏 離子交換水，—邊分卿磁力難ϋ (magnetie sti贿） =12〇〜l5〇rpm的速度進行麟’一邊加入上述樣品 溶液溫度為4G°C或25ΐ時分 "口 溫度為紙_ σ^ f彳貝n解時間。溶液 S。此外，溶解時間是指 入 f樣口口篁為 具體講是指投入樣口徭s ，〇口凡王，合解所需的時間， 後至=確認沒有固體存在為止的時 200920481 間。得到的結果如表2所示II 200920481 Grain. At the time of granulation, the compression granulator has a roll pressure of about 5 MPa, and at the same time, the pocket is rotated into various shapes such as briquettes or almonds to produce granules of various shapes. However, the granules obtained in any case are liable to cause lamination and thus cannot form a neat block type. • In addition, since the obtained granules are discharged in a shape in which thin portions are connected, the thin portions are either divided and broken, or are mixed into the granules (presumably granulated which is not well formed like this) The ratio of the body is 20% to 30%). Therefore, tests such as evaluation of the storage state described later cannot be performed. Further, "layering" refers to a phenomenon in which a tablet is peeled off and divided into layers. Second Comparative Example An potassium silicate powder having a particle diameter of less than 1000 / / m (average particle diameter of 250 / / m) manufactured by using a flow dryer was prepared in the same manner as the potassium iodide raw material powder used in Example 1. ί \, Evaluation of Physical Properties of Tablets The surface areas, particle density, specific surface area, Bulk density, and crush strength of the tablets of Examples 1 and 2 were evaluated. Further, the surface area, particle density, specific surface area, and bulk density of the powder in Comparative Example 2 as a comparative article were also evaluated. The results are shown in Table 1. Further, in Table 1, in order to calculate the surface area, the particle density of Comparative Example 2 was taken as the true density. Further, the surface area, particle density, specific surface area, and bulk density were calculated in the following manner. 12 200920481 : Bu ping application... The formed key is taken out of the material and the surface area, while the weight is 岐. The specific surface area is calculated by dividing the value of the area by the weight value, which is calculated from the weight = volume value. In addition, since the powder of Comparative Example 2 has a particle size distribution property, the particle density and the like cannot be calculated by the above method. Therefore, in addition to the powder particle size distribution of the (iv) sub-powder, the material is divided into the surface area and volume of the spherical shape, and the bulk density of the surface examples 1 and 2 is calculated. The weight was determined by placing the tablet in a 250 mL graduated cylinder and dividing the weight by the volume. Further, the bulk density of the powder of Comparative Example 2 was calculated by the same operation using a 100 mL graduated cylinder. _ Example 1 Example 2 Comparative Example 2 Surface area (cm2) 3.61 3.85 134 Particle density (g/cm3) 2.76 2.62 3.13 (true density) specific surface area (cm2/g) 2.30 2.36 307 Bulk density (g/cm3) 2.02 1.95 1.98 Crush strength (kgf) about 5 to 7 about 6 to 10 - Table 1 The results of Table 1 show that the specific surface areas of the examples 1 and 2 are much smaller than those of the powder of Comparative Example 2. Therefore, it can be easily imagined that the indirect cause of the reduction in the consolidation problem is hygroscopicity. Further, the bulk density of Examples 1 and 2 Red Agent 13 200920481 was almost the same as the volume density value of Comparative Example 2 powder. It is thus indicated that the tablets of Examples 1 and 2 can be packaged using the same packaging materials as the conventional packaging materials of Comparative Example 2 powder. Evaluation of Prevention of Consolidation of Tablets The powders of Example 1 and the powder of Comparative Example 2 were evaluated for storage in the following manner. The spinning agent of Example 1 was wrapped in a plastic bag, and the packaged toner was stored in a 500 Φ l〇〇L flexible container (Fiec〇n) (registered trademark) for one month, and the occurrence of consolidation was visually observed. The stored tablets were almost unchanged from the package and were completely unconsolidated. While the powder of Comparative Example 2 was packaged in a cardboard box for one month, the powder was solidified in the shape of the cardboard box. Evaluation of dissolution characteristics of the keying agent 1 (Evaluation of the dissolution characteristics was carried out by the following method for the tablet of Example 1. Two 1 L beakers were prepared, and 5 leak-exchanged water was added to each beaker. , - Bianqing magnetic difficulty (magnetie sti bribe) = 12 〇 ~ l5 〇 rpm speed Lin's side of the above sample solution temperature is 4G ° C or 25 ΐ ° ° ° mouth temperature for paper _ σ ^ f彳The solution time is S. In addition, the dissolution time refers to the mouth of the f-type mouth. Specifically, it refers to the time of the input sample 徭s, 〇口凡王, the time required for the solution, and then to confirm that no solid exists. The time between 200920481. The results obtained are shown in Table 2.
表2結果表明，在溶液溫度分別為4 01：及2 5 的條 件下，貫施例1的錠劑顯示出充分的溶解特性。 第三〜第七實施例 當鍵劑的粒徑分別為5.0、7.〇、9 〇、115、15 〇咖時， 打錠壓力為3kN，在其他條件與實施例}相同的條件下製 造實施例3〜7的碘化鉀錠劑。採用上述“錠劑物理性質的 評偏方法，计算制得錠劑的表面積、粒子密度、比表面 積、體積饴度等。結果如表3所示。並且，當旋劑粒徑為 9.0mm時，將打錠壓力變化為3、5、8kN進行錠劑製造…， 也沒有發現錠劑物理性質有特別明顯的變化。 ---- -- ------- 實施例 3 實施例4 實施例5 實施例6 實施例 7 15 200920481 錠劑的粒徑（mm ) 錠劑的高度（mm ) 表面積（cm2 ) 比表面積（cm2/g) 體積 #X(g/Cm3) 0.86 0.247 0.081 1.02 4.13 3.03The results in Table 2 show that the tablet of Example 1 showed sufficient solubility characteristics under the conditions of solution temperatures of 4 01: and 2 5 , respectively. In the third to seventh embodiments, when the particle diameters of the bonding agents were 5.0, 7., 9 〇, 115, and 15 Å, respectively, the tableting pressure was 3 kN, and other conditions were carried out under the same conditions as in Example}. Potassium iodide tablets of Examples 3 to 7. The surface area, particle density, specific surface area, volume twist, etc. of the obtained tablet were calculated by the above-mentioned "softening method of the physical properties of the tablet". The results are shown in Table 3. And, when the particle diameter of the spinner is 9.0 mm, The tableting pressure was changed to 3, 5, and 8 kN for tablet production... and no significant change in the physical properties of the tablet was observed. ----------- Example 3 Example 4 Implementation Example 5 Example 6 Example 7 15 200920481 Particle size of the tablet (mm) Height of the tablet (mm) Surface area (cm2) Specific surface area (cm2/g) Volume #X(g/Cm3) 0.86 0.247 0.081 1.02 4.13 3.03
>20 高度/粒徑 平均重量（g/錠） 每l〇g的錠劑個 數 體積（cm3) 壓碎強度（kgf) 錠劑溶解特性的評價2 針對實施例3〜7的鍵劑’採用以下方法進行了溶解特 性的評價。 在20〜100„11的容器中，通過調整錠劑個數及水溶液 :量’從而使“鍵劑重量/水重量，’的值約為5 4w/v%，同 ^7整Λ子^^轉數使其符合_大小，在溶液溫度為 C的條件下測定至鍵劑完全 間）。其結果如表4所示。 奋解所需時間（溶解時 霣施例3 ----->. 實施例4 實施例5 實施例6 實 2 1 - —_Li ' 9.0 —---- 1 O r ~~~^~~ 1 1 ~~----- X . D ~~~------ 29.3 K 7^0^ 5.49 5.42 ----- 5.47 5.43 -—---_ 5.45 量（w/v% ) 16 200920481 溶解時間（sec) 130 -'—1 165 ---- 197 145 199 表4 ·* ! 此外，錠劑粒徑與溶解度的關係，以及錠劑粒徑與錠 劑高度的關係分別如附圖2所示 练上所述，雖然本發明已以較佳之實施例揭露如上， 然其並非用錄定本發明。本發料屬技㈣域巾具有通 ，在我離本發明之精神和_内，#可作 。因此，本發明之保護範圍當視後 寻利乾圍所界定者為準。 τ月>20 Height/particle size average weight (g/ingot) Number of tablets per 1 〇g (cm3) Crush strength (kgf) Evaluation of dissolution characteristics of tablets 2 Key agents for Examples 3 to 7 The dissolution characteristics were evaluated by the following methods. In the container of 20~100„11, by adjusting the number of tablets and the amount of the aqueous solution: the amount of 'key agent weight/water weight,' is about 5 4w/v%, the same as ^7 whole tweezers ^^ The number of revolutions is such that it conforms to the _ size and is measured to the full extent of the bond at a solution temperature of C). The results are shown in Table 4. Time required for dissolving (in the case of dissolution, Example 3 ----->. Example 4 Example 5 Example 6 Real 2 1 - —Li ' 9.0 —---- 1 O r ~~~^~ ~ 1 1 ~~----- X . D ~~~------ 29.3 K 7^0^ 5.49 5.42 ----- 5.47 5.43 -----_ 5.45 Quantity (w/v% 16 200920481 Dissolution time (sec) 130 -'-1 165 ---- 197 145 199 Table 4 ·* ! In addition, the relationship between the particle size and solubility of the tablet, and the relationship between the particle size of the tablet and the height of the tablet are as follows: The invention has been described above with reference to the accompanying drawings, although the invention has been disclosed above in the preferred embodiments, which are not intended to illustrate the invention. The present invention belongs to the art (4) domain towel having a pass, and I am away from the spirit of the present invention. Therefore, #可作. Therefore, the scope of protection of the present invention is subject to the definition of the latter.
17 200920481 【圖式簡單說明】 益 、 <、、、 【主要元件符號說明】17 200920481 [Simple description of the schema] Benefits, <,,, [Description of main component symbols]