JPS6168133A - Granulating method - Google Patents

Abstract

PURPOSE:To obtain efficiently granules of various grain sizes by charging powder to be granulated and a powder binder into a hermetic tank, mixing uniformly, reducing the inside pressure of the hermetic vessel, spraying a solvent, granulating the powder, and drying the granules. CONSTITUTION:Powder to be granulated and a powder binder are charged into a hermetic tank 1, and mixed uniformly. The pressure in the tank 1 is reduced by a vacuum mechanism 2 to vacuum, and a solvent is sprayed by a solvent spray mechanism 3 to granulate the powder. The obtained granules are dried. By continuing said mixing and drying for an appropriate time, the granules are stabilized. The grain size of the granules can be optionally controlled with high precision by selecting the kind of powder binder and solvent, the spraying and mixing conditions, the temps., and the pressure reducing conditions. This method contributes to the omission of a binder dissolution stage, the reduction of the amt. of the solvent to be used, the reduction of time for the drying stage, and efficient operability, and the design of grain size, etc. can be facilitated.

Description

【発明の詳細な説明】 〈発明の技術分野〉 本発明は、諸々粉粒体工業において実施する造粒方法に
関する。DETAILED DESCRIPTION OF THE INVENTION Technical Field of the Invention The present invention relates to a granulation method implemented in various powder and granule industries.

〈発明の背景〉 従来、造粒には種々方法が実施されているが、その一つ
として、バインダーを含む溶液を造粒しようとする粉体
に対して噴霧し、造粒する方法がある。しかし、上記方
法の場合、バインダーを溶解させる作業に手数、時間を
要す。しかも、溶液の濃度が低い場合は溶液量の増大の
ため乾燥に多大のエネルギーを要し、逆に、溶液の濃度
が高い場合は粘性が増して作業性がわるくなり品質低下
等の問題がある。<Background of the Invention> Conventionally, various methods have been used for granulation, one of which is a method in which a solution containing a binder is sprayed onto the powder to be granulated. However, in the case of the above method, it takes time and effort to dissolve the binder. Moreover, if the concentration of the solution is low, a large amount of energy is required for drying due to the increase in the amount of solution, and conversely, if the concentration of the solution is high, the viscosity increases, which reduces workability and causes problems such as quality deterioration. .

〈発明の目的〉 本発明は上記の問題に鑑み、バインダー溶解工程の省略
、溶媒使用量の削減、乾燥工程の短縮等効率的作業性に
寄与し且つ粒度設計の容易化等を実現する。また使用し
た溶媒を耐層して再利用することにより更に資源の節減
に効果を発揮することもできる新規な造粒方法を提供す
ることを目的とする。<Object of the Invention> In view of the above problems, the present invention contributes to efficient workability such as omitting the binder dissolving step, reducing the amount of solvent used, and shortening the drying step, and also realizes ease of particle size design. Another object of the present invention is to provide a new granulation method that can further reduce resources by reusing the used solvent.

〈発明の構成および効果〉 上記目的を達成するため、本発明では、造粒しようとす
る粉体と粉末バインダーとを密閉タンクへ収容して均一
に混合し、密閉タンク内を真空および乾燥状態となし、
斯る真空条件下の粉体、粉末バインダー混合物に対し溶
媒を噴霧して造粒する方法を採用した。斯くなる方法に
よると、特に、真空条件下で噴霧された溶媒は、同条件
下の粉体、粉末バインダー混合物に瞬時に拡散浸透し、
粉体の適当数が凝集して顆粒を形成する。噴霧終了後、
適当時間に亘り混合および乾燥工程を継続することによ
り、造粒品として安定化し発明目的を達成した所期の効
果を奏する。<Structure and Effects of the Invention> In order to achieve the above object, in the present invention, the powder to be granulated and the powder binder are placed in a closed tank and mixed uniformly, and the inside of the closed tank is kept in a vacuum and dry state. none,
A method of granulating the powder and powder binder mixture under such vacuum conditions by spraying a solvent was adopted. According to this method, in particular, the solvent sprayed under vacuum conditions instantly diffuses and permeates into the powder and powder binder mixture under the same conditions.
A suitable number of powders agglomerate to form granules. After spraying,
By continuing the mixing and drying steps for an appropriate period of time, the granulated product is stabilized and achieves the desired effect of achieving the purpose of the invention.

〈実施例の説明〉 図面は本発明の方法の実施に適用する装置の全体概略図
を示す。DESCRIPTION OF THE PREFERRED EMBODIMENTS The drawings show an overall schematic diagram of an apparatus adapted for carrying out the method of the invention.

上記装置は、前面にハツチ型開閉扉１１を有し内面にバ
ッフルと称する混合羽根が配備された密閉タンク１に対
し、密閉タンク１の回転支軸１２中を導通してタンク内
に連通した減圧機構２および溶媒噴霧機構３を連繋配備
してなる。The above device consists of a sealed tank 1 having a hatch-shaped opening/closing door 11 on the front side and a mixing vane called a baffle on the inside, and a reduced pressure connected to the inside of the tank by conducting through a rotating shaft 12 of the sealed tank 1. The mechanism 2 and the solvent spray mechanism 3 are connected and arranged.

前記密閉タンク１は、回転駆動装置（図示せず）に連繋
して回転すると共に、タンク周壁および混合羽根を二重
構造となして一連の通路を形成し、温水等の加熱媒体を
流通してタンク内を加熱乾燥するようになしている。The sealed tank 1 rotates in conjunction with a rotary drive device (not shown), and has a double structure of the tank peripheral wall and mixing blades to form a series of passages through which a heating medium such as hot water is circulated. The inside of the tank is heated and dried.

威圧機構２は、タンク１中へ導入された通気管２１の一
端にフィルタ２２を取付け、通気管２１の他端にコール
ドトラップ２３を接続すると共に、該ゴールドトラップ
２３の排気口を、管軸上にダストフィルタ２４、弁２５
を有す排気管２６を介して真空ポンプ２７に接続してい
る。The intimidation mechanism 2 attaches a filter 22 to one end of a vent pipe 21 introduced into the tank 1, connects a cold trap 23 to the other end of the vent pipe 21, and connects the exhaust port of the gold trap 23 to the top of the pipe axis. Dust filter 24, valve 25
It is connected to a vacuum pump 27 via an exhaust pipe 26 having a.

溶媒噴霧機構３は、前記ゴールドトラップの液排出口を
、管軸上に溶媒補給タンク３１、ポンプ３２を有す給液
管３３を接続し、該給液管３３の先端を密閉タンク１中
へ導入して口径、方向可変噴霧ノズル３４を取付けてお
り、密閉タンク１中へ一定量の粉体および粉末バインダ
ーを収容し、これをタンクの回転により混合し、減圧機
構２を作動して粉体、粉末バインダーを含むタンク１内
を真空状態となした後、噴Ｍ機構３を作動して真空条件
下のタンク１内へ溶媒を噴霧する。噴霧された溶媒は、
同真空条件下の粉体、粉末バインダーに対し瞬時に拡散
浸透し、浸透後直ちに粉末バインダーを溶解して隣接粉
体間を一体結合し、造粒化する。このとき、密閉タンク
１中は真空、且つ、加熱乾燥状態を呈しており、噴霧さ
れた溶媒は粉体造粒に機能の後、直ちに気化して吸気管
２１よりゴールドトラップ２３に流入回収され、混合お
よび乾燥を適当時間に亘り継続することにより、造粒品
として安定化する。造粒品の粒度は、粉末バインダーお
よび溶媒の選択または溶媒噴霧の条件の選定、或いは、
噴霧工程と混合条件並びに温度、減圧条件の選定に゛よ
って任意レベルに且つ高精度に制御できる。以下本発明
の実施例を比較例と対照して示すが、本発明は該実施例
に限定されない。The solvent spraying mechanism 3 connects the liquid outlet of the gold trap to a liquid supply pipe 33 having a solvent replenishment tank 31 and a pump 32 on the pipe axis, and inserts the tip of the liquid supply pipe 33 into the closed tank 1. A spray nozzle 34 with a variable diameter and direction is installed, and a fixed amount of powder and powder binder are placed in the closed tank 1, mixed by the rotation of the tank, and the pressure reducing mechanism 2 is activated to release the powder. After the inside of the tank 1 containing the powder binder is brought into a vacuum state, the spray M mechanism 3 is operated to spray the solvent into the tank 1 under the vacuum condition. The sprayed solvent is
Under the same vacuum conditions, the powder instantly diffuses and permeates into the powder binder, and immediately after permeation, the powder binder is dissolved, adjacent powders are integrally bonded, and granulated. At this time, the inside of the closed tank 1 is in a vacuum and heated drying state, and the sprayed solvent functions to granulate the powder, then immediately vaporizes, flows into the gold trap 23 from the intake pipe 21, and is collected. By continuing mixing and drying for an appropriate period of time, the granulated product is stabilized. The particle size of the granulated product is determined by the selection of the powder binder and solvent, the selection of solvent spray conditions, or
By selecting the spraying process, mixing conditions, temperature, and pressure reduction conditions, it can be controlled to any desired level and with high precision. Examples of the present invention will be shown below in comparison with comparative examples, but the present invention is not limited to these Examples.

実施例 粉体として、トリクロルメチアジド０．２　Ｋ９、乳糖
５　Ｋ９、トウモロコシ澱粉２．２４　Ｋｇ、結晶セル
ロース（アビセルＰＨ１０１、旭化成製）２．２５に７
の合計９．９５　Ｋ９を秤取して、これを粉体処理装置
に投入した。この装置の内部を減圧状態および５０　’
Ｃに保ち、装置本体を５　ｒ、ｐｏｍにて２０分間に亘
り回転させ、粉体を混合した。混合が均一であることを
確認の後、次の噴霧工程として、装置内部を減圧状態の
ま５回転数を１５ｒ、ｐ、　ｍに上げ、溶媒として塩化
メチレン・メタノール（２：８）混液Ｉ　Ｋ９を上記混
合物に噴霧した。引続き装置内部を減圧状態および５０
°Ｃに保ち回転数を５ｒ、ｐ、ｍに下げて２０分間に亘
る減圧乾燥工程を実施した（最高減圧到達度５馴Ｈｇ　
）。その結果、下記第１〜第２表に示す如く、従来法（
比較例）のものと変らない良質の造粒品が得られた。Example powders include trichlormethiazide 0.2 K9, lactose 5 K9, corn starch 2.24 Kg, crystalline cellulose (Avicel PH101, manufactured by Asahi Kasei) 2.25 to 7 Kg.
A total of 9.95 K9 was weighed out and put into a powder processing device. The inside of this device is under reduced pressure and 50'
The main body of the apparatus was rotated for 20 minutes at 5 rpm and pom to mix the powder. After confirming that the mixture is homogeneous, the next spraying process is performed by increasing the rotation speed to 15 r, p, m while the inside of the device is under reduced pressure, and using a mixture of methylene chloride and methanol (2:8) as the solvent. was sprayed onto the above mixture. Continue to reduce the pressure inside the device and
A vacuum drying process was carried out for 20 minutes by keeping the temperature at
). As a result, as shown in Tables 1 and 2 below, the conventional method (
A granulated product of good quality similar to that of Comparative Example) was obtained.

比較例 トリクロルメチアジド０．２　Ｋｇ、乳糖０．５　Ｋｙ
、トウモロコシ澱粉２．２４　Ｋｇ、　結晶セルロース
（アビセルＰＨ１０１、旭化成製）２．２５Ｋｇの合計
９、８５　Ｋ９を秤取して、これを実施例と同様に粉体
処理装置に投入し、該装置の内部を５０　’Ｃおよび減
圧状態に保ち、装置本体を５ｒ、ｐ、ｍにて２０分間に
亘り回転させ、粉体を混合した。混合が均一となったこ
とを確認の後、噴霧工程として装置内部を減圧状態に保
ち回転数を１５ｒ、　ｐ、　ｍに上げ、メチルセルロー
ス（メトローズ５ＱＳＩ（信越化学製）３％を含む塩化
メチレン、メタノール（２：８）ｉ昆液３．３３　Ｋｓ
＋を〆見合中の粉体に噴霧した。引続き装置内部を減圧
状態および５０°Ｃに保ち回転数を５ｒ、ｐ、ｍに下げ
て減圧乾燥した結果、第１〜第２表に示す如きデータが
得られた。また、上記実施例、比較例にて得た造粒品を
錠剤に適用したところ、第３表に示すデータが得られた
。Comparative example Trichlormethiazide 0.2 Kg, lactose 0.5 Ky
, 2.24 Kg of corn starch, and 2.25 Kg of crystalline cellulose (Avicel PH101, manufactured by Asahi Kasei), a total of 9.85 K9, was weighed out and put into the powder processing equipment in the same manner as in the example. The interior was kept at 50'C and reduced pressure, and the main body of the apparatus was rotated at 5r, p, m for 20 minutes to mix the powder. After confirming that the mixture was homogeneous, the inside of the device was kept under reduced pressure during the spraying process, and the rotation speed was increased to 15r, p, m, and methylcellulose (Metrose 5QSI (manufactured by Shin-Etsu Chemical), methylene chloride containing 3%, and methanol was added. (2:8) i Konji 3.33 Ks
+ was sprayed onto the powder during finishing. Subsequently, the inside of the apparatus was kept in a reduced pressure state and at 50 DEG C., and the rotational speed was lowered to 5 r, p, m for drying under reduced pressure. As a result, the data shown in Tables 1 and 2 were obtained. Furthermore, when the granulated products obtained in the above Examples and Comparative Examples were applied to tablets, the data shown in Table 3 were obtained.

【図面の簡単な説明】[Brief explanation of drawings]

図面は本発明の実施に使用する装置の全体概略図である
。The drawing is an overall schematic diagram of the apparatus used to carry out the invention.

Claims (1)

【特許請求の範囲】 造粒しようとする粉体と粉末バインダーと を密閉タンク中へ収容し均一に混合する行程と、密閉タ
ンク内を減圧し真空となし溶媒を噴霧して造粒し得られ
た造粒物を乾燥する行程を行なうことを特徴とする造粒
方法。[Claims] Powder to be granulated and a powder binder are placed in a closed tank and mixed uniformly, and the inside of the closed tank is depressurized and vacuumed, and a solvent is sprayed to obtain granulation. A granulation method characterized by performing a step of drying a granulated product.