JPH03278830A - Production of material having core material coated with fine particle shell - Google Patents
Production of material having core material coated with fine particle shellInfo
- Publication number
- JPH03278830A JPH03278830A JP2080456A JP8045690A JPH03278830A JP H03278830 A JPH03278830 A JP H03278830A JP 2080456 A JP2080456 A JP 2080456A JP 8045690 A JP8045690 A JP 8045690A JP H03278830 A JPH03278830 A JP H03278830A
- Authority
- JP
- Japan
- Prior art keywords
- core material
- particle group
- suspension
- fine particle
- particles
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000011162 core material Substances 0.000 title claims abstract description 13
- 239000010419 fine particle Substances 0.000 title claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000000463 material Substances 0.000 title abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 42
- 239000000725 suspension Substances 0.000 claims abstract description 10
- 238000001694 spray drying Methods 0.000 claims description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 abstract description 9
- 229910010271 silicon carbide Inorganic materials 0.000 abstract description 9
- 239000003814 drug Substances 0.000 abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 6
- 239000008119 colloidal silica Substances 0.000 abstract description 6
- 239000003337 fertilizer Substances 0.000 abstract description 6
- 229940079593 drug Drugs 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 4
- 239000003905 agrochemical Substances 0.000 abstract description 3
- 238000005507 spraying Methods 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 description 13
- 238000013268 sustained release Methods 0.000 description 9
- 239000012730 sustained-release form Substances 0.000 description 9
- 239000008186 active pharmaceutical agent Substances 0.000 description 4
- 229940088679 drug related substance Drugs 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002344 surface layer Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000010828 elution Methods 0.000 description 3
- 229920000620 organic polymer Polymers 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 2
- 239000001095 magnesium carbonate Substances 0.000 description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〈産業化の利用分野〉
本発明は、徐放性の医薬、農薬又は肥料として有効に活
用できる物体の製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION <Field of Industrial Application> The present invention relates to a method for producing an object that can be effectively utilized as a sustained-release medicine, agricultural chemical, or fertilizer.
〈従来の技術〉
従来より徐放性の医薬、農薬又は肥料は、有効成分から
成る芯物質の周囲にセルロース系やラテンクス系から成
る有機高分子をスプレ一方式でコーティングすることに
より造られている。<Prior art> Traditionally, sustained-release medicines, pesticides, or fertilizers have been produced by coating a core material consisting of an active ingredient with organic polymers such as cellulose or Latinx using a one-way spray method. .
一方粒子懸濁液を噴霧乾燥すると得られる製品に粒子の
偏析が見られることは古くから知られているが、この事
実は均質な粉体を得ようとする場合の欠点として認識さ
れてきた。On the other hand, it has been known for a long time that particle segregation is observed in the product obtained by spray drying a particle suspension, and this fact has been recognized as a drawback when attempting to obtain a homogeneous powder.
〈発明が解決しようとする課題〉
上記有機高分子膜で覆設した従来の徐放性の医薬、農薬
又は肥料は、該高分子をスプレーする際に有機溶媒を使
う必要があり該有機溶媒が完全には飛散しきらず製品中
に残存し人体や土地に有害となることもある。又有機高
分子膜である為に耐熱性に劣り、かつ強度もさほど大と
なることはない等の欠点があった。<Problem to be solved by the invention> Conventional sustained-release drugs, pesticides, or fertilizers covered with the above-mentioned organic polymer film require the use of an organic solvent when spraying the polymer. It may not be completely dispersed and may remain in the product, causing harm to humans and the land. Furthermore, since it is an organic polymer film, it has disadvantages such as poor heat resistance and not very high strength.
本発明では、これら従来の欠点を解消し優れた徐放性の
医薬、！ｆ４薬又は肥料として活用できる物体の製造方
法を提供することを目的とするものである。The present invention eliminates these conventional drawbacks and provides an excellent sustained-release drug! The purpose of the present invention is to provide a method for producing an object that can be used as an f4 medicine or fertilizer.
〈課題を解決する為の手段〉
上記本発明の目的は次の如き手段を採用することにより
達成できる。即ち、芯物質としての大粒子群と、該大粒
子の１７５以下の膜物質としての小粒子群とから成る懸
濁液を噴霧乾燥することで、芯物質の周囲が微粒子殻で
覆われた物体を製造することができる。<Means for Solving the Problems> The above object of the present invention can be achieved by employing the following means. That is, by spray-drying a suspension consisting of a group of large particles as a core material and a group of small particles as a membrane material of 175 or less of the large particles, an object in which the periphery of the core material is covered with a fine particle shell is created. can be manufactured.
なおここで大粒子というのはその径がミクロンオーダー
のものを指称し、小粒子というのは該大粒子の径の１７
５以下のものを指称する。小粒子の径が大粒子の径の１
７５よりも大なる場合には、後述する実施例の結果から
も明らかな如く大粒子と小粒子が完全には別れきれずに
十分な微粒子殻が得られない。Note that large particles here refer to those whose diameter is on the order of microns, and small particles refer to those with a diameter of 17 microns.
5 or less. The diameter of the small particle is 1 of the diameter of the large particle.
If it is larger than 75, large particles and small particles cannot be completely separated and a sufficient particle shell cannot be obtained, as is clear from the results of Examples described later.
く作用〉
本発明の方法では、第１図の（イ）に示す様に大粒子群
と小粒子群とが混在した懸濁液を噴霧乾燥すると、途中
第１図の（０）に示す様な形態を採り乾燥後は第１図（
ハ）に示す様に小粒子群が大粒子群を取り囲んだ様な形
態となる。In the method of the present invention, when a suspension containing a mixture of large particle groups and small particle groups is spray-dried as shown in (a) of FIG. 1, during the process, as shown in (0) of FIG. Figure 1 (
As shown in c), a group of small particles surrounds a group of large particles.
〈実施例〉
この実施例では、ミクロンオーダーの粒子としては、市
販の研磨剤である不二見研磨剤工業■の炭化ケイ素を、
サブミクロンの超微粒子としては、触媒化成工業■のコ
ロイダルシリカ５ｉ５００ （６ｎｍ） 及びＳｉＳｉ
３０Ｐ（８０ｎを用いた。又薬物質としては、徳山曹達
■の炭酸マグネシウムを用いた。これらの粒子を含んだ
懸濁液を塔径１．６ｍ、円筒部高さ０．９１の噴霧乾燥
装置により乾燥した。乾燥条件は人口温度１２０°Ｃ９
予熱時出ロ温度約９０°Ｃ１操作時温度約８０°Ｃとし
た。回転円板は直径７ ｃｍで回転数１２００Ｏｒｐｍ
、風量は４．４ｒｒｒ ／ ｍｔｎ、供給液量７０１ｎ
１／ｍｉｎとした。<Example> In this example, silicon carbide from Fujimi Abrasive Industry ■, a commercially available abrasive, was used as the micron-order particles.
As submicron ultrafine particles, colloidal silica 5i500 (6 nm) and SiSi manufactured by Catalysts & Chemical Industry ■ are used.
30P (80n) was used. Magnesium carbonate from Tokuyama Soda ■ was used as the drug substance. The suspension containing these particles was dried in a spray dryer with a tower diameter of 1.6 m and a cylindrical part height of 0.91 m. The drying conditions were a population temperature of 120°C9.
The temperature at the time of preheating was approximately 90°C, and the temperature during operation was approximately 80°C. The rotating disk has a diameter of 7 cm and a rotation speed of 1200 rpm.
, air volume is 4.4rrr/mtn, supply liquid volume is 701n
It was set to 1/min.
乾燥された粒子は主として本体下部より回収し、これの
７４μｍふるい下を上品とし、サイクロンで回収したも
のの７４μｍふるい下をサイクロン品とし、１００°Ｃ
の乾燥器で再乾燥したものを実験試料とした。さらに一
部の製品は電気炉により最高４００°Ｃまで加熱した。The dried particles were mainly collected from the bottom of the main body, the part under the 74 μm sieve was classified as high-quality, and the part collected in a cyclone was classified as the 74 μm sieve under the cyclone, and the part was heated at 100°C.
The sample was re-dried in a dryer and used as an experimental sample. Additionally, some products were heated to a maximum of 400°C in an electric furnace.
なお薬物質の溶出試験は、製品０．１ｇをｐＨ２の緩衝
溶液５００ｄに懸濁浮遊させ、溶出したＭｇイオンを経
時的に原子吸光分光光度計により測定するというもので
ある。In the elution test of the drug substance, 0.1 g of the product is suspended in 500 d of a pH 2 buffer solution, and the eluted Mg ions are measured over time using an atomic absorption spectrophotometer.
■ 〈作用〉の実験的確認
下記第１表に示す様に１０μｍと１μｍの炭化ケイ素を
組合せ、その懸濁液を噴霧乾燥した場合の製品について
細孔径分布を測定した。その結果を第２図に示す。(2) Experimental Confirmation of <Effect> As shown in Table 1 below, the pore size distribution of a product obtained by combining 10 μm and 1 μm silicon carbide and spray-drying the resulting suspension was measured. The results are shown in FIG.
第 １ 表
Ｓ−〇からＳ−５の各製品の走査電子顕微鏡観察による
と、Ｓ−２では不十分だがＳ−３では十分な小粒子によ
る被膜が得られていることが判った。又第２図に示す水
銀圧入ポロシメーターにょる細孔分布の測定結果よりＳ
−３以上の体積分率で大粒子から成る構造の示す細孔径
がなくなり、小粒子から成る構造の示す細孔径が主体と
なっていることが判る。According to scanning electron microscope observation of each product in Table 1 S-0 to S-5, it was found that S-2 had an insufficient coating, but S-3 had a sufficient coating of small particles. Also, from the measurement results of pore distribution using a mercury intrusion porosimeter shown in Figure 2, S
It can be seen that at a volume fraction of -3 or more, the pore diameter indicated by the structure consisting of large particles disappears, and the pore diameter indicated by the structure consisting of small particles becomes the main component.
中心部と表面層のみがけ密度が等しいとすると、Ｓ−３
で表面層の厚さと中心部の直径との比は約０．２となり
、製品径が４０μｍのとき表面層の厚さは約６μｍであ
る。第１表に示したＳ−５以外の各体積分率での製品の
空隙率はいずれも０．５１〜０．５３となっており、こ
れは大小の各成分粒子が混在することなく、それぞれ別
々の位置を占めていることを示唆している。即ち、これ
らの製品は大粒子で構成された芯部分と小粒子で構成さ
れた殻部分とから成るものと考えられ、〈作用〉で述べ
たことが実験的に確認された。Ｓ−５の結果からは、製
品の内部に空孔が形成されていることが示唆される。Assuming that the polishing density of the center and surface layers is equal, S-3
The ratio of the thickness of the surface layer to the diameter of the center is about 0.2, and when the product diameter is 40 μm, the thickness of the surface layer is about 6 μm. The porosity of the products at each volume fraction other than S-5 shown in Table 1 is all 0.51 to 0.53, which means that there is no mixture of large and small component particles, and each product has a porosity of 0.51 to 0.53. This suggests that they occupy separate positions. That is, these products are thought to consist of a core portion made up of large particles and a shell portion made up of small particles, and the above-mentioned ``effect'' was experimentally confirmed. The results of S-5 suggest that pores are formed inside the product.
次に１０μｍと５μｍの炭化ケイ素、及び１０μｍと２
μｍの炭化ケイ素の組合せについて同様に製品の細孔径
分布状態を測定した結果をそれぞれ第３図及び第４図に
示すが、これらの結果から大粒子径と小粒子径の比が５
以上ないとそれらが十分に別れないことが判る。Next, silicon carbide of 10 μm and 5 μm, and 10 μm and 2
Figures 3 and 4 show the results of similarly measuring the pore size distribution of products for combinations of μm silicon carbide, and these results indicate that the ratio of large particle size to small particle size is 5.
It turns out that they cannot be separated sufficiently unless there is more than that.
■ 徐放性物体の製造
小粒子としてコロイダルシリカを用い微細な細孔を有す
る徐放性の物体の製造方法について述べる、即ち、大粒
子としては、炭酸マグネシウムと炭化ケイ素の混合物を
用いた。(2) Production of sustained-release material A method for producing a sustained-release material having fine pores using colloidal silica as small particles will be described. That is, a mixture of magnesium carbonate and silicon carbide was used as the large particles.
これはモデル薬物質である。コロイダルシリカとモデル
薬物質の配合を第２表に示す、コロイダルシリカを２種
類の混合物としたのは乾燥の促進を図るためである。This is a model drug substance. The combination of colloidal silica and model drug substance is shown in Table 2. The reason why two types of colloidal silica were used as a mixture was to promote drying.
第 ２ 表
第５図及び第６図にそれぞれＭｇの溶出率と時間との関
係を示すグラフを示す。これによるとコロイダルシリカ
Ｓ １５００ （６μｍ）を比較的多く用いたＣ−１及
びＣ−２が強い徐放性を示している事が判る。なお第６
図中Ｃ−２１（３００°Ｃ）としているのはＣ−２１を
更に３００°Ｃまで加熱したもので、この様に加熱する
と溶出抑制能が更に強化される。Table 2, Figures 5 and 6 respectively show graphs showing the relationship between the Mg elution rate and time. This shows that C-1 and C-2, which used a relatively large amount of colloidal silica S 1500 (6 μm), exhibited strong sustained release properties. Furthermore, the sixth
C-21 (300°C) in the figure is C-21 further heated to 300°C, and heating in this manner further strengthens the elution suppression ability.
〈発明の効果〉
以上述べて来た如く、本発明によれば噴霧乾燥させるこ
とで大粒子群は芯部に、小粒子群は表層部に移動し、従
来は均質な成分を造る際の欠点とされていた現象を有効
に活用し芯物質の周囲を微粒子殻で覆われた物体を造る
ことができ、この物体は徐放性の医薬、農薬又は肥料と
して有効利用ができるものである。<Effects of the Invention> As described above, according to the present invention, by spray drying, large particles move to the core and small particles move to the surface layer, which eliminates the drawbacks of conventional methods when producing homogeneous ingredients. By effectively utilizing this phenomenon, it is possible to create an object in which a core material is surrounded by a shell of fine particles, and this object can be effectively used as a sustained-release medicine, agricultural chemical, or fertilizer.
第１図は本発明方法による懸濁液滴の乾燥過程を示す概
念図、第２図は１０μｍと１μｍの炭化ケイ素の組合せ
による製品の細孔径と微分空孔容積との関係を示すグラ
フ、第３図は１０μｍと５μｍの炭化ケイ素の組合せに
よる製品の細孔径と微分空孔容積との関係を示すグラフ
、第４図は１０μｍと２μｍの炭化ケイ素の組合せによ
る製品の細孔径と微分空孔容積との関係を示すグラフ、
第５図及び第６図は共に製品の徐放特性を示すグラフ。Fig. 1 is a conceptual diagram showing the drying process of suspension droplets according to the method of the present invention, Fig. 2 is a graph showing the relationship between pore diameter and differential pore volume of products made of a combination of 10 μm and 1 μm silicon carbide, and Fig. Figure 3 is a graph showing the relationship between the pore diameter and differential pore volume of a product made from a combination of 10 μm and 5 μm silicon carbide, and Figure 4 is a graph showing the relationship between the pore diameter and differential pore volume of a product made from a combination of 10 μm and 2 μm silicon carbide. A graph showing the relationship between
Figures 5 and 6 are graphs showing the sustained release characteristics of the product.
Claims (1)
ら成る懸濁液を噴霧乾燥することを特徴とする芯物質の
周囲を微粒子殻で覆われた物体の製造方法。1. A method for producing an object having a core material surrounded by a fine particle shell, which comprises spray-drying a suspension consisting of a group of large particles and a group of small particles that are 1/5 or less of the large particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2080456A JP2560220B2 (en) | 1990-03-27 | 1990-03-27 | Sustained release granular material and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2080456A JP2560220B2 (en) | 1990-03-27 | 1990-03-27 | Sustained release granular material and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03278830A true JPH03278830A (en) | 1991-12-10 |
| JP2560220B2 JP2560220B2 (en) | 1996-12-04 |
Family
ID=13718764
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2080456A Expired - Lifetime JP2560220B2 (en) | 1990-03-27 | 1990-03-27 | Sustained release granular material and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2560220B2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999051091A1 (en) * | 1998-04-07 | 1999-10-14 | Shionogi & Co., Ltd. | Pulse release pesticide granule having hydrophobic coating film containing silica |
| WO2001026809A1 (en) * | 1999-10-13 | 2001-04-19 | Engelhard Corporation | Catalyst compositions employing sol particles and methods of using the same |
| FR2801227A1 (en) * | 1999-11-22 | 2001-05-25 | Univ Fed Do Rio Grande Do Sul | Spray-drying colloidal suspensions of polymer nanocapsules or nanospheres, e.g. containing drug such as diclofenac, including addition of silicon dioxide before drying to improve suspension stability |
| WO2014036572A3 (en) * | 2012-08-31 | 2014-11-06 | Aeci Limited | Particulate products and process for manufacture thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110128699B (en) * | 2019-06-03 | 2021-03-16 | 江苏极易新材料有限公司 | Method for granulating composite antioxidant |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59222224A (en) * | 1983-04-22 | 1984-12-13 | イ−・アイ・デユポン・デ・ニモアス・アンド・カンパニ− | Production of surface porous macro-particle |
-
1990
- 1990-03-27 JP JP2080456A patent/JP2560220B2/en not_active Expired - Lifetime
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59222224A (en) * | 1983-04-22 | 1984-12-13 | イ−・アイ・デユポン・デ・ニモアス・アンド・カンパニ− | Production of surface porous macro-particle |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999051091A1 (en) * | 1998-04-07 | 1999-10-14 | Shionogi & Co., Ltd. | Pulse release pesticide granule having hydrophobic coating film containing silica |
| WO2001026809A1 (en) * | 1999-10-13 | 2001-04-19 | Engelhard Corporation | Catalyst compositions employing sol particles and methods of using the same |
| FR2801227A1 (en) * | 1999-11-22 | 2001-05-25 | Univ Fed Do Rio Grande Do Sul | Spray-drying colloidal suspensions of polymer nanocapsules or nanospheres, e.g. containing drug such as diclofenac, including addition of silicon dioxide before drying to improve suspension stability |
| WO2014036572A3 (en) * | 2012-08-31 | 2014-11-06 | Aeci Limited | Particulate products and process for manufacture thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2560220B2 (en) | 1996-12-04 |
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