JP4833567B2 - Magnesium oxide particles - Google Patents
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Description
本発明は、酸化マグネシウム錠剤製造用の酸化マグネシウム粒子に関する。 The present invention relates to magnesium oxide particles for producing magnesium oxide tablets.
制酸剤や緩下剤として、酸化マグネシウム錠剤が利用されている。このような目的に利用される酸化マグネシウム錠剤は、酸化マグネシウム粒子に賦形剤などを加えて、打錠成型することにより製造されている。ところが、酸化マグネシウム粒子は硬度が高いため、酸化マグネシウム粒子を錠剤に形成する際に酸化マグネシウム粒子と打錠成型機との摩耗により、酸化マグネシウム錠剤の表面に部分的な黒ずみが発生することがあることが知られている。 Magnesium oxide tablets are used as antacids and laxatives. Magnesium oxide tablets used for such purposes are manufactured by adding excipients and the like to magnesium oxide particles and tableting them. However, since the magnesium oxide particles have high hardness, when the magnesium oxide particles are formed into tablets, wear of the magnesium oxide particles and the tableting machine may cause partial darkening on the surface of the magnesium oxide tablets. It is known.
黒ずみのない酸化マグネシウム錠剤を製造する方法として、特許文献１には、粒状の酸化マグネシウム（適当な造粒機を用いて粉末状の酸化マグネシウムを粒状に造粒したもの）、賦形剤、及びタルク、並びにステアリン酸マグネシウム又はステアリン酸カルシウムを含有する混合粉末を打錠成型する方法が記載されている。 As a method for producing a blackened magnesium oxide tablet, Patent Document 1 discloses granular magnesium oxide (which is obtained by granulating powdered magnesium oxide in a granular form using an appropriate granulator), an excipient, and A method for tableting a mixed powder containing talc and magnesium stearate or calcium stearate is described.
特許文献２には、レーザ回折散乱法で測定された平均二次粒子径が０．５〜１０μｍの酸化マグネシウム粒子と結合材及び崩壊剤からなる混合物を造粒して得た顆粒状粒子に、潤滑剤（好ましくは、ステアリン酸マグネシウム又はステアリン酸カルシウム）を混合して打錠成型する方法が記載されている。
本発明の課題は、黒ずみを発生させずに酸化マグネシウム錠剤を製造するのに適した酸化マグネシウム粒子を提供することにある。 The subject of this invention is providing the magnesium oxide particle suitable for manufacturing a magnesium oxide tablet, without producing darkening.
本発明は、１０００℃の温度で１時間加熱したときの質量減少率が５〜１０質量％の範囲となるような量にて、表面が水酸化マグネシウム及び／又は炭酸マグネシウムからなる被覆層で覆われている酸化マグネシウム錠剤製造用の酸化マグネシウム粒子にある。
ここで、質量減少率（％）とは、（加熱前の酸化マグネシウム粒子の質量（ｇ）−加熱後の酸化マグネシウム粒子の質量（ｇ））／加熱前の酸化マグネシウム粒子の質量（ｇ）×１００（％）により算出される値を意味する。
The present invention covers the surface with a coating layer composed of magnesium hydroxide and / or magnesium carbonate in such an amount that the mass reduction rate when heated at 1000 ° C. for 1 hour is in the range of 5 to 10% by mass. It is in magnesium oxide particles for manufacturing magnesium oxide tablets.
Here, the mass reduction rate (%) is (mass of magnesium oxide particles before heating (g) −mass of magnesium oxide particles after heating (g)) / mass of magnesium oxide particles before heating (g) × It means a value calculated by 100 (%).
上記本発明の酸化マグネシウム粒子は、酸化マグネシウム粒子に、５０〜２００℃の温度下にて、水蒸気又は水蒸気と二酸化炭素ガスとの混合ガスを接触させる方法により製造することができる。 The magnesium oxide particles of the present invention can be produced by contacting the magnesium oxide particles with water vapor or a mixed gas of water vapor and carbon dioxide gas at a temperature of 50 to 200 ° C.
本発明の酸化マグネシウム粒子を用いることにより、打錠成型機を利用しながらも黒ずみのない酸化マグネシウム錠剤を高い得率で製造することが可能となる。また、本発明の酸化マグネシウム粒子の製造方法を利用することにより、表面が水酸化マグネシウム及び／又は炭酸マグネシウムからなる被覆層で覆われている酸化マグネシウム粒子を工業的に有利に製造することが可能となる。 By using the magnesium oxide particles of the present invention, it becomes possible to produce a magnesium oxide tablet without darkening with a high yield while using a tableting molding machine. Further, by using the method for producing magnesium oxide particles of the present invention, it is possible to industrially advantageously produce magnesium oxide particles whose surface is covered with a coating layer made of magnesium hydroxide and / or magnesium carbonate. It becomes.
本発明の酸化マグネシウム粒子は、１０００℃の温度で１時間加熱したときの質量減少率（以下、強熱質量減少率という）が５〜１０質量％の範囲となるように、その表面が水酸化マグネシウム又は炭酸マグネシウムあるいは水酸化マグネシウムと炭酸マグネシウムとの混合物からなる被覆層で覆われている。被覆層を形成している水酸化マグネシウム及び炭酸マグネシウムは酸化マグネシウムよりも硬度が低いため、本発明の酸化マグネシウム粒子は摩耗による着色が起こりにくい。
この強熱質量減少率は、加熱により水酸化マグネシウム又は炭酸マグネシウムが酸化マグネシウムに変化することにより生じる水又は二酸化炭素の揮発分に相当する。
The surface of the magnesium oxide particles of the present invention is hydroxylated so that the mass reduction rate (hereinafter referred to as ignition mass reduction rate) when heated at 1000 ° C. for 1 hour is in the range of 5 to 10 mass%. It is covered with a coating layer made of magnesium, magnesium carbonate, or a mixture of magnesium hydroxide and magnesium carbonate. Since the magnesium hydroxide and magnesium carbonate forming the coating layer have lower hardness than magnesium oxide, the magnesium oxide particles of the present invention are hardly colored by abrasion.
This ignition mass reduction rate corresponds to the volatile content of water or carbon dioxide that is generated when magnesium hydroxide or magnesium carbonate changes to magnesium oxide by heating.
本発明の酸化マグネシウム粒子は、酸化マグネシウム粒子に、５０〜２００℃（好ましくは６０〜１８０℃）の温度下にて、水蒸気又は水蒸気と二酸化炭素ガスとの混合ガスを接触させる方法により好適に製造することができる。酸化マグネシウム粒子に水蒸気を接触させると、酸化マグネシウムの粒子表面が水和され、水酸化マグネシウムからなる被覆層が生成する。そして、その水酸化マグネシウムからなる被覆層に、二酸化炭素ガスを接触させると、水酸化マグネシウムが炭酸化され炭酸マグネシウムが生成する。 The magnesium oxide particles of the present invention are suitably produced by a method in which water vapor or a mixed gas of water vapor and carbon dioxide gas is brought into contact with the magnesium oxide particles at a temperature of 50 to 200 ° C. (preferably 60 to 180 ° C.). can do. When water vapor is brought into contact with the magnesium oxide particles, the particle surfaces of the magnesium oxide are hydrated to form a coating layer made of magnesium hydroxide. When carbon dioxide gas is brought into contact with the coating layer made of magnesium hydroxide, the magnesium hydroxide is carbonated to produce magnesium carbonate.
原料となる酸化マグネシウム粒子としては、海水に生石灰を投入して水酸化マグネシウムを生成させる方法（いわゆる、海水法）により得た水酸化マグネシウム粒子を、７００〜１３００℃の温度、好ましくは７５０〜１２００℃の温度で焼成して製造したものを用いることができる。原料の酸化マグネシウム粒子は、強熱質量減少率が１質量％以下であることが好ましく、０．５質量％以下であることが特に好ましい。 As magnesium oxide particles used as raw materials, magnesium hydroxide particles obtained by a method (so-called seawater method) in which quick lime is introduced into seawater to produce magnesium hydroxide are used at a temperature of 700 to 1300 ° C., preferably 750 to 1200. What was baked and manufactured at the temperature of (degreeC) can be used. The raw material magnesium oxide particles preferably have an ignition mass reduction rate of 1% by mass or less, and particularly preferably 0.5% by mass or less.
原料の酸化マグネシウム粒子は、レーザ回折法により測定される平均二次粒子径が０．５〜１０μｍの範囲にあることが好ましい。また、粒子径が８μｍ以上の二次粒子の含有量が５体積％未満であることが好ましい。さらに、一次粒子の粒子サイズを表す指標の一つである比表面積が１〜５０ｍ2／ｇの範囲にあることが好ましい。 The raw material magnesium oxide particles preferably have an average secondary particle diameter in the range of 0.5 to 10 μm as measured by a laser diffraction method. In addition, the content of secondary particles having a particle diameter of 8 μm or more is preferably less than 5% by volume. Furthermore, it is preferable that the specific surface area which is one of the indexes representing the particle size of the primary particles is in the range of 1 to 50 m 2 / g.
原料の酸化マグネシウム粒子に水蒸気又は水蒸気と二酸化炭素ガスとの混合ガスを接触させる操作は、混練機などの攪拌混合装置を用いて、酸化マグネシウム粒子を攪拌しながら行なうことが好ましい。
酸化マグネシウム粒子と水蒸気又は混合ガスとの接触時間は、通常は３０分間〜５時間の範囲である。
The operation of bringing the raw material magnesium oxide particles into contact with water vapor or a mixed gas of water vapor and carbon dioxide gas is preferably performed while stirring the magnesium oxide particles using a stirring and mixing device such as a kneader.
The contact time between the magnesium oxide particles and water vapor or mixed gas is usually in the range of 30 minutes to 5 hours.
本発明の酸化マグネシウム粒子は、単独で、または公知の賦形剤、崩壊剤及び潤滑剤などの添加剤を加えて、酸化マグネシウム錠剤の製造材料として使用される。賦形剤の例としては、乳糖、結晶セルロース、澱粉及びリン酸水素カルシウムを挙げることができる。崩壊剤の例としては、カルボキシメチルセルロースナトリウム、カルボキシメチルセルロースカルシウム、クロスカルメロースナトリウム及びカルボキシ澱粉ナトリウムを挙げることができる。潤滑剤の例としては、ステアリン酸及びその塩（ナトリウム塩、マグネシウム塩、カルシウム塩）を挙げることができる。 The magnesium oxide particles of the present invention are used as a material for producing a magnesium oxide tablet alone or with the addition of known additives such as excipients, disintegrants and lubricants. Examples of excipients include lactose, crystalline cellulose, starch and calcium hydrogen phosphate. Examples of disintegrants include sodium carboxymethyl cellulose, calcium carboxymethyl cellulose, croscarmellose sodium and sodium carboxy starch. Examples of lubricants include stearic acid and its salts (sodium salt, magnesium salt, calcium salt).
賦形剤の添加量は、酸化マグネシウム粒子１００質量部に対して、１〜２０質量部の範囲にあることが好ましい。崩壊剤の添加量は、酸化マグネシウム粒子１００質量部に対して、１〜２０質量部の範囲にあることが好ましい。潤滑剤の添加量は０．１〜１０質量部の範囲にあることが好ましい。 The amount of the excipient added is preferably in the range of 1 to 20 parts by mass with respect to 100 parts by mass of the magnesium oxide particles. It is preferable that the addition amount of a disintegrating agent exists in the range of 1-20 mass parts with respect to 100 mass parts of magnesium oxide particles. The addition amount of the lubricant is preferably in the range of 0.1 to 10 parts by mass.
本発明の酸化マグネシウム粒子を、打錠成型機を用いて錠剤に形成する際の打錠圧は、１錠あたり５００〜２０００ｋｇの範囲にあることが好ましく、８００〜１２００ｋｇの範囲にあることが特に好ましい。 The tableting pressure when the magnesium oxide particles of the present invention are formed into tablets using a tableting machine is preferably in the range of 500 to 2000 kg, particularly in the range of 800 to 1200 kg. preferable.
［実施例１］
（１）酸化マグネシウム粒子の製造
海水法により得られた水酸化マグネシウム粒子１５ｋｇを９５０℃の温度で１時間焼成して酸化マグネシウム粒子１０ｋｇを製造した。得られた酸化マグネウム粒子の強熱質量減少率は０．４質量％であった。また、この酸化マグネウム粒子は、レーザ回折法により測定した平均二次粒子径が３μｍ、粒子径が８μｍ以上の二次粒子の含有量が０．２体積％であり、比表面積が１０ｍ2／ｇであった。
[Example 1]
(1) Production of Magnesium Oxide Particles 15 kg of magnesium hydroxide particles obtained by the seawater method were fired at a temperature of 950 ° C. for 1 hour to produce 10 kg of magnesium oxide particles. The ignition mass reduction rate of the obtained magnesium oxide particles was 0.4% by mass. The magnesium oxide particles have an average secondary particle diameter of 3 μm measured by a laser diffraction method, a content of secondary particles having a particle diameter of 8 μm or more is 0.2% by volume, and a specific surface area of 10 m 2 / g. Met.
（２）被覆層の形成
上記（１）にて得られた酸化マグネシウム粒子２ｋｇを、加熱装置付き万能混練機（内容積：５Ｌ）に投入した。次いで、酸化マグネシウム粒子を攪拌しながら、混練機内に水量として約１１５ｇ相当のスチームを導入して、密閉した。その後、混練機の内部温度を９５℃に加熱した。混練機の内部温度を９５℃に保持し、酸化マグネシウム粒子の攪拌を２時間続けて、酸化マグネシウム粒子の表面に被覆層を形成した。
得られた被覆層付き酸化マグネシウム粒子の強熱質量減少率は５．２質量％であった。
(2) Formation of coating layer 2 kg of the magnesium oxide particles obtained in (1) above were charged into a universal kneader equipped with a heating device (internal volume: 5 L). Next, while stirring the magnesium oxide particles, steam corresponding to about 115 g of water was introduced into the kneader and sealed. Thereafter, the internal temperature of the kneader was heated to 95 ° C. The internal temperature of the kneader was maintained at 95 ° C., and the stirring of the magnesium oxide particles was continued for 2 hours to form a coating layer on the surface of the magnesium oxide particles.
The ignition mass reduction rate of the obtained magnesium oxide particles with a coating layer was 5.2% by mass.
上記の被覆層付き酸化マグネシウム粒子５ｇをステンレス製の丸底容器に入れて、乳棒で酸化マグネシウム粒子を丸底容器の底部に６０秒間擦りつけて、摩耗による酸化マグネシウム粒子の着色状態を目視で観察した。その結果、酸化マグネシウム粒子の表面に着色は認められなかった。 Put 5 g of the above magnesium oxide particles with a coating layer in a stainless steel round bottom container, rub the magnesium oxide particles against the bottom of the round bottom container with a pestle for 60 seconds, and visually observe the colored state of the magnesium oxide particles due to wear. did. As a result, no coloration was observed on the surfaces of the magnesium oxide particles.
上記の被覆層付き酸化マグネシウム粒子を用いて、単発打錠機（金型：ステンレス製）にて打錠圧１０００ｋｇの条件で、質量１ｇの丸錠型酸化マグネシウム錠剤を１０個製造した。得られた酸化マグネシウム錠剤の表面を目視で観察した結果、全ての錠剤の表面に黒ずみは認められなかった。 Using the magnesium oxide particles with a coating layer, ten round tablet type magnesium oxide tablets having a mass of 1 g were produced using a single tableting machine (die: made of stainless steel) under a tableting pressure of 1000 kg. As a result of visual observation of the surface of the obtained magnesium oxide tablets, no darkening was observed on the surfaces of all the tablets.
［実施例２］
前記実施例１（１）にて得られた酸化マグネシウム粒子２ｋｇを、加熱装置付き万能混練機（内容積：５Ｌ）に投入した。次いで、酸化マグネシウム粒子を攪拌しながら、混練機内に水量として約１１５ｇ相当のスチームを導入した。次いで、混練機の内部温度を９０℃に加熱した。混練機の内部温度を９０℃に保持し、混練機内に二酸化炭素ガスを２Ｌ／分の流量で導入しながら、酸化マグネシウム粒子の攪拌を３時間続けて、酸化マグネシウム粒子の表面に被覆層を形成した。
得られた被覆層付き酸化マグネシウム粒子の強熱質量減少率は８．７質量％であった。
[Example 2]
2 kg of magnesium oxide particles obtained in Example 1 (1) were charged into a universal kneader equipped with a heating device (internal volume: 5 L). Next, while stirring the magnesium oxide particles, steam corresponding to about 115 g of water was introduced into the kneader. Next, the internal temperature of the kneader was heated to 90 ° C. While maintaining the internal temperature of the kneader at 90 ° C. and introducing carbon dioxide gas at a flow rate of 2 L / min into the kneader, the magnesium oxide particles are stirred for 3 hours to form a coating layer on the surfaces of the magnesium oxide particles. did.
The ignition mass reduction rate of the obtained magnesium oxide particles with a coating layer was 8.7% by mass.
上記の被覆層付き酸化マグネシウム粒子５ｇを前記実施例１と同様にステンレス製丸底容器の底部に６０秒間擦りつけて、摩耗による酸化マグネシウム粒子の着色状態を目視で観察した。その結果、酸化マグネシウム粒子の表面に着色は認められなかった。 In the same manner as in Example 1, 5 g of the magnesium oxide particles with a coating layer were rubbed against the bottom of a stainless steel round bottom container for 60 seconds, and the colored state of the magnesium oxide particles due to wear was visually observed. As a result, no coloration was observed on the surfaces of the magnesium oxide particles.
上記の被覆層付き酸化マグネシウム粒子を用いて、前記実施例１と同様に丸錠型酸化マグネシウム錠剤を１０個製造した。得られた酸化マグネシウム錠剤の表面を目視で観察した結果、全ての錠剤の表面に黒ずみは認められなかった。 Ten tablet-shaped magnesium oxide tablets were produced in the same manner as in Example 1 using the magnesium oxide particles with a coating layer. As a result of visual observation of the surface of the obtained magnesium oxide tablets, no darkening was observed on the surfaces of all the tablets.
［比較例１］
前記実施例１の（１）にて製造した被覆層無しの酸化マグネシウム粒子（強熱質量減少率：０．４質量％）５ｇを、前記実施例１と同様にステンレス製丸底容器の底部に６０秒間擦りつけて、摩耗による酸化マグネシウム粒子の着色状態を目視で観察した。酸化マグネシウム粒子は灰色に着色していた。
[Comparative Example 1]
5 g of magnesium oxide particles without a coating layer (ignition mass reduction rate: 0.4 mass%) produced in (1) of Example 1 were placed on the bottom of a stainless steel round bottom container in the same manner as in Example 1. By rubbing for 60 seconds, the colored state of the magnesium oxide particles due to abrasion was visually observed. Magnesium oxide particles were colored gray.
上記の被覆層無しの酸化マグネシウム粒子を用いて、前記実施例１と同様に丸錠型酸化マグネシウム錠剤を１０個製造した。得られた酸化マグネシウム錠剤の表面を目視で観察した結果、全ての錠剤の表面に黒ずみが認められた。 Ten round tablet-type magnesium oxide tablets were produced in the same manner as in Example 1 using the above magnesium oxide particles without a coating layer. As a result of visual observation of the surface of the obtained magnesium oxide tablets, darkening was observed on the surfaces of all the tablets.
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| JP2025021028A (en) * | 2023-07-31 | 2025-02-13 | セトラスホールディングス株式会社 | Magnesium oxide powder for tablets and its manufacturing method |
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| JP2000001428A (en) * | 1998-04-16 | 2000-01-07 | Nippon Shinyaku Co Ltd | Tablet and its production |
| JP4015485B2 (en) * | 2001-08-27 | 2007-11-28 | 協和化学工業株式会社 | Antacid / loose tablets |
| JP2004352633A (en) * | 2003-05-28 | 2004-12-16 | Kowa Co | Magnesium oxide tablets |
| JP2006022060A (en) * | 2004-07-09 | 2006-01-26 | Kyowa Chem Ind Co Ltd | Antacid / loose water dispersion and tablets therefor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0712828B2 (en) | 1989-06-06 | 1995-02-15 | 日産車体株式会社 | Horizontal slide device for steering column |
| CN107428550A (en) * | 2015-03-16 | 2017-12-01 | 宇部材料工业株式会社 | Magnesium oxide powder and resin combination and the manufacture method of magnesium oxide powder containing it |
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| JP2006249052A (en) | 2006-09-21 |
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