JP5328285B2 - Aluminum hydroxide gel particles and production method thereof - Google Patents
Aluminum hydroxide gel particles and production method thereof Download PDFInfo
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本発明は、酸に対する反応速度が速く且つ経時変化しにくい水酸化アルミニウムゲル粒子およびその製造方法に関する。 The present invention relates to aluminum hydroxide gel particles having a high reaction rate with respect to an acid and hardly changing over time, and a method for producing the same.
水酸化アルミニウムゲルは従前より医薬用制酸剤として多用されている。しかしながら、従来の水酸化アルミニウムゲルは、胃酸に対する反応速度が遅く、しかも製造後比較的急速に老化が進み、制酸剤として要求される胃酸のｐＨを約３にまで中和するのに１０分近く要する程度に老化し、更に、酸中和量が低くて制酸剤としての機能を十分満足し得ない難点がある。 Aluminum hydroxide gel has been widely used as a pharmaceutical antacid. However, the conventional aluminum hydroxide gel has a slow reaction rate to gastric acid and ages relatively rapidly after production, and it takes 10 minutes to neutralize the pH of gastric acid required as an antacid to about 3. Aging is required to the extent necessary, and further, there is a drawback that the acid neutralization amount is low and the function as an antacid cannot be sufficiently satisfied.
酸に対する反応速度が速く且つ経時変化しにくい水酸化アルミニウムゲルに関しては、例えば、特許文献１には、乾燥前のゲルの平均二次粒子径を４μｍ以下とし、
（Ｍ２Ｏ）ｘ１Ａｌ２Ｏ３（ＣＯ２）ｙＲｚ・ｍＨ２Ｏ、（Ｍ２Ｏ）ｘ１（ＣａＯ）ｘ２Ａｌ２Ｏ３（ＣＯ２）ｙＲｚ・ｍＨ２Ｏ、（Ｍ２Ｏ）ｘ１（ＭｇＯ）ｘ３Ａｌ２Ｏ３（ＣＯ２）ｙＲｚ・ｍＨ２Ｏ、（Ｍ２Ｏ）ｘ１（ＣａＯ）ｘ２（ＭｇＯ）ｘ３Ａｌ２Ｏ３（ＣＯ２）ｙＲｚ・ｍＨ２Ｏ
（式中、Ｍは１価のアルカリ金属、Ｒは２価以上の有機酸）
の組成で示される水酸化アルミニウムゲルが提案されているが、不純物等が含まれているために本発明の水酸化アルミニウムゲルとは明らかに別の物質である。
Regarding aluminum hydroxide gel that has a high reaction rate with respect to acid and hardly changes with time, for example, Patent Document 1 discloses that the average secondary particle size of the gel before drying is 4 μm or less,
(M 2 O) x 1 Al 2 O 3 (CO 2 ) y Rz · mH 2 O, (M 2 O) x 1 (CaO) x 2 Al 2 O 3 (CO 2 ) y Rz · mH 2 O, (M 2 O ) x1 (MgO) x3 Al 2 O 3 (CO 2) y Rz · mH 2 O, (M 2 O) x1 (CaO) x2 (MgO) x3 Al 2 O 3 (CO 2) y Rz · mH 2 O
(In the formula, M is a monovalent alkali metal, R is a divalent or higher organic acid)
An aluminum hydroxide gel represented by the following composition has been proposed, but it is clearly a different substance from the aluminum hydroxide gel of the present invention because it contains impurities and the like.
また、特許文献２には、
［（ＣａＯ）ｘ１（ＭｇＯ）ｘ２（Ｍ２Ｏ）ｘ３］Ａｌ２Ｏ３（ＣＯ２）ｙ・ｍＨ２Ｏ
（式中、Ｍはアルカリ金属）
の組成で示される水酸化アルミニウムゲルが提案されているが、多くの不純物が含まれることおよびその不純物がアルカリ金属、アルカリ土類金属であるために得られた水酸化アルミニウムの液性が中性でなく、日本薬局方第十五改正に不適合品であることより、本発明の水酸化アルミニウムゲルとは明らかに別物質である。
[(CaO) x1 (MgO) x2 (M 2 O) x3] Al 2 O 3 (CO 2) y · mH 2 O
(Where M is an alkali metal)
The aluminum hydroxide gel represented by the composition of the above has been proposed, but the liquidity of the obtained aluminum hydroxide is neutral because it contains many impurities and the impurities are alkali metals and alkaline earth metals In addition, since it is incompatible with the 15th revision of the Japanese Pharmacopoeia, it is clearly a different substance from the aluminum hydroxide gel of the present invention.
本発明は、酸反応性が極めて良く、経時変化しにくい水酸化アルミニウムゲル粒子及びその製造方法を提供するものである。 The present invention provides an aluminum hydroxide gel particle that has very good acid reactivity and hardly changes with time, and a method for producing the same.
本発明者らは、従来の前記課題を解決するために鋭意研究を重ねた結果、水酸化アルミニウムゲル製造において、反応で得られた水酸化アルミニウムゲル粒子を固液分離、洗浄・脱水後ケーキを再乳化しスプレー乾燥において高温で瞬時に乾燥することにより、水酸化アルミニウムゲル中の酸化アルミニウム含量を高くすることにより、また、脱水後ケーキを真空冷凍乾燥器を用いて低温で乾燥することにより、酸に対する反応性が極めて良く、且つ経時変化しにくい水酸化アルミニウムゲル粒子が得られることを見出し、本発明の完成に至った。 As a result of intensive studies to solve the above-mentioned conventional problems, the present inventors have conducted solid-liquid separation, washing and dehydration of the aluminum hydroxide gel particles obtained by the reaction in the production of aluminum hydroxide gel. By re-emulsifying and instantly drying at high temperature in spray drying, by increasing the aluminum oxide content in the aluminum hydroxide gel, and by drying the cake after dehydration at low temperature using a vacuum freeze dryer, The inventors have found that aluminum hydroxide gel particles having extremely good reactivity with an acid and hardly change over time can be obtained, and the present invention has been completed.
すなわち、本発明は、
下記式（Ｉ）で表わされる水酸化アルミニウムゲル粒子である。
Ａｌ２Ｏ３（ＣＯ２）ｘ・ｍＨ２Ｏ （Ｉ）
但し式（Ｉ）中、ｘ、ｍは、それぞれ下記範囲を満足する。
１≦ｘ≦０．７、０．５≦ｍ＜４．０である。
本発明の水酸化アルミニウムゲル粒子は、酸化アルミニウム量が式（１）化合物の重量に基づいて、６０〜９０％であり、日本薬局方第十五改正に適合するものである。
That is, the present invention
Aluminum hydroxide gel particles represented by the following formula (I).
Al 2 O 3 (CO 2 ) x · mH 2 O (I)
However, in formula (I), x and m each satisfy the following ranges.
1 ≦ x ≦ 0.7 and 0.5 ≦ m <4.0.
The aluminum hydroxide gel particles of the present invention have an aluminum oxide content of 60 to 90% based on the weight of the compound of formula (1), and conform to the 15th revision of the Japanese Pharmacopoeia.
また本発明は、可溶性アルミニウム塩水溶液と炭酸イオン供給化合物水溶液とをｐＨ５．８〜６．８、温度１０〜４０℃の条件で反応させ、反応生成液を固液分離し、洗浄後乾燥することにより得られる水酸化アルミニウムゲル粒子の製造方法である。 In the present invention, a soluble aluminum salt aqueous solution and a carbonate ion supplying compound aqueous solution are reacted under the conditions of pH 5.8 to 6.8 and temperature of 10 to 40 ° C., the reaction product solution is separated into solid and liquid, washed and dried. It is a manufacturing method of the aluminum hydroxide gel particle obtained by this.
水酸化アルミニウムの理想的な化学組成式は、Ａｌ２Ｏ３・３Ｈ２Ｏであるが、従前より市販されている水酸化アルミニウムゲル粒子の化学組成式はＡｌ２Ｏ３・４．０〜５．０Ｈ２Ｏである。前記式から、市販の水酸化アルミニウムゲル粒子は理想形の水酸化アルミニウムに比べてフリーの水（自由水）をＡｌ２Ｏ３１個に対して１．０〜２．０個多く含有していることが分かる。そして、このフリーの水が老化（経時変化）を促進することを見出した。さらに、乾燥時にこのフリーの水を品温が可能な限り低く、また、可及的速やかに飛ばすことにより、目的とする水酸化アルミニウムゲル粒子が得られることを見出し本発明を完成した。
本発明で得られる水酸化アルミニウムゲル粒子は、日本薬局方第十五改正に適合し、更に酸に対する反応性が極めて良く且つ経時変化しにくい物質である。
本発明の製造方法によれば、日本薬局方第十五改正に適合し、酸に対する反応性が極めて良く且つ経時変化しにくい水酸化アルミニウムゲル粒子を製造することができる。
The ideal chemical composition formula of aluminum hydroxide is Al 2 O 3 · 3H 2 O, but the chemical composition formula of aluminum hydroxide gel particles that have been commercially available is Al 2 O 3 · 4.0 to 5-5. 0.0H 2 O. From the above formula, the commercially available aluminum hydroxide gel particles contain 1.0 to 2.0 more free water (free water) relative to one Al 2 O 3 than the ideal form aluminum hydroxide. I understand that. And it discovered that this free water promoted aging (aging). Further, the present invention has been completed by finding that the desired aluminum hydroxide gel particles can be obtained by drying the free water as low as possible at the time of drying and as quickly as possible.
The aluminum hydroxide gel particles obtained according to the present invention are a substance that conforms to the 15th revision of the Japanese Pharmacopoeia, has very good reactivity with acids, and hardly changes over time.
According to the production method of the present invention, it is possible to produce aluminum hydroxide gel particles that comply with the 15th revision of the Japanese Pharmacopoeia, have extremely good reactivity with acids, and hardly change over time.
本発明の水酸化アルミニウムゲル粒子は、可溶性アルミニウム塩水溶液と炭酸イオン供給化合物水溶液とをｐＨ５．８〜６．８、温度１０〜４０℃の条件で反応させ、反応生成液を固液分離し、洗浄後乾燥することにより得られる。 In the aluminum hydroxide gel particles of the present invention, a soluble aluminum salt aqueous solution and a carbonate ion supply compound aqueous solution are reacted under the conditions of pH 5.8 to 6.8 and temperature of 10 to 40 ° C., and the reaction product liquid is separated into solid and liquid. Obtained by drying after washing.
可溶性アルミニウム塩としては、塩化アルミニウム、硝酸アルミニウム、硫酸アルミニウム等が挙げられるが、硫酸アルミニウムが安価であり好ましい。 Examples of the soluble aluminum salt include aluminum chloride, aluminum nitrate, and aluminum sulfate. Aluminum sulfate is inexpensive and preferable.
炭酸イオン供給塩としては、炭酸カリウム、炭酸アンモニウム、炭酸ナトリウム等が挙げられるが、炭酸ナトリウムが最も有効である。 Examples of the carbonate ion supply salt include potassium carbonate, ammonium carbonate, sodium carbonate and the like, but sodium carbonate is most effective.
反応は、炭酸アルカリの水溶液の一定量を反応槽に投入しかき混ぜながら、可溶性アルミニウム塩の水溶液一定量を、一定の速度で注加する、また、逆に可溶性アルミニウム塩の水溶液の一定量を反応槽に投入しかき混ぜながら、炭酸アルカリの水溶液の一定量を一定の速度で注加するバッチ反応で行うことができる。更に、可溶性アルミニウム塩の水溶液と炭酸アルカリの水溶液を一定の割合で、予め一定量の水を投入したオーバーフロー付き反応槽に注加する連続反応等で行うこともできるが、生産性（反応能力）の良い連続反応方式が好ましい。 In the reaction, a certain amount of an aqueous solution of an alkali carbonate is added to a reaction vessel, and a constant amount of an aqueous solution of a soluble aluminum salt is added at a constant rate. It can be carried out by a batch reaction in which a certain amount of an alkali carbonate aqueous solution is poured at a constant rate while being stirred into the tank. Furthermore, it can be carried out in a continuous reaction or the like in which an aqueous solution of a soluble aluminum salt and an aqueous solution of alkali carbonate are poured into a reaction tank with an overflow in which a predetermined amount of water has been added in advance. A continuous reaction system with good quality is preferred.
反応ｐＨは、５．８〜６．８、好ましくは６．４〜６．７である。反応ｐＨが、５．８以下になると得られる水酸化アルミニウムゲル粒子の構造中に硫酸イオンが取り込まれ、この硫酸イオンを除くための洗浄が複雑となる。逆に、反応ｐＨが６．８を超えると得られる水酸化アルミニウムゲルの構造中にナトリウムイオンが取り込まれ、このナトリウムイオンを除くための洗浄が複雑となる。
反応温度は、１０〜４０℃、好ましくは２０〜３０℃である。
The reaction pH is 5.8 to 6.8, preferably 6.4 to 6.7. When the reaction pH is 5.8 or lower, sulfate ions are incorporated into the structure of the resulting aluminum hydroxide gel particles, and cleaning for removing the sulfate ions becomes complicated. On the other hand, when the reaction pH exceeds 6.8, sodium ions are taken into the structure of the aluminum hydroxide gel obtained, and cleaning for removing the sodium ions becomes complicated.
The reaction temperature is 10 to 40 ° C, preferably 20 to 30 ° C.
乾燥は、洗浄・脱水により得られたケーキを乾燥する工程であるが、本発明においてこの乾燥工程が最も重要な工程である。すなわち、同ケーキが含有するフリーの水を品温を上げずに瞬時に乾燥しなければならないことによる。
このための乾燥器としては、噴霧乾燥機（スプレードライヤー）、真空冷凍乾燥器が最も好ましい。従前より市販されている水酸化アルミニウムゲル粒子の乾燥もそのほとんどが噴霧乾燥機によるものであるが、乾燥温度（出口温度→排気温度）が低いために前記したように、多量のフリーの水を含有している。市販されている水酸化アルミニウムゲル粒子のスプレードライヤーにおける乾燥条件は、出口温度として１００℃以下で乾燥されているが、本発明の水酸化アルミニウムゲル粒子を得るための、出口温度は１２０℃〜１６０℃、好ましくは１２５〜１４０℃である。乾燥温度（出口温度）を高くすることは品温が高くなり、得られる水酸化アルミニウム粒子の酸反応性が悪くなり不利となるが、スプレードライヤーによる乾燥は瞬時乾燥であるために、その影響が非常に少ない。
真空冷凍乾燥器は、最も理想的な乾燥器である。すなわち、洗浄・脱水により得られたケーキに含まれるフリーの水を冷凍し、真空状態にすることにより氷を昇華する乾燥方法であることによる。また、乾燥に要する温度も３０〜３５℃と極低温であることによる。
Drying is a step of drying the cake obtained by washing and dehydration, and this drying step is the most important step in the present invention. That is, free water contained in the cake must be instantly dried without raising the product temperature.
As the dryer for this purpose, spray dryers (spray dryers) and vacuum freeze dryers are most preferable. Most of the aluminum hydroxide gel particles that have been marketed in the past are also spray spray dryers, but because the drying temperature (exit temperature → exhaust temperature) is low, as described above, a large amount of free water is used. Contains. The drying conditions of the commercially available aluminum hydroxide gel particles in the spray dryer are dried at 100 ° C. or less as the outlet temperature, but the outlet temperature for obtaining the aluminum hydroxide gel particles of the present invention is 120 ° C. to 160 ° C. ° C, preferably 125-140 ° C. Increasing the drying temperature (outlet temperature) increases the product temperature, resulting in a disadvantageous acid reactivity of the resulting aluminum hydroxide particles. Very few.
The vacuum freeze dryer is the most ideal dryer. That is, it is because it is a drying method in which free water contained in the cake obtained by washing and dehydration is frozen and the ice is sublimated by evacuation. Moreover, it is because the temperature required for drying is 30-35 degreeC and very low temperature.
本発明の製造方法によれば、下記式（Ｉ）で表わされる水酸化アルミニウムゲル粒子が得られる。
Ａｌ２Ｏ３（ＣＯ２）ｘ・ｍＨ２Ｏ （Ｉ）
但し式（Ｉ）中、ｘ、ｍは、それぞれ下記範囲を満足する。
０．１≦ｘ≦０．７、０．５≦ｍ＜４．０
ｘの上限の制限はないが、０．７が好ましく、さらに好ましくは、０．５である。
ｘの下限が０．１以下になると経時変化しやすいものとなり目的とする水酸化アルミニウムゲル粒子を得ることができない。
ｍの好ましい下限は０．５、さらに好ましくは１．０、特に好ましくは１．８であり、ｍの上限は４．０未満、好ましくは３．５、さらに好ましくは３．２である。
ｍは、４．０以上となると得られる水酸化アルミニウムゲル粒子がフリーの水を含有することになり、本発明の目的物質を得ることができない。下限についての制限はないが、０．５以下とするためには乾燥温度を更に高くしなければならなく、製造コストの面から不利となる。
また、得られた水酸化アルミニウムゲル粒子の、酸化アルミニウム含有量は式（１）化合物の重量に基づいて、６０〜９０％となるが、好ましくは６０〜７０％である。
According to the production method of the present invention, aluminum hydroxide gel particles represented by the following formula (I) are obtained.
Al 2 O 3 (CO 2 ) x · mH 2 O (I)
However, in formula (I), x and m each satisfy the following ranges.
0.1 ≦ x ≦ 0.7, 0.5 ≦ m <4.0
Although there is no upper limit of x, 0.7 is preferable, and 0.5 is more preferable.
When the lower limit of x is 0.1 or less, it tends to change with time and the intended aluminum hydroxide gel particles cannot be obtained.
The lower limit of m is preferably 0.5, more preferably 1.0, particularly preferably 1.8, and the upper limit of m is less than 4.0, preferably 3.5, and more preferably 3.2.
If m is 4.0 or more, the resulting aluminum hydroxide gel particles contain free water, and the target substance of the present invention cannot be obtained. Although there is no restriction on the lower limit, in order to make it 0.5 or less, the drying temperature must be further increased, which is disadvantageous from the viewpoint of production cost.
Moreover, although aluminum oxide content of the obtained aluminum hydroxide gel particle becomes 60 to 90% based on the weight of the compound of formula (1), it is preferably 60 to 70%.
得られた水酸化アルミニウムゲル粒子は、日本薬局方第十五改正に適合する。液性が中性であるのでＮａが少なく腎障害、高血圧を引き起こすことがない。
第十五回正日本薬局方乾燥水酸化アルミニウムゲル規格は下記の通りである。
１）性状
色→白色、形状→無晶性の粉末、におい→なし、味→なし
２）溶解性
水→ほとんど溶けない、エタノール（９５）→ほとんど溶けない、ジエチルエーテル→ほとんど溶けない、希塩酸→大部分溶ける、ＮａＯＨ試液→大部分溶ける
３）確認試験
アルミニウム塩→適合
４）純度試験
液性→中性、塩化物→０．２８４％以下、硫酸塩→０．４８％以下、硝酸塩→褐色の輪帯を生じない、重金属→１０ｐｐｍ以下、ヒ素→５ｐｐｍ以下
５）制酸力→２５０ｍＬ以上
６）酸化アルミニウム→５０．０％以上
The obtained aluminum hydroxide gel particles conform to the Japanese Pharmacopoeia 15th revision. Since the liquid is neutral, there is little Na and it does not cause renal damage and hypertension.
The 15th Japanese Pharmacopoeia dry aluminum hydroxide gel standard is as follows.
1) Properties Color → white, shape → amorphous powder, odor → none, taste → none 2) Solubility Water → Insoluble, ethanol (95) → Insoluble, diethyl ether → Insoluble, diluted hydrochloric acid → Mostly soluble, NaOH solution → Mostly soluble 3) Confirmation test Aluminum salt → Conformity 4) Purity test Liquid → Neutral, Chloride → 0.284% or less, Sulfate → 0.48% or less, Nitrate → Brown No heavy metal zone, heavy metal → 10 ppm or less, arsenic → 5 ppm or less 5) Antacid power → 250 mL or more 6) Aluminum oxide → 50.0% or more
以下実施例に基づき本発明をより詳細に説明するが、本発明はこれに限定されるものではない。また、得られた水酸化アルミニウムゲル粒子の特性は以下の方法により測定した。
（１）第十五改正日本薬局方乾燥水酸化アルミニウムゲル規格：日本薬局方乾燥水酸化アルミニウムゲルに準じて測定した。
（２）酸反応性試験
１００ｍＬ容ビーカーに、濃度０．１モル／Ｌ塩酸５０ｍＬを正確に採り、３７℃の恒温槽に浸し、液温を３７℃に昇温する。つづいて、ｐＨメータの電極を液に浸し、マグネティックスタラーによる攪拌下に、試料粉末１．０ｇを加え、同時にストップウオッチを作動させ、液ｐＨが３．０および３．５に至るまでの時間および１０分後のｐＨを測定する。
（３）炭酸ガス→ＡＧＫ式 炭酸ガスの簡易精密定量法に準じた。
EXAMPLES Hereinafter, although this invention is demonstrated in detail based on an Example, this invention is not limited to this. Moreover, the characteristic of the obtained aluminum hydroxide gel particle was measured with the following method.
(1) Fifteenth revision Japanese Pharmacopoeia dry aluminum hydroxide gel standard: Measured according to Japanese Pharmacopoeia dry aluminum hydroxide gel.
(2) Acid Reactivity Test In a 100 mL beaker, accurately take 50 mL of a concentration of 0.1 mol / L hydrochloric acid, immerse it in a 37 ° C. constant temperature bath, and raise the liquid temperature to 37 ° C. Subsequently, the electrode of the pH meter is immersed in the liquid, and 1.0 g of the sample powder is added with stirring by a magnetic stirrer, and at the same time, the stopwatch is operated, and the time until the liquid pH reaches 3.0 and 3.5 and The pH after 10 minutes is measured.
(3) Carbon dioxide gas → AGK type It conformed to the simple and precise quantitative method for carbon dioxide gas.
オーバーフロー付容量２．２Ｌのステンレス製反応槽に、予め水道水５００ｍＬを入れ攪拌下に、１．０５モル／Ｌ硫酸アルミニウム水溶液を１１．５ｍＬ／分および０．７６モル／Ｌ炭酸ナトリウム水溶液を６１．８ｍＬ／分の流速でそれぞれの定量ポンプを用いて供給し、反応温度２２〜２４℃で１２０分間反応した。なお、反応ｐＨは終始６．５１〜６．５３であった。
得られた反応懸濁液を、ヌッチエを用いて吸引ろ過により固液分離し、得られたケーキを１４Ｌの水道水を通水（洗浄）した。洗浄後ケーキに水を加えてＡｌ２Ｏ３として２５０ｇ／Ｌに再乳化し、ラボスケールのスプレードライヤーを用いて、入口温度（熱風温度）４５０℃、出口温度（排気温度）１２０℃で乾燥し、水酸化アルミニウムゲル粒子を得た。
得られた水酸化アルミニウムゲル粒子の化学組成式は以下の通りであった。
Ａｌ２Ｏ３（ＣＯ２）０．２４・２．７７Ｈ２Ｏであった。
また、得られた水酸化アルミニウムゲルの特性を表１に、酸反応性試験結果を表２に示す。
In a 2.2 L stainless steel reaction tank with overflow, 500 mL of tap water was previously added, and under stirring, 1.05 mol / L aluminum sulfate aqueous solution was added to 11.5 mL / min and 0.76 mol / L sodium carbonate aqueous solution was added to 61 mL. It was supplied using each metering pump at a flow rate of 8 mL / min, and reacted at a reaction temperature of 22 to 24 ° C. for 120 minutes. The reaction pH was 6.51 to 6.53 throughout.
The obtained reaction suspension was subjected to solid-liquid separation by suction filtration using a Nuccie, and the obtained cake was passed (washed) with 14 L of tap water. After washing, water is added to the cake and re-emulsified to 250 g / L as Al 2 O 3 , and dried at a inlet temperature (hot air temperature) of 450 ° C. and outlet temperature (exhaust temperature) of 120 ° C. using a laboratory scale spray dryer. The aluminum hydroxide gel particles were obtained.
The chemical composition formula of the obtained aluminum hydroxide gel particles was as follows.
Al 2 O 3 (CO 2) was 0.24 · 2.77H 2 O.
Table 1 shows the characteristics of the obtained aluminum hydroxide gel, and Table 2 shows the results of the acid reactivity test.
実施例１において、ラボスケールのスプレードライヤー乾燥における出口温度を１４０℃とした以外は、実施例１と同じ方法で水酸化アルミニウムゲル粒子を得た。
得られた水酸化アルミニウムゲル粒子の化学組成式は以下の通りであった。
Ａｌ２Ｏ３（ＣＯ２）０．２０・２．１２Ｈ２Ｏであった。
また、得られた水酸化アルミニウムゲルの特性を表１に、酸反応性試験結果を表２に示す。
In Example 1, aluminum hydroxide gel particles were obtained in the same manner as in Example 1 except that the outlet temperature in lab-scale spray dryer drying was 140 ° C.
The chemical composition formula of the obtained aluminum hydroxide gel particles was as follows.
It was Al 2 O 3 (CO 2 ) 0.20 · 2.12H 2 O.
Table 1 shows the characteristics of the obtained aluminum hydroxide gel, and Table 2 shows the results of the acid reactivity test.
実施例１において、固液分離により得られたケーキをラボスケールの真空乾燥機を用いて乾燥した以外は、実施例１と同じ方法で水酸化アルミニウムゲル粒子を得た。なお、乾燥終了時の品温は３３℃であった。
得られた水酸化アルミニウムゲル粒子の化学組成式は以下の通りであった。
Ａｌ２Ｏ３（ＣＯ２）０．４５・１．９５Ｈ２Ｏであった。
また、得られた水酸化アルミニウムゲルの特性を表１に、酸反応性試験結果を表２に示す。
（比較例１）
In Example 1, aluminum hydroxide gel particles were obtained in the same manner as in Example 1 except that the cake obtained by solid-liquid separation was dried using a lab-scale vacuum dryer. The product temperature at the end of drying was 33 ° C.
The chemical composition formula of the obtained aluminum hydroxide gel particles was as follows.
Al 2 O 3 (CO 2) was 0.45 · 1.95H 2 O.
Table 1 shows the characteristics of the obtained aluminum hydroxide gel, and Table 2 shows the results of the acid reactivity test.
(Comparative Example 1)
実施例１において、ラボスケールのスプレードライヤー乾燥時の出口温度（排気温度）を９０℃とした以外は、実施例１と同じ方法で水酸化アルミニウムゲル粒子を得た。
得られた水酸化アルミニウムゲル粒子の化学組成式は以下の通りであった。
Ａｌ２Ｏ３（ＣＯ２）０．３３・４．３０Ｈ２Ｏであった。
また、得られた水酸化アルミニウムゲルの特性を表１に、酸反応性試験結果を表２に示す。
（比較例２）
In Example 1, aluminum hydroxide gel particles were obtained in the same manner as in Example 1 except that the outlet temperature (exhaust temperature) at the time of drying the laboratory scale spray dryer was 90 ° C.
The chemical composition formula of the obtained aluminum hydroxide gel particles was as follows.
Al 2 O 3 (CO 2) was 0.33 · 4.30H 2 O.
Table 1 shows the characteristics of the obtained aluminum hydroxide gel, and Table 2 shows the results of the acid reactivity test.
(Comparative Example 2)
市販の水酸化アルミニウムゲル粒子（協和化学工業株式会社製、銘柄Ｓ−１００）の化学組成式はその一例として以下の通りである。
Ａｌ２Ｏ３（ＣＯ２）０．３１・４．１５Ｈ２Ｏであった。
また、同水酸化アルミニウムゲルの特性を表１に、酸反応性試験結果を表２に示めす。
An example of the chemical composition formula of commercially available aluminum hydroxide gel particles (Kyowa Chemical Industry Co., Ltd., brand S-100) is as follows.
It was Al 2 O 3 (CO 2 ) 0.31 · 4.15H 2 O.
The characteristics of the aluminum hydroxide gel are shown in Table 1, and the acid reactivity test results are shown in Table 2.
表１より、本発明の水酸化アルミニウムゲル粒子は日本薬局方第十五改正に適合し、酸化アルミニウム含有量が６０〜７０％の範囲にあることが分かる。また、表２より本発明の水酸化アルミニウムゲル粒子は酸反応性が極めて良く、更に、経時変化しにくいことが分かる。 From Table 1, it can be seen that the aluminum hydroxide gel particles of the present invention conform to the Japanese Pharmacopoeia 15th revision and the aluminum oxide content is in the range of 60 to 70%. Further, it can be seen from Table 2 that the aluminum hydroxide gel particles of the present invention have very good acid reactivity and are hardly changed over time.
本発明の水酸化アルミニウムゲル粒子は、従前より市販されている水酸化アルミニウムゲル粒子に比して、酸に対する反応速度が速く且つ経時変化しにくい。よって、医薬用制酸剤としての利用に多くの改善が期待される。 The aluminum hydroxide gel particles of the present invention have a higher reaction rate with respect to acids and are less likely to change over time as compared with aluminum hydroxide gel particles that have been commercially available. Therefore, many improvements are expected for use as a pharmaceutical antacid.
Claims (6)
Ａｌ2Ｏ3（ＣＯ2）ｘ・ｍＨ2Ｏ （1）
但し式（1）中、ｘ、ｍはそれぞれ下記範囲を満足する。
0.1≦ｘ≦0.7、0.5≦ｍ≦2.12
さらに式（1）において、酸化アルミニウム量が式（1）化合物の重量に基づいて、60〜90％である。 A soluble aluminum salt aqueous solution and aqueous carbonate ion supplying compound PH5.8～6.8, reacted at a temperature of 10 to 40 ° C., the reaction solution was solid-liquid separated, washed, by spray-drying or vacuum freeze-drying An obtained antacid comprising aluminum hydroxide gel particles represented by the following formula (1).
Al 2 O 3 (CO 2 ) x · mH 2 O (1)
However, in formula (1), x and m each satisfy the following ranges.
0.1 ≦ x ≦ 0.7, 0.5 ≦ m ≦ 2.12
Furthermore, in Formula (1), the amount of aluminum oxide is 60 to 90% based on the weight of the compound of Formula (1).
ＡｌAl 22 ＯO 3Three （ＣＯ(CO 22 ）) ｘx ・ｍＨ・ MH 22 Ｏ （1）O (1)
但し式（1）中、ｘ、ｍはそれぞれ下記範囲を満足する。However, in formula (1), x and m each satisfy the following ranges.
0.1≦ｘ≦0.7、0.5≦ｍ≦2.120.1 ≦ x ≦ 0.7, 0.5 ≦ m ≦ 2.12
さらに式（1）において、酸化アルミニウム量が式（1）化合物の重量に基づいて、60〜90％である。Furthermore, in Formula (1), the amount of aluminum oxide is 60 to 90% based on the weight of the compound of Formula (1).
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| JPS571440A (en) * | 1980-06-03 | 1982-01-06 | Kyowa Chem Ind Co Ltd | Adsorbing agent and utilization thereof |
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