JP4381083B2 - Sodium percarbonate particles with excellent tablet formability and storage stability - Google Patents
Sodium percarbonate particles with excellent tablet formability and storage stability Download PDFInfo
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- JP4381083B2 JP4381083B2 JP2003345494A JP2003345494A JP4381083B2 JP 4381083 B2 JP4381083 B2 JP 4381083B2 JP 2003345494 A JP2003345494 A JP 2003345494A JP 2003345494 A JP2003345494 A JP 2003345494A JP 4381083 B2 JP4381083 B2 JP 4381083B2
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Description
本発明は、錠剤成形性及び保存安定性に優れた過炭酸ナトリウム粒子に関する。本発明の過炭酸ナトリウム粒子は、義歯洗浄剤等の漂白成分含有発泡洗浄錠剤に好適に使用される。 The present invention relates to sodium percarbonate particles excellent in tablet moldability and storage stability. The sodium percarbonate particles of the present invention are suitably used for foamed cleaning tablets containing bleaching components such as denture cleaning agents.
義歯洗浄剤等の発泡洗浄剤として、過ホウ酸ナトリウム等のアルカリ性過酸化物とモノ過硫酸カリウム等の酸性過酸化物を主成分とする組成物を錠剤化したものが用いられている。アルカリ性過酸化物としては過炭酸ナトリウムも使用可能であるが、過炭酸ナトリウムは過ホウ酸ナトリウムに比べて、錠剤成形性が劣ることや、組成物中の水分や酸性過酸化物によって分解されやすいことから、その使用が限られていた。 As foaming detergents such as denture detergents, tablets obtained by tableting a composition mainly composed of an alkaline peroxide such as sodium perborate and an acidic peroxide such as potassium monopersulfate are used. Sodium percarbonate can be used as the alkaline peroxide, but sodium percarbonate is inferior in tablet formability to sodium perborate and is easily decomposed by moisture and acidic peroxide in the composition. Therefore, its use was limited.
本発明の目的は、従来技術における上記したような課題を解決し、錠剤成形性に優れ、酸性過酸化物と配合しても高い安定性を示す過炭酸ナトリウムを提供することにある。 An object of the present invention is to solve the above-described problems in the prior art, and to provide sodium percarbonate that is excellent in tablet moldability and exhibits high stability even when blended with an acidic peroxide.
本発明者らは、上記の問題を解決するべく鋭意検討した結果、過炭酸ナトリウムに炭酸水素ナトリウムを添加して造粒し、次いでポリエチレングリコールを被覆することにより、上記の課題が解決された過炭酸ナトリウム粒子が得られることを見いだし、本発明に到達した。 As a result of intensive studies to solve the above problems, the inventors of the present invention added granulated sodium bicarbonate to sodium percarbonate, and then coated with polyethylene glycol to overcome the above problem. The inventors have found that sodium carbonate particles can be obtained and have reached the present invention.
すなわち、本発明は、１〜２０重量％の水分を含有した湿潤結晶である過炭酸ナトリウムに炭酸水素ナトリウム５〜３０重量部を添加して造粒し、次いでポリエチレングリコール３〜２０重量部を被覆してなることを特徴とする過炭酸ナトリウム粒子に関するものである。 That is, in the present invention, 5-30 parts by weight of sodium bicarbonate is added to sodium percarbonate, which is a wet crystal containing 1-20% by weight of water, and granulated, and then 3-20 parts by weight of polyethylene glycol is coated. It is related with the sodium percarbonate particle | grains characterized by these.
本発明によれば、保存安定性や発泡性の優れた発泡洗浄錠剤の原料として有用であり、錠剤成形性も優れた過炭酸ナトリウムを得ることができる。 According to the present invention, sodium percarbonate, which is useful as a raw material for foam-washed tablets having excellent storage stability and foamability, and excellent tablet moldability, can be obtained.
原料となる過炭酸ナトリウムとしては、過酸化水素水溶液と炭酸ナトリウムを安定剤の存在下で反応させて得られた湿潤状態あるいは乾燥状態の過炭酸ナトリウムを用いることができ、特に湿潤結晶の過炭酸ナトリウムが好ましい。 As the sodium percarbonate used as a raw material, wet or dry sodium percarbonate obtained by reacting an aqueous hydrogen peroxide solution with sodium carbonate in the presence of a stabilizer can be used. Sodium is preferred.
本発明では、過炭酸ナトリウムの造粒時に炭酸水素ナトリウムを添加する。特に、１〜２０重量％の水分を含有した湿潤状態の過炭酸ナトリウムに炭酸水素ナトリウムを添加させる方法が、重炭酸ナトリウムを過炭酸ナトリウム中に均一に分散させることができ、より安定且つ安全な過炭酸ナトリウム粒子を得ることができ好ましい。さらに、一般的な造粒結合剤等を併用することもできる。造粒方法に特に制限はなく、公知の造粒機械を用いることができる。 In the present invention, sodium hydrogen carbonate is added during granulation of sodium percarbonate. In particular, the method of adding sodium bicarbonate to wet sodium percarbonate containing 1 to 20% by weight of water can disperse sodium bicarbonate uniformly in sodium percarbonate, making it more stable and safe. Sodium percarbonate particles can be obtained, which is preferable. Furthermore, a general granulating binder or the like can be used in combination. There is no restriction | limiting in particular in the granulation method, A well-known granulation machine can be used.
被覆に用いるポリエチレングリコールとしては、分子量１０００〜２００００のものを用いることができる。被覆の方法に特に制限はなく、ポリエチレングリコールを水または有機溶媒で溶液として流動している過炭酸ナトリウム粒子に噴霧し乾燥する方法や、液状のポリエチレングリコールを過炭酸ナトリウム粒子と混練することもできる。 As the polyethylene glycol used for coating, those having a molecular weight of 1000 to 20000 can be used. There is no particular limitation on the coating method, and polyethylene glycol can be sprayed onto sodium percarbonate particles flowing as a solution in water or an organic solvent and dried, or liquid polyethylene glycol can be kneaded with sodium percarbonate particles. .
炭酸水素ナトリウムの添加量は、過炭酸ナトリウム１００重量部に対して５〜３０重量部である。ポリエチレングリコールの被覆量は、過炭酸ナトリウム１００重量部に対して３〜２０重量％である。 The amount of sodium bicarbonate added is 5 to 30 parts by weight per 100 parts by weight of sodium percarbonate. The coating amount of polyethylene glycol is 3 to 20% by weight with respect to 100 parts by weight of sodium percarbonate.
配合量または被覆量が上記の範囲より少ないと発泡洗浄錠剤を製造する際に、所望の錠剤成形性、配合安定性、発泡性が得られない。また、配合量または被覆量が上記の範囲より多いと溶解性が低下するとともに、過炭酸ナトリウム粒子の有効酸素濃度が低下することから経済性の点でも好ましくない。 When the blending amount or the coating amount is less than the above range, desired tablet moldability, blending stability, and foamability cannot be obtained when producing foamed washed tablets. On the other hand, when the blending amount or the coating amount is larger than the above range, the solubility is lowered and the effective oxygen concentration of the sodium percarbonate particles is lowered, which is not preferable from the economical viewpoint.
被覆された過炭酸ナトリウム粒子の粒径は１００〜２０００μｍであり、好ましくは２００〜１０００μｍである。過炭酸ナトリウム粒子の粒径が小さすぎると、単位重量あたりの表面積が大きくなって粒子表面への均一な被覆がされずに安定性が低くなる。一方、粒径が大きすぎると、被覆操作時の粒子の流動性が悪くなって、均一な被覆が困難になるとともに粒子の凝集が起きやすくなる。 The particle size of the coated sodium percarbonate particles is 100 to 2000 μm, preferably 200 to 1000 μm. If the particle size of the sodium percarbonate particles is too small, the surface area per unit weight is increased, and the particle surface is not uniformly coated and the stability is lowered. On the other hand, if the particle size is too large, the fluidity of the particles during the coating operation deteriorates, and uniform coating becomes difficult and the particles tend to aggregate.
本発明の過炭酸ナトリウム粒子は非常に柔らかく、発泡洗浄錠剤を成形する際の他の成分との結合力が大きいため、錠剤成形性に優れている。粒子の柔らかさは粒子の硬度（破壊加重）で測定することができる。 Since the sodium percarbonate particles of the present invention are very soft and have a high binding force with other components when molding foamed washed tablets, they are excellent in tablet moldability. The softness of the particles can be measured by the hardness (destructive weight) of the particles.
本発明の過炭酸ナトリウムは、酸性過酸化物等と混合して成形することにより、保存安定性、発泡性に優れた発泡洗浄錠剤とすることができる。 The sodium percarbonate of the present invention can be made into a foam-washed tablet excellent in storage stability and foamability by being mixed with an acidic peroxide or the like and molded.
以下、本発明を実施例により具体的に説明するが、本発明はこれら実施例に限定されるものではない。 EXAMPLES The present invention will be specifically described below with reference to examples, but the present invention is not limited to these examples.
実施例１
炭酸ナトリウムと過酸化水素を水溶液中で反応させ、生成した結晶を遠心分離器によって分離、脱水して１０重量％の水分を含有する湿潤状態の過炭酸ナトリウムを得た。湿潤状態の過炭酸ナトリウムに、炭酸水素ナトリウムを過炭酸ナトリウムに対して乾燥状態基準で２０重量部とバインダーを加え、さらに水を加えて含水率を１１重量％に調整し、穴径１．０ｍｍのスクリーンをつけた造粒機で押出し造粒を行った後に乾燥して、平均粒径４００μｍの未被覆過炭酸ナトリウムを得た。得られた未被覆過炭酸ナトリウム３００ｇを流動乾燥式被覆装置（ヤマト科学（株）製パルビスコーティング装置）を用い被覆を行った。被覆は、多孔板より加熱空気を入れて過炭酸ナトリウムを流動乾燥させながら、取付けた噴霧ノズルよりポリエチレングリコール（分子量６０００）１０重量％を含有する水溶液２００ｇを噴霧した後、５分間乾燥を継続することにより行った。
Example 1
Sodium carbonate and hydrogen peroxide were reacted in an aqueous solution, and the produced crystals were separated by a centrifugal separator and dehydrated to obtain wet sodium percarbonate containing 10% by weight of water. To sodium percarbonate in a wet state, sodium bicarbonate is added to sodium percarbonate in an amount of 20 parts by weight and a binder on a dry basis, water is further added to adjust the water content to 11% by weight, and the hole diameter is 1.0 mm. Extrusion granulation was carried out using a granulator equipped with the above screen, followed by drying to obtain uncoated sodium percarbonate having an average particle diameter of 400 μm. 300 g of the obtained uncoated sodium percarbonate was coated using a fluidized drying coating apparatus (Palvis coating apparatus manufactured by Yamato Scientific Co., Ltd.). The coating is performed by spraying 200 g of an aqueous solution containing 10% by weight of polyethylene glycol (molecular weight: 6000) from the attached spray nozzle while fluidly drying sodium percarbonate by flowing heated air from a perforated plate and then continuing drying for 5 minutes. Was done.
得られた過炭酸ナトリウム粒子の粒子強度をグラノ式粒子硬度計で測定したところ、粒子はいずれも割れることなくつぶれて破壊加重は測定されなかった。この過炭酸ナトリウム７重量％、モノ過硫酸水素カリウム（デュポン社製オキソン）３０重量％、無水クエン酸３０重量％、炭酸水素ナトリウム２８重量％、ポリエチレングリコール（分子量６０００）５重量％の組成で、１錠あたり１０ｇの錠剤を成形した。錠剤成形性は良好であった。得られた錠剤をアルミパックで包装して５０℃の恒温槽で５日間保存したが、包装のふくれはみられなかった。また、得られた錠剤を２５℃の水５０ｇに投入したところ、１分間で１１０ｍｌのガスが発生した。 When the particle strength of the obtained sodium percarbonate particles was measured with a grano type particle hardness meter, all the particles were crushed without cracking, and the fracture load was not measured. With a composition of 7% by weight of sodium percarbonate, 30% by weight of potassium hydrogen persulfate (Oxone manufactured by DuPont), 30% by weight of anhydrous citric acid, 28% by weight of sodium bicarbonate, and 5% by weight of polyethylene glycol (molecular weight 6000), A tablet of 10 g was formed per tablet. Tablet moldability was good. The obtained tablet was packaged in an aluminum pack and stored in a thermostatic bath at 50 ° C. for 5 days, but no blistering was observed. Moreover, when the obtained tablet was put into 50 g of water at 25 ° C., 110 ml of gas was generated in 1 minute.
比較例１
過炭酸ナトリウムを造粒する際に炭酸水素ナトリウムを添加しないこと以外は、実施例１と同様に過炭酸ナトリウム粒子を得た。得られた過炭酸ナトリウム粒子の粒子強度をグラノ式粒子硬度計で測定したところ、破壊加重は２００ｇであった。また、実施例１と同様の組成の錠剤を成形しようとしたが、剥離や割れが多数発生しうまく成形できなかった。
Comparative Example 1
Sodium percarbonate particles were obtained in the same manner as in Example 1 except that sodium bicarbonate was not added when granulating sodium percarbonate. When the particle strength of the obtained sodium percarbonate particles was measured with a grano particle hardness tester, the breaking load was 200 g. In addition, a tablet having the same composition as in Example 1 was tried, but many peelings and cracks occurred, and the tablet could not be molded well.
比較例２
過炭酸ナトリウムを被覆する際にポリエチレングリコールの代わりに硫酸ナトリウムを用いること以外は、実施例１と同様に過炭酸ナトリウム粒子を得た。得られた過炭酸ナトリウム粒子の粒子強度をグラノ式粒子硬度計で測定したところ、粒子はいずれも割れることなくつぶれて破壊加重は測定されなかった。また、実施例１と同様の組成の錠剤を成形したが、錠剤成形性は良好であった。得られた錠剤をアルミパックで包装して５０℃の恒温槽で５日間保存したが、包装のふくれがみられた。また、得られた錠剤を２５℃の水５０ｇに投入したところ、１分間で５０ｍｌしかガスが発生しなかった。
Comparative Example 2
Sodium percarbonate particles were obtained in the same manner as in Example 1 except that sodium sulfate was used instead of polyethylene glycol when coating sodium percarbonate. When the particle strength of the obtained sodium percarbonate particles was measured with a grano particle hardness tester, none of the particles collapsed without cracking, and no fracture load was measured. Moreover, although the tablet of the composition similar to Example 1 was shape | molded, the tablet moldability was favorable. The obtained tablet was packaged in an aluminum pack and stored in a thermostatic bath at 50 ° C. for 5 days. Moreover, when the obtained tablet was put into 50 g of water at 25 ° C., only 50 ml of gas was generated in one minute.
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