JP4100964B2 - Briquette preparation and method for producing the same - Google Patents
Briquette preparation and method for producing the same Download PDFInfo
- Publication number
- JP4100964B2 JP4100964B2 JP2002157816A JP2002157816A JP4100964B2 JP 4100964 B2 JP4100964 B2 JP 4100964B2 JP 2002157816 A JP2002157816 A JP 2002157816A JP 2002157816 A JP2002157816 A JP 2002157816A JP 4100964 B2 JP4100964 B2 JP 4100964B2
- Authority
- JP
- Japan
- Prior art keywords
- briquette
- preparation
- acid
- fragrance
- powder
- 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.)
- Expired - Fee Related
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- 239000004484 Briquette Substances 0.000 title claims description 56
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 238000002360 preparation method Methods 0.000 title description 42
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 10
- 239000003788 bath preparation Substances 0.000 claims description 10
- 150000007524 organic acids Chemical class 0.000 claims description 8
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 7
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 7
- 239000000314 lubricant Substances 0.000 claims description 7
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 6
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 6
- 239000001630 malic acid Substances 0.000 claims description 6
- 235000011090 malic acid Nutrition 0.000 claims description 6
- 239000002304 perfume Substances 0.000 claims description 6
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 6
- 239000001530 fumaric acid Substances 0.000 claims description 5
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 3
- 235000005985 organic acids Nutrition 0.000 claims description 3
- 239000003205 fragrance Substances 0.000 description 29
- 239000000843 powder Substances 0.000 description 27
- 239000002245 particle Substances 0.000 description 22
- 239000000203 mixture Substances 0.000 description 20
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 16
- 239000002994 raw material Substances 0.000 description 15
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 14
- 239000005871 repellent Substances 0.000 description 13
- 230000002940 repellent Effects 0.000 description 13
- 238000005187 foaming Methods 0.000 description 10
- 238000009472 formulation Methods 0.000 description 10
- 239000004615 ingredient Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000002156 mixing Methods 0.000 description 8
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 8
- 235000017557 sodium bicarbonate Nutrition 0.000 description 8
- 238000013329 compounding Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
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- 238000000034 method Methods 0.000 description 6
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- 235000013402 health food Nutrition 0.000 description 5
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- 239000013040 bath agent Substances 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
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- 239000000825 pharmaceutical preparation Substances 0.000 description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 4
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- 244000144725 Amygdalus communis Species 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 3
- 235000020224 almond Nutrition 0.000 description 3
- 238000003287 bathing Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
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- 235000011087 fumaric acid Nutrition 0.000 description 3
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- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
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- XMGQYMWWDOXHJM-JTQLQIEISA-N (+)-α-limonene Chemical compound CC(=C)[C@@H]1CCC(C)=CC1 XMGQYMWWDOXHJM-JTQLQIEISA-N 0.000 description 2
- WQNHWIYLCRZRLR-UHFFFAOYSA-N 2-(3-hydroxy-2,5-dioxooxolan-3-yl)acetic acid Chemical compound OC(=O)CC1(O)CC(=O)OC1=O WQNHWIYLCRZRLR-UHFFFAOYSA-N 0.000 description 2
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- NEHNMFOYXAPHSD-UHFFFAOYSA-N citronellal Chemical compound O=CCC(C)CCC=C(C)C NEHNMFOYXAPHSD-UHFFFAOYSA-N 0.000 description 2
- QMVPMAAFGQKVCJ-UHFFFAOYSA-N citronellol Chemical compound OCCC(C)CCC=C(C)C QMVPMAAFGQKVCJ-UHFFFAOYSA-N 0.000 description 2
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- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 2
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- KJPRLNWUNMBNBZ-QPJJXVBHSA-N (E)-cinnamaldehyde Chemical compound O=C\C=C\C1=CC=CC=C1 KJPRLNWUNMBNBZ-QPJJXVBHSA-N 0.000 description 1
- OOCCDEMITAIZTP-QPJJXVBHSA-N (E)-cinnamyl alcohol Chemical compound OC\C=C\C1=CC=CC=C1 OOCCDEMITAIZTP-QPJJXVBHSA-N 0.000 description 1
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- UFLHIIWVXFIJGU-ARJAWSKDSA-N (Z)-hex-3-en-1-ol Chemical compound CC\C=C/CCO UFLHIIWVXFIJGU-ARJAWSKDSA-N 0.000 description 1
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 description 1
- ODHCTXKNWHHXJC-VKHMYHEASA-N 5-oxo-L-proline Chemical compound OC(=O)[C@@H]1CCC(=O)N1 ODHCTXKNWHHXJC-VKHMYHEASA-N 0.000 description 1
- 240000002234 Allium sativum Species 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- WTEVQBCEXWBHNA-UHFFFAOYSA-N Citral Natural products CC(C)=CCCC(C)=CC=O WTEVQBCEXWBHNA-UHFFFAOYSA-N 0.000 description 1
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- AUNGANRZJHBGPY-UHFFFAOYSA-N D-Lyxoflavin Natural products OCC(O)C(O)C(O)CN1C=2C=C(C)C(C)=CC=2N=C2C1=NC(=O)NC2=O AUNGANRZJHBGPY-UHFFFAOYSA-N 0.000 description 1
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- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 description 1
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- 239000002202 Polyethylene glycol Substances 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 241000220317 Rosa Species 0.000 description 1
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- 229920002472 Starch Polymers 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Cosmetics (AREA)
- Detergent Compositions (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Fertilizers (AREA)
- Disinfection, Sterilisation Or Deodorisation Of Air (AREA)
- Fats And Perfumes (AREA)
Description
【0001】
【発明の属する技術分野】
本発明はブリケット製剤とその製造方法に関し、詳しくは、粒子形状の見た目が良好で商品価値が高く、かつ、発泡時に香料成分が容易に揮散する発泡性ブリケット製剤及び該製剤を容易に得ることができる製造方法に関する。
【0002】
【従来の技術】
本発明のブリケット製剤とは、粉体組成物をブリケッティングマシンにて成形加工して得られるブリケット状の製剤を意味する。ブリケッティングマシンとは、同速で互いに反対方向に回転する2本のロール間で原料粉体を圧縮し成型する乾式圧縮造粒機の一つであり、このロールの表面には、ブリケットの母型であるポケットが刻まれている。そのポケットの形状や大きさによって、種々の形状や大きさのブリケットを得ることが可能となる。ブリケットの形状としては、ピロー状、レンズ状、アーモンド状、プリズム状、棒状、フィンガー状などの形状を作ることができ、大きさとしては、0.3ccから200cc程度のブリケットの製造が可能である。通常、ブリケット製造においては、ロール間のクリアランスの大きさやロール同士の押さえ圧、フィードスクリューの押圧力などを調整することによりシート状一次成形体が得られる。ブリケットは、更にこの複数のブリケット粒子が連結部を介してシート状に成形されたシート状一次成形体を解砕することにより、得ることができる。つまり、ブリケットを製造する作業工程中、必ず解砕という工程をとることになり、粒子形状の「欠け」や「バリ」は必然的に発生することとなる。
【0003】
一般的に、ブリケットは化学、窯業、精錬、肥料などの工業用分野において、作業上や環境上の問題改善や反応の効率化のために、原料の成形加工によって得た中間製品として取り扱われる場合が殆どであり、従来、粒子形状の「欠け」や「バリ」などという製剤の見た目に関して、大きな問題となることは少なかった。一方、見栄えの改善を目的に、転動工程を設けることによりバリの少ないブリケット製剤を得ることも提案されているが、実際にブリケット製剤の見た目を100%改善ということは困難と考えられ、半ばあきらめられてきた。
【0004】
しかし、店頭や実使用において消費者の目にとまる最終商品である場合、そのブリケット形状の見た目は商品価値を左右する重要な因子でもあり、この見た目に関する改善がブリケット製剤の課題として挙げられてきた。
【0005】
具体的には、大きなブリケット粒子を得ようとした場合、解砕時のバリ取り作業と同時に粒子本体に「欠け」が多数生じ、また、小さなブリケット粒子を得ようとした場合は、解砕時に「バリ」を完全にとることが難しく、きれいな粒子形状のものを作ることができなかった。つまり、いずれの場合も、見た目で満足するものが得られないという問題点を有していた。
【0006】
さらに、ブリケット製剤を製造する上で、使用原料の中には、圧縮成形時にロールのポケットへの粉体の付着や詰まりなどが生じ易いものがあり、生産効率を著しく低下させることが問題として指摘されてきた。特に、水溶性高分子、炭酸塩および有機酸などの空気中の水分で付着性が高まる成分を配合した製剤を製造する場合に、ポケットへの付着、粉体の詰まりが頻発して生じる傾向が認められ、製造時問題となっていた。ロールのポケットに粉体が詰まってふさがった場合、ブリケット粒子を得ることはできず、ポケットに粉体が詰まるたびにロールの洗浄や清掃が必要となり、連続生産が不可能となってしまうため、生産効率の改善が求められてきた。
【0007】
【発明が解決しようとする課題】
本発明は、粒子形状が均一で見栄えが良く、かつ発泡時に香料成分が容易に揮散し、生産効率に優れた発泡性ブリケット製剤を提供することをその課題とする。
【0008】
【課題を解決するための手段】
本発明者らは、上記課題を解決すべく鋭意研究を重ねた結果、炭酸塩、有機酸および香料成分を配合する浴用剤において、ブリケット粒子をある特定の範囲の粒子径にすることにより、ブリケット製剤を効率よく得ることができることを見出した。更に、上記ブリケット製剤を製造する際、ロール面に滑沢剤を付着させることにより、ブリケッティングマシンのロールポケットへの粉体の付着、詰まりがなく、生産効率の高い製造が可能となることを見出し、本発明を完成するに至った。
【0009】
すなわち本発明は、
(1)炭酸塩、有機酸および香料を必須成分とし、直径3〜10mmかつ厚さ2.5〜10mmの大きさであることを特徴とした発泡性ブリケット製剤。
(2)浴用剤であることを特徴とした(1)記載のブリケット製剤。
(3)ブリケッティングマシンのロール面に滑沢剤を付着させることを特徴とする(1)または(2)のブリケット製剤の製造方法。
に関する。
【0010】
ブリケットの厚さとは、シート状一次成形体の垂直方向の長さを意味し、厚さは2.5〜10mm、特に3〜8mmが好ましい。この範囲を下回ると、ブリケット粒子と「バリ」との境界がはっきりしないため、きれいな粒子形状を留めることが難しく、この範囲を上回るとロールポケットからの製剤の抜けが著しく悪化し、連続生産が困難となり、好ましくない。
【0011】
ここでいう直径とは、シート状一次成形体の水平方向における、最長径を意味し、ブリケット製剤の直径は3〜10mm、特に4〜8mmが好ましい。この範囲を下回ると、解砕時のバリ取り作業をしてもきれいな粒子形状のものが得られず、好ましくない。また、この範囲を上回ると、解砕時のバリ取り作業と同時に粒子本体に「欠け」を多数生じ、見栄えの点で商品価値を大きく減じるため好ましくない。
【0012】
ブリケット製剤がアーモンド状などの楕円形状を有する場合、楕円形状の長径を、前記直径の範囲の上限内に設定することが好ましい。また、楕円形状の短径は前記直径の範囲の下限内に含まれることが好ましい。さらに、短径は長径の1/2以上1未満がより好ましい。この範囲を下回ると、出来上がりのブリケットは、解砕時や輸送時に粒子の折れが多数見られ、これも商品として満足できるものではなく、好ましくない。
【0013】
ブリケット製剤がピロー形などの多角形状を有する場合も、最長径が前記楕円形状の長径にあたり、最も短い辺の長さが、前記楕円形状の短径にあたる。
【0014】
本発明で用いられる炭酸塩としては、例えば、炭酸水素ナトリウム、炭酸ナトリウム、セスキ炭酸ナトリウム、炭酸カリウム、炭酸水素カリウム、炭酸マグネシウム、炭酸アンモニウムなどが挙げられ、特に炭酸水素ナトリウム、炭酸ナトリウムが入手の容易さから好ましい。これらの炭酸塩は、単独または2種以上を組み合わせて用いることができる。
【0015】
また、本発明の炭酸塩の配合量は、それを配合する発泡性ブリケット製剤の総量を基準として10〜80重量%であり、好ましくは15〜75重量%、特に20〜50重量%の範囲であることが好ましい。この範囲を下回ると、発泡力が弱く充分な香料成分の揮散が得られない。また、この範囲を超えると、保存安定性の確保が難しくなってくる。
【0016】
本発明で用いられる有機酸としては、例えば、リンゴ酸、コバク酸、フマル酸、クエン酸、酒石酸、マレイン酸、ピロリドンカルボン酸、アジピン酸、グルタミン酸、アスコルビン酸などが挙げられ、特にコハク酸、フマル酸、リンゴ酸が成形性の面で好ましい。これらの有機酸は、単独または2種以上を組み合わせて用いることができる。
【0017】
また、本発明の有機酸の配合量は、それを配合する発泡性ブリケット製剤の総量を基準として10〜80重量%であり、好ましくは15〜75重量%、特に20〜50重量%の範囲であることが好ましい。この範囲を下回ると、発泡力が弱く充分な香料成分の揮散が得られない。また、この範囲を超えると、保存安定性の確保が難しくなってくる。
【0018】
香料成分は0.05〜2重量%が好ましく、特に0.1〜1重量%が好ましい。この範囲を下回ると、香りの絶対的なボリューム感が弱く商品の魅力度も小さくなってしまい、かつロールポケットへの付着、詰まり現象の改善効果が充分発揮されず、連続生産も困難になってくる。また、この範囲を上回ると、粒子自体が固まりにくく、輸送時の振動に耐えうる粒子硬度を確保することが困難となってくる。特に香料成分の配合量が多いと、成形時の圧力によりブリケット粒子表面に現れる香料のシミ出しが見た目を悪化させると同時に、特に浴用剤などへ利用する場合、浴湯表面に香料膜が目立ち商品としても好ましくない。
【0019】
それでも吸湿性や付着性の高い原料を用いたり、そうでない原料であっても長時間、高温多湿環境下に保管しておいた場合などには、成形時にロールポケットへの付着・詰まりを生じることが多い。この場合、ブリケティングマシンのロール面に滑沢剤を付着させると、ロールポケットへの製剤の付着・詰まりをなくすことが可能である。滑沢剤としては、タルク、ステアリン酸マグネシウム、揮発性シリコーン油などが挙げられ、特に100μm以下の粒子径のタルクを用いるのが好ましい。
【0020】
付着させる方法としては、噴霧または塗布が好ましい。噴霧方法としては、加圧空気などとともに成型ロール表面に均一に吹き付ける方法が最も簡単で効率的である。また、塗布方法としては、同じく成型ロール表面に揮発性シリコーン油などを含浸させた吸収体を圧着させる方法が挙げられる。どちらの方法も一次成形体がロールから抜け、次の圧縮工程前までに行うことが、作業効率の面で好ましい。
【0021】
ブリケット製剤の全体への配合比率は、粉体など別形態の原料と同時に配合すると、1回使用あたりの均一性が担保されないが、使用量ごと個別包装すれば、この限りではない。
【0022】
また、輸送時にブリケット製剤が崩壊する「こなれ」現象については、本発明の直径、厚さを有するブリケット製剤が、使用時に製造時の95重量%以上が維持されるようにするべきである。
【0023】
ブリケット製剤の形状としては、レンズ状またはアーモンド状が好ましく、特に、レンズ状が好ましい。
【0024】
本発明のブリケット製剤の用途としては、服用する医薬品、浴用剤、芳香剤、忌避剤、健康食品、食品、家畜用飼料、肥料、洗浄剤などが挙げられる。配合する香料成分により、浴用剤、芳香剤はより香りを楽しむことができる。食品や飼料にフレーバーとして配合することで、商品価値はより高まる。また肥料には、猫や害虫などの忌避成分として配合することにより新たに忌避剤を散布する必要がないなど、本発明以外の効果も期待できる。また、これらのブリケット製剤は、粉体製剤と異なり、使用する際に飛散せずにその場にとどまり、発泡して効果を発揮するため、屋内での使用はもちろんのこと、屋外で使用するのも問題がない。また浴湯や田圃など水面に散布する場合にも濡れやすく、飛散しない。
【0025】
【実施例】
実験1
下記に示す処方の発泡性浴用剤組成物を用い、各種の大きさのブリケット状浴用剤を調製し、見た目と生産性について評価を行った。(浴用剤は、1回分(浴湯200L)として、約50gを投入する。)
【0026】
<組成物処方>
成分名 配合量(重量%)
リンゴ酸 30.0
炭酸水素ナトリウム 15.0
炭酸ナトリウム 12.5
硫酸ナトリウム 40.0
デキストリン 2.0
香料(ラベンダー) 0.5
色素 微 量
【0027】
<実験結果>
【0028】
(見た目の評価方法)
男女12人のモニターを用い、アンケート形式で見た目を評価し、その結果を集計した。
【0029】
(見た目に関するアンケート)
見た目が非常にきれい…5点
見た目がきれい …4点
気にならない程度 …3点
少し見栄えが悪い …2点
見栄えが非常に悪い …1点
【0030】
(評価基準)
上記アンケート結果を集計して、下記判定基準をもって評価した。
平均点5 〜4.5 … ◎
平均点4.5〜3.5 … ○
平均点3.5〜2.5 … △
平均点2.5〜1.5 … ×
平均点1.5〜1 … ××
【0031】
(生産性評価)
上記組成物20Kgをブリケティングマシンに供給し連続的に成形した場合、ロールポケットへの付着・詰まり具合を目視にて評価する。
【0032】
(評価基準)
ポケットへの付着・詰まりが全く認められない … ◎
ポケットへ若干の付着が認められたが自然に剥離した … ○
製剤が数カ所のポケットに詰まった … △
製剤の供給と共に、徐々にポケットへの詰まりが生じた … ×
製剤を供給したと同時にポケットへの詰まりが生じた … ××
【0033】
実験2
下記に示すトイレ用消臭芳香剤組成物を、ブリケッティングマシンを用いて試作し、滑沢剤使用による生産性向上の効果を評価した。
【0034】
<トイレ用消臭芳香剤>
水洗トイレの水を流した後、ブリケットタイプの消臭芳香剤約5gを便器に投入する。便器内で勢いよく発泡し爽快なローズの香りがトイレ中に広がると同時に、お茶の成分の消臭効果により、快適な使用感が得られる。
【0035】
<組成物処方>
【0036】
(生産性評価結果)
上記組成物10Kgをブリケティングマシンに供給し連続的に成形した場合、各条件でのロールポケットへの付着・詰まり具合を目視にて評価する。
【0037】
ブリケット形状(直径;4.8mm、厚さ;4.2mm、レンズ状)
【0038】
(評価基準)
ポケットへの付着・詰まりが全く認められない … ◎
ポケットへ若干の付着が認められたが自然に剥離した … ○
製剤が数カ所のポケットに詰まった … △
製剤の供給と共に、徐々にポケットへの詰まりが生じた … ×
製剤を供給したと同時にポケットへの詰まりが生じた … ××
【0039】
実施例9 浴用剤
万能混合攪拌機を用い下記粉体原料を均一に混合した後、予め均一に混合した液体原料を加え、粉体製剤を得る。更に、この粉体製剤をブリケッティングマシンで成形、粉砕、篩別し、直径4.8mm、厚さ4.2mmのレンズ状のブリケットタイプ浴用剤を得た。本ブリケットタイプの製剤は、生産性に何ら問題がなく、見た目にも優れた浴用剤であった。
【0040】
得られたブリケットタイプ浴用剤約50gを、200Lの浴湯の中に投入すると、浴湯表面で勢いよく発泡しユズの香りが浴室中に広がることにより、アロマテラピー効果が得られた。
【0041】
成分名 配合量(重量%)
フマル酸 30.0
炭酸水素ナトリウム 20.0
炭酸ナトリウム 15.0
硫酸ナトリウム 20.0
デキストリン 13.9
香料(ユズ) 0.5
ホホバ油 0.1
リボフラビン 微 量
チンピ抽出末 0.5
【0042】
実施例10 忌避芳香剤
万能混合攪拌機を用い下記粉体原料を均一に混合した後、予め均一に混合した液体原料を加え、粉体製剤を得る。更に、この粉体製剤をブリケッティングマシンで成形、粉砕、篩別し、直径6.6mm、厚さ5.2mmのアーモンド状のブリケットタイプ忌避芳香剤を得た。本ブリケットタイプの製剤は、生産性に何ら問題がなく、見た目にも優れた忌避芳香剤であった。
【0043】
得られたブリケットタイプ忌避芳香剤約10gを、250mLの水を溜めたポットの中に投入すると、勢いよく発泡し、蚊に対して忌避効果を有するカレンソウエッセンシャルオイルを部屋中に揮散させることができた。更に、嗜好性の低いカレンソウエッセンシャルオイルの香りをペパーミント調香料でマスキングすることにより、多くの人に受け入れられる嗜好性の高い商品とすることが可能となった。
【0044】
成分名 配合量(重量%)
コハク酸 40.0
炭酸水素ナトリウム 33.0
炭酸カリウム 20.0
ポリエチレングリコール 5.0
ケイ酸カルシウム 0.5
カレンソウエッセンシャルオイル 1.0
香料(ペパーミント) 0.5
【0045】
実施例11 健康食品
万能混合攪拌機を用い下記粉体原料を均一に混合した後、予め均一に混合した液体原料を加え、粉体製剤を得る。更に、この粉体製剤をブリケッティングマシンで成形、粉砕、篩別し、直径9.4mm、厚さ8.8mmのアーモンド状のブリケットタイプ健康食品を得た。本ブリケットタイプの製剤は、生産性に何ら問題がなく、見た目にも優れた健康食品であった。
【0046】
得られた健康食品1粒を水と一緒に口の中に含むと、発泡しながら爽やかな香りが感じられ、ショウガやニンニクの臭いが気にならない飲み口に優れたものであった。
【0047】
成分名 配合量(重量%)
アスコルビン酸 10.0
無水クエン酸 34.0
炭酸水素ナトリウム 20.0
炭酸ナトリウム 16.0
還元麦芽糖水飴 15.0
ショウガ抽出末 1.0
無臭ニンニク抽出末 0.5
食物繊維 3.0
香料(グレープフルーツフレーバー) 0.5
【0048】
実施例12 パイプクリーナー
万能混合攪拌機を用い下記粉体原料を均一に混合した後、予め均一に混合した液体原料を加え、粉体製剤を得る。更に、この粉体製剤をブリケッティングマシンで成形、粉砕、篩別し、直径3.8mm、厚さ3.2mmのレンズ状のブリケットタイプパイプクリーナーを得た。尚、ブリケティングマシンによる成形時には、滑沢剤として100μm以下に整粒したタルクをロール面に噴霧して試作を行った。本ブリケットタイプの製剤は、生産性に何ら問題がなく、見た目にも優れたパイプクリーナーであった。
【0049】
得られたパイプクリーナー約20gを、洗面所の排水口に投入すると、排水口内の水と反応して勢いよく発泡しながら、排水口内の汚れを落とした。同時に、レモンの香りが洗面所に広がり、排水口から出てくる嫌な臭いをマスキングして気にならない状態となった。
【0050】
成分名 配合量(重量%)
無水クエン酸 34.0
炭酸水素ナトリウム 20.0
炭酸ナトリウム 16.0
硫酸ナトリウム 20.0
ラウリル硫酸ナトリウム 7.5
無水ケイ酸 1.5
ヤシ油アルキルジメチルアミンオキシド 0.5
香料(レモン) 0.5
【0051】
実施例13 忌避性肥料
万能混合攪拌機を用い、下記粉体原料を均一に混合した後、予め均一に混合した液体原料を加え、粉体製剤を得る。さらに、この粉体製剤をブリケッティングマシンで成形、粉砕、篩分し、直径4.8mm、厚さ4.0mmのレンズ場のブリケットタイプ忌避性肥料を得た。本ブリケットタイプの製剤は、生産性に何ら問題がなく、見た目にも優れた忌避性肥料であった。
【0052】
得られたブリケットタイプ忌避性肥料を、畑1km2 当たり30kgの割合で散布したところ、土中の水分や降雨によって、時間をかけて発泡し、鳥害を防ぐことができた。また散布の方法も簡便であり、植物の生育にも好ましいものであった。
【0053】
成分名 配合量(重量%)
リンゴ酸 35.0
炭酸水素ナトリウム 15.0
炭酸ナトリウム 20.0
消石灰 10.0
生薬抽出残滓堆肥物 10.0
ゼオライト 5.0
香料 5.0
【0054】
なお、香料は桂皮オイル、シンナミックアルデヒド、シンナミックアルコール、d−リモネン、ターピネオール、レモングラスオイル、メチルノニルケトン、メチルフェニルケトン、青葉アルコール、青葉アルデヒド、メントール、シトラール、シトロネラール、シトロネロール、リナロール、パインオイル等の忌避効果の高い香料成分を適宜配合した。
【0055】
【発明の効果】
本発明によれば、粒子形状の見た目が良好で商品価値が高く、かつ、発泡時に香料成分が容易に揮散する発泡性ブリケット製剤が得られ、かつ該製剤を容易に製造することができる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a briquette preparation and a method for producing the same, and more specifically, a foamable briquette preparation having a good particle shape appearance and high commercial value, and in which a fragrance component easily volatilizes during foaming, and the preparation can be easily obtained. It relates to a manufacturing method that can be used.
[0002]
[Prior art]
The briquette preparation of the present invention means a briquette preparation obtained by molding and processing a powder composition with a briquetting machine. A briquetting machine is a dry compression granulator that compresses and molds raw material powder between two rolls rotating in the opposite directions at the same speed. A pocket that is a mother mold is engraved. Depending on the shape and size of the pocket, briquettes of various shapes and sizes can be obtained. Briquettes can be made in the shape of pillows, lenses, almonds, prisms, rods, fingers, etc., and the size of briquettes of about 0.3cc to 200cc can be manufactured. . Usually, in briquette production, a sheet-like primary molded body is obtained by adjusting the clearance between rolls, the pressing pressure between rolls, the pressing force of a feed screw, and the like. The briquette can be obtained by further crushing a sheet-like primary molded body in which the plurality of briquette particles are formed into a sheet shape via the connecting portion. In other words, during the work process of manufacturing briquettes, a process of crushing is necessarily taken, and “chips” and “burrs” in the particle shape are inevitably generated.
[0003]
In general, briquettes are handled as intermediate products obtained by molding raw materials in order to improve work and environmental problems and improve reaction efficiency in chemical, ceramics, refining, and fertilizer industrial fields. In the past, there have been few problems with regard to the appearance of preparations such as “chips” and “burrs” in the particle shape. On the other hand, for the purpose of improving the appearance, it has also been proposed to obtain a briquette preparation with less burr by providing a rolling process, but it is considered difficult to actually improve the appearance of the briquette preparation by 100%. I have been given up.
[0004]
However, when it is a final product that can be seen by consumers in stores and in actual use, the appearance of the briquette is also an important factor that affects the value of the product, and improvements related to this appearance have been cited as an issue for briquette formulations. .
[0005]
Specifically, when trying to obtain large briquette particles, many “chips” occur in the particle body at the same time as the deburring operation during crushing, and when trying to obtain small briquette particles, It was difficult to completely remove the “burr”, and it was impossible to produce a product with a clean particle shape. That is, in either case, there is a problem that a product that satisfies the appearance cannot be obtained.
[0006]
Furthermore, when manufacturing briquette preparations, some of the raw materials used tend to cause powder sticking or clogging in the pockets of the roll during compression molding, and this has been pointed out as a problem that production efficiency is significantly reduced. It has been. In particular, when manufacturing a preparation that contains ingredients that increase adhesion due to moisture in the air, such as water-soluble polymers, carbonates and organic acids, there is a tendency for adhesion to pockets and powder clogging to occur frequently. It was recognized and was a problem at the time of manufacture. When powder is stuck in the pocket of the roll, the briquette particles cannot be obtained, and each time the powder is packed in the pocket, the roll needs to be washed and cleaned, making continuous production impossible. Improvements in production efficiency have been demanded.
[0007]
[Problems to be solved by the invention]
An object of the present invention is to provide a foamable briquette preparation having a uniform particle shape, good appearance, and a fragrance component that easily evaporates at the time of foaming and excellent in production efficiency.
[0008]
[Means for Solving the Problems]
As a result of intensive studies to solve the above problems, the present inventors have determined that briquette particles have a particle diameter within a certain range in a bath preparation containing a carbonate, an organic acid and a fragrance component. It has been found that a preparation can be obtained efficiently. Furthermore, when manufacturing the above briquette preparations, by attaching a lubricant to the roll surface, there is no adhesion or clogging of powder to the roll pocket of the briquetting machine, and production with high production efficiency becomes possible. As a result, the present invention has been completed.
[0009]
That is, the present invention
(1) An effervescent briquette preparation comprising carbonate, an organic acid and a fragrance as essential components, and having a diameter of 3 to 10 mm and a thickness of 2.5 to 10 mm.
(2) The briquette preparation according to (1), which is a bath preparation.
(3) The method for producing a briquette preparation according to (1) or (2), wherein a lubricant is adhered to the roll surface of the briquetting machine.
About.
[0010]
The thickness of the briquette means the length in the vertical direction of the sheet-like primary molded body, and the thickness is preferably 2.5 to 10 mm, particularly 3 to 8 mm. Below this range, the boundary between briquette particles and “burrs” is not clear, making it difficult to maintain a clean particle shape. Beyond this range, the removal of the formulation from the roll pocket is significantly worsened, making continuous production difficult. This is not preferable.
[0011]
A diameter here means the longest diameter in the horizontal direction of a sheet-like primary molded object, and the diameter of a briquette formulation is 3-10 mm, Especially 4-8 mm is preferable. Below this range, a clean particle shape cannot be obtained even if deburring is performed during crushing, which is not preferable. On the other hand, if it exceeds this range, a large number of “chips” are generated in the particle body at the same time as the deburring operation at the time of crushing, and the commercial value is greatly reduced in terms of appearance.
[0012]
When the briquette preparation has an elliptical shape such as an almond shape, the major axis of the elliptical shape is preferably set within the upper limit of the diameter range. The elliptical minor axis is preferably included within the lower limit of the diameter range. Further, the minor axis is more preferably 1/2 or more and less than 1 of the major axis. Below this range, the finished briquette is not preferable because many broken particles are observed at the time of crushing and transportation, which is not satisfactory as a product.
[0013]
Even when the briquette preparation has a polygonal shape such as a pillow shape, the longest diameter corresponds to the major axis of the elliptical shape, and the length of the shortest side corresponds to the minor axis of the elliptical shape.
[0014]
Examples of the carbonate used in the present invention include sodium hydrogen carbonate, sodium carbonate, sodium sesquicarbonate, potassium carbonate, potassium hydrogen carbonate, magnesium carbonate, ammonium carbonate and the like, and particularly sodium hydrogen carbonate and sodium carbonate are available. It is preferable because of its ease. These carbonates can be used alone or in combination of two or more.
[0015]
The amount of the carbonate of the present invention is 10 to 80% by weight, preferably 15 to 75% by weight, particularly 20 to 50% by weight, based on the total amount of the foamable briquette preparation containing the carbonate. Preferably there is. Below this range, the foaming power is weak and sufficient perfume ingredient volatilization cannot be obtained. Moreover, if this range is exceeded, it becomes difficult to ensure storage stability.
[0016]
Examples of the organic acid used in the present invention include malic acid, succinic acid, fumaric acid, citric acid, tartaric acid, maleic acid, pyrrolidone carboxylic acid, adipic acid, glutamic acid, ascorbic acid and the like, and particularly succinic acid and fumaric acid. Acid and malic acid are preferable in terms of moldability. These organic acids can be used alone or in combination of two or more.
[0017]
Moreover, the compounding quantity of the organic acid of this invention is 10 to 80 weight% on the basis of the total amount of the foamable briquette formulation which mix | blends it, Preferably it is 15 to 75 weight%, Especially in the range of 20 to 50 weight%. Preferably there is. Below this range, the foaming power is weak and sufficient perfume ingredient volatilization cannot be obtained. Moreover, if this range is exceeded, it becomes difficult to ensure storage stability.
[0018]
The fragrance component is preferably 0.05 to 2% by weight, particularly preferably 0.1 to 1% by weight. Below this range, the absolute volume of the fragrance is weak and the attractiveness of the product is reduced, and the effect of improving adhesion to the roll pocket and clogging phenomenon is not fully demonstrated, making continuous production difficult. come. On the other hand, if it exceeds this range, the particles themselves are difficult to solidify, and it becomes difficult to ensure particle hardness that can withstand vibration during transportation. In particular, when the amount of the fragrance component is large, the appearance of the fragrance stain appearing on the surface of the briquette particles deteriorates due to the pressure during molding, and at the same time, the fragrance film is conspicuous on the surface of the bath water, especially when used for bathing agents. However, it is not preferable.
[0019]
Still, if materials that are highly hygroscopic or adherent are used, or if they are not, raw materials that are stored in a high-temperature, high-humidity environment for a long time may cause sticking or clogging in the roll pocket during molding. There are many. In this case, if a lubricant is adhered to the roll surface of the briquetting machine, it is possible to eliminate adhesion and clogging of the preparation to the roll pocket. Examples of the lubricant include talc, magnesium stearate, volatile silicone oil and the like, and it is particularly preferable to use talc having a particle size of 100 μm or less.
[0020]
As a method of attaching, spraying or coating is preferable. As a spraying method, a method of spraying uniformly on the surface of the forming roll together with pressurized air is the simplest and most efficient. Moreover, as a coating method, the method of crimping | bonding the absorber which impregnated volatile silicone oil etc. to the surface of the forming roll similarly is mentioned. In both methods, it is preferable from the viewpoint of work efficiency that the primary molded body is removed from the roll and before the next compression step.
[0021]
The blending ratio of the briquette preparation as a whole is not limited as long as it is packaged at the same time as another form of raw material such as powder, but the uniformity per use is not ensured.
[0022]
In addition, regarding the “completion” phenomenon in which the briquette preparation collapses during transportation, the briquette preparation having the diameter and thickness of the present invention should be maintained at 95% by weight or more at the time of manufacture.
[0023]
As the shape of the briquette preparation, a lens shape or an almond shape is preferable, and a lens shape is particularly preferable.
[0024]
Applications of the briquette preparation of the present invention include pharmaceuticals to be taken, bath preparations, fragrances, repellents, health foods, foods, livestock feeds, fertilizers, detergents and the like. Depending on the fragrance component to be blended, the bath agent and the fragrance can more enjoy the scent. Combining food and feed as a flavor increases the commercial value. In addition, the fertilizer can be expected to have an effect other than the present invention, for example, it is not necessary to newly spray a repellent by blending it as a repellent component such as cats and pests. In addition, unlike the powder preparations, these briquette preparations stay in place without being scattered when used, and are effective by foaming, so they are used indoors as well as outdoors. There is no problem. Also, when sprayed on the surface of a water such as a bath or rice field, it is easy to get wet and does not scatter.
[0025]
【Example】
Experiment 1
Using the foaming bath agent composition having the formulation shown below, briquette bath agents of various sizes were prepared, and the appearance and productivity were evaluated. (About 50 g of bathing agent is added as a single dose (200 L of bath water).)
[0026]
<Composition formulation>
Ingredient name Compounding amount (% by weight)
Malic acid 30.0
Sodium bicarbonate 15.0
Sodium carbonate 12.5
Sodium sulfate 40.0
Dextrin 2.0
Fragrance (lavender) 0.5
Dye amount [0027]
<Experimental result>
[0028]
(Appearance evaluation method)
Using a monitor of 12 men and women, the appearance was evaluated in a questionnaire format, and the results were tabulated.
[0029]
(Questionnaire about appearance)
Appearance is very beautiful ... 5 Appearance is beautiful ... 4 Appearance is unpleasant ... 3 Appearance is a little worse ... 2 Appearance is very poor ... 1 Appearance
(Evaluation criteria)
The questionnaire results were tabulated and evaluated according to the following criteria.
Average score 5-4.5 ... ◎
Average score 4.5-3.5… ○
Average score 3.5-2.5 ... △
Average score 2.5-1.5 ... ×
Average point 1.5 to 1 ... XX
[0031]
(Productivity evaluation)
When 20 kg of the composition is supplied to a briquetting machine and continuously molded, the degree of adhesion and clogging to the roll pocket is visually evaluated.
[0032]
(Evaluation criteria)
There is no adhesion or clogging in the pocket.
Slight adhesion to the pocket was observed, but it peeled naturally… ○
The drug product is stuck in several pockets… △
The clogging of the pockets gradually occurred with the supply of the drug… ×
At the same time as the drug product was supplied, clogging occurred in the pocket.
[0033]
Experiment 2
The toilet deodorant fragrance composition shown below was prototyped using a briquetting machine, and the effect of improving productivity by using a lubricant was evaluated.
[0034]
<Deodorant fragrance for toilet>
After flushing water from the flush toilet, about 5 g of briquette deodorant fragrance is put into the toilet bowl. A refreshing rose fragrance spreads in the toilet, and at the same time a comfortable feeling of use is obtained due to the deodorizing effect of the tea components.
[0035]
<Composition formulation>
[0036]
(Productivity evaluation results)
When 10 kg of the composition is supplied to a briquetting machine and continuously molded, the degree of adhesion and clogging to the roll pocket under each condition is visually evaluated.
[0037]
Briquette shape (diameter: 4.8 mm, thickness: 4.2 mm, lens shape)
[0038]
(Evaluation criteria)
There is no adhesion or clogging in the pocket.
Slight adhesion to the pocket was observed, but it peeled naturally… ○
The drug product is stuck in several pockets… △
The clogging of the pockets gradually occurred with the supply of the drug… ×
At the same time as the drug product was supplied, clogging occurred in the pocket.
[0039]
Example 9 A powder preparation is obtained by uniformly mixing the following powder raw materials with a universal mixing stirrer for bathing agents and then adding a liquid raw material uniformly mixed in advance. Further, this powder preparation was molded, pulverized and sieved with a briquetting machine to obtain a lens-shaped briquette-type bath preparation having a diameter of 4.8 mm and a thickness of 4.2 mm. This briquette type preparation had no problem in productivity and was an excellent bath preparation.
[0040]
When about 50 g of the obtained briquette-type bath agent was put into 200 L of bath water, an aromatherapy effect was obtained by vigorously foaming on the surface of the bath water and spreading the scent of yuzu into the bathroom.
[0041]
Ingredient name Compounding amount (wt%)
Fumaric acid 30.0
Sodium bicarbonate 20.0
Sodium carbonate 15.0
Sodium sulfate 20.0
Dextrin 13.9
Fragrance (Yuzu) 0.5
Jojoba oil 0.1
Riboflavin Fine powder extract 0.5
[0042]
Example 10 The following powder raw materials are uniformly mixed using a repellent fragrance universal mixing stirrer, and then a liquid raw material uniformly mixed in advance is added to obtain a powder preparation. Further, this powder preparation was molded, pulverized and sieved with a briquetting machine to obtain an almond-shaped briquette type repellent fragrance having a diameter of 6.6 mm and a thickness of 5.2 mm. This briquette type preparation had no problem in productivity and was an excellent repellent fragrance.
[0043]
When about 10 g of the obtained briquette-type repellent fragrance is put into a pot in which 250 mL of water is stored, it can foam vigorously and volatilize the calenso wet oil that has a repellent effect against mosquitoes in the room. It was. Furthermore, by masking the fragrance of the less-priced carroto essential oil with a peppermint-like fragrance, it has become possible to obtain a highly-preferred product that can be accepted by many people.
[0044]
Ingredient name Compounding amount (wt%)
Succinic acid 40.0
Sodium bicarbonate 33.0
Potassium carbonate 20.0
Polyethylene glycol 5.0
Calcium silicate 0.5
Carenso Westin Oil 1.0
Fragrance (Peppermint) 0.5
[0045]
Example 11 The following powder raw materials are uniformly mixed using a health food universal mixing stirrer, and then a liquid raw material uniformly mixed in advance is added to obtain a powder preparation. Further, this powder preparation was molded, pulverized and sieved with a briquetting machine to obtain an almond-shaped briquette type health food having a diameter of 9.4 mm and a thickness of 8.8 mm. This briquette type preparation had no problem in productivity and was a health food excellent in appearance.
[0046]
When one of the obtained health foods was included in the mouth together with water, the refreshing scent was felt while foaming, and it was excellent in a drinking mouth that did not bother the smell of ginger and garlic.
[0047]
Ingredient name Compounding amount (% by weight)
Ascorbic acid 10.0
Citric anhydride 34.0
Sodium bicarbonate 20.0
Sodium carbonate 16.0
Reduced maltose starch syrup 15.0
Ginger extract powder 1.0
Odorless garlic extract powder 0.5
Dietary fiber 3.0
Fragrance (Grapefruit Flavor) 0.5
[0048]
Example 12 The following powder raw materials are uniformly mixed using a pipe cleaner universal mixing stirrer, and then a liquid raw material uniformly mixed in advance is added to obtain a powder preparation. Further, this powder preparation was molded, pulverized, and sieved with a briquetting machine to obtain a lens-shaped briquette type pipe cleaner having a diameter of 3.8 mm and a thickness of 3.2 mm. At the time of molding by a briquetting machine, talc adjusted to 100 μm or less as a lubricant was sprayed on the roll surface to make a prototype. This briquette type preparation had no problem in productivity and was an excellent pipe cleaner.
[0049]
When about 20 g of the obtained pipe cleaner was put into the drain outlet of the toilet, the dirt in the drain outlet was removed while reacting with the water in the drain outlet and foaming vigorously. At the same time, the scent of lemon spread in the bathroom, masking the unpleasant odor coming out of the drain outlet, and becoming unconscious.
[0050]
Ingredient name Compounding amount (% by weight)
Citric anhydride 34.0
Sodium bicarbonate 20.0
Sodium carbonate 16.0
Sodium sulfate 20.0
Sodium lauryl sulfate 7.5
Silica anhydride 1.5
Coconut oil alkyldimethylamine oxide 0.5
Fragrance (lemon) 0.5
[0051]
Example 13 A repellent fertilizer universal mixing stirrer is used to uniformly mix the following powder raw materials, and then a liquid raw material uniformly mixed in advance is added to obtain a powder formulation. Further, this powder preparation was molded, pulverized and sieved with a briquetting machine to obtain a briquette type repellent fertilizer with a lens field of 4.8 mm in diameter and 4.0 mm in thickness. This briquette type preparation had no problem in productivity and was an excellent repellent fertilizer.
[0052]
When the obtained briquette type repellent fertilizer was sprayed at a rate of 30 kg per 1 km 2 of field, it was foamed over time due to moisture in the soil and rainfall, and bird damage could be prevented. Also, the spraying method was simple and preferred for plant growth.
[0053]
Ingredient name Compounding amount (% by weight)
Malic acid 35.0
Sodium bicarbonate 15.0
Sodium carbonate 20.0
Slaked lime 10.0
Crude drug extraction residue compost 10.0
Zeolite 5.0
Fragrance 5.0
[0054]
In addition, perfume is cinnamon oil, cinnamic aldehyde, cinnamic alcohol, d-limonene, terpineol, lemongrass oil, methyl nonyl ketone, methyl phenyl ketone, green leaf alcohol, green leaf aldehyde, menthol, citral, citronellal, citronellol, linalool, pine Perfume ingredients with high repellent effect such as oil were appropriately blended.
[0055]
【The invention's effect】
ADVANTAGE OF THE INVENTION According to this invention, the foam shape briquette formulation which the appearance of a particle shape is favorable, has a high commercial value, and a fragrance | flavor component volatilizes easily at the time of foaming is obtained, and this formulation can be manufactured easily.
Claims (3)
Priority Applications (2)
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JP2002157816A JP4100964B2 (en) | 2002-05-30 | 2002-05-30 | Briquette preparation and method for producing the same |
CN03138231A CN1461668A (en) | 2002-05-30 | 2003-05-29 | Block preparation and preparing method thereof |
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JP2002157816A JP4100964B2 (en) | 2002-05-30 | 2002-05-30 | Briquette preparation and method for producing the same |
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JP2003342164A JP2003342164A (en) | 2003-12-03 |
JP4100964B2 true JP4100964B2 (en) | 2008-06-11 |
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Cited By (1)
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JP2013253056A (en) * | 2012-06-08 | 2013-12-19 | Bathclin Corp | Foaming briquette formulation |
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JP4826884B2 (en) * | 2005-08-19 | 2011-11-30 | 株式会社バスクリン | Briquette machine for producing solid bath agent and method for producing solid bath agent |
KR20090015954A (en) * | 2006-06-07 | 2009-02-12 | 노파르티스 아게 | Method for producing multiparticulates using a roller compactor |
KR100969323B1 (en) * | 2010-01-22 | 2010-07-09 | 화광 교역 주식회사 | Skin cleaning agent having excellent water-soluble |
JP6209323B2 (en) * | 2012-10-12 | 2017-10-04 | 花王株式会社 | Effervescent compression formulation |
JP6075759B2 (en) * | 2013-01-16 | 2017-02-08 | シオノギヘルスケア株式会社 | Briquette formulation |
-
2002
- 2002-05-30 JP JP2002157816A patent/JP4100964B2/en not_active Expired - Fee Related
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JP2013253056A (en) * | 2012-06-08 | 2013-12-19 | Bathclin Corp | Foaming briquette formulation |
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