JP2016098293A - Method for producing milled soap - Google Patents
Method for producing milled soap Download PDFInfo
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- JP2016098293A JP2016098293A JP2014235612A JP2014235612A JP2016098293A JP 2016098293 A JP2016098293 A JP 2016098293A JP 2014235612 A JP2014235612 A JP 2014235612A JP 2014235612 A JP2014235612 A JP 2014235612A JP 2016098293 A JP2016098293 A JP 2016098293A
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- soap
- fatty acid
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- sodium salt
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- 239000000344 soap Substances 0.000 title claims abstract description 81
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 66
- 239000000194 fatty acid Substances 0.000 claims abstract description 66
- 229930195729 fatty acid Natural products 0.000 claims abstract description 66
- 239000000203 mixture Substances 0.000 claims abstract description 29
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000004898 kneading Methods 0.000 claims abstract description 12
- 239000005639 Lauric acid Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000002844 melting Methods 0.000 claims abstract description 7
- 230000008018 melting Effects 0.000 claims abstract description 6
- 150000004671 saturated fatty acids Chemical class 0.000 claims abstract description 6
- -1 fatty acid sodium salt Chemical class 0.000 claims description 46
- 125000004432 carbon atom Chemical group C* 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 9
- 238000005187 foaming Methods 0.000 abstract description 20
- 150000004665 fatty acids Chemical group 0.000 description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 10
- 239000013078 crystal Substances 0.000 description 8
- 230000008961 swelling Effects 0.000 description 8
- 238000001556 precipitation Methods 0.000 description 7
- 235000019482 Palm oil Nutrition 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000002540 palm oil Substances 0.000 description 6
- 239000011780 sodium chloride Substances 0.000 description 5
- 239000006260 foam Substances 0.000 description 4
- 239000003346 palm kernel oil Substances 0.000 description 4
- 235000019865 palm kernel oil Nutrition 0.000 description 4
- 239000008399 tap water Substances 0.000 description 4
- 235000020679 tap water Nutrition 0.000 description 4
- 239000004677 Nylon Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 229920001778 nylon Polymers 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- JUQGWKYSEXPRGL-UHFFFAOYSA-M sodium;tetradecanoate Chemical compound [Na+].CCCCCCCCCCCCCC([O-])=O JUQGWKYSEXPRGL-UHFFFAOYSA-M 0.000 description 3
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 3
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- TWJNQYPJQDRXPH-UHFFFAOYSA-N 2-cyanobenzohydrazide Chemical compound NNC(=O)C1=CC=CC=C1C#N TWJNQYPJQDRXPH-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 235000021360 Myristic acid Nutrition 0.000 description 2
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 239000003925 fat Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- BTURAGWYSMTVOW-UHFFFAOYSA-M sodium dodecanoate Chemical compound [Na+].CCCCCCCCCCCC([O-])=O BTURAGWYSMTVOW-UHFFFAOYSA-M 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- CZIBPNKKMSNWQH-UHFFFAOYSA-N (2-chloroquinolin-4-yl)-morpholin-4-ylmethanone Chemical compound C=12C=CC=CC2=NC(Cl)=CC=1C(=O)N1CCOCC1 CZIBPNKKMSNWQH-UHFFFAOYSA-N 0.000 description 1
- DCXXMTOCNZCJGO-UHFFFAOYSA-N Glycerol trioctadecanoate Natural products CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 235000015278 beef Nutrition 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 235000019864 coconut oil Nutrition 0.000 description 1
- 239000003240 coconut oil Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019197 fats Nutrition 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 235000014593 oils and fats Nutrition 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229940082004 sodium laurate Drugs 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 235000019871 vegetable fat Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
Abstract
Description
本発明は、機械練り石鹸の製造方法に関する。 The present invention relates to a method for producing mechanically kneaded soap.
従来、機械練り石鹸は、製造のしやすさ、製造コストの低減から、汎用の石鹸素地を用いて製造されることが多い。しかし、石鹸素地をそのまま石鹸に応用すると、石鹸素地に含まれる脂肪酸の組成がそのまま石鹸の性能に反映されるため、泡立ちやざらつきなどの使用性などで、充分な性能が得られない場合がある。これを改善するためには、石鹸素地に他の脂肪酸を追加で添加することや、特定の製造方法を応用することなどが考えられる。しかしながら、その場合であっても、泡立ち、使用性などの全ての性能を必ずしも満足できるものではなかった。 Conventionally, machine-kneaded soap is often manufactured using a general-purpose soap base because it is easy to manufacture and reduces manufacturing costs. However, if the soap base is applied to soap as it is, the composition of the fatty acid contained in the soap base is directly reflected in the performance of the soap. . In order to improve this, it is conceivable to add another fatty acid to the soap base or to apply a specific production method. However, even in that case, all performances such as foaming and usability were not always satisfactory.
例えば、特許文献1には、パーム核脂肪酸塩とパームステアリン脂肪酸塩とを特定の比率で含有し、さらに高級脂肪酸を加えることにより、泡立ちを向上させた石鹸組成物が記載されている。しかしながら、この石鹸組成物は、泡立ちは向上するものの、低温で使用したときに、石鹸表面にざらつきが感じられた。
また、特許文献2には、ざらつきのない石鹸を製造することができる石鹸の製造方法が記載されている。しかしながら、この方法により得られる石鹸は、ざらつきが改善されるものの、特別な製造設備が必要で、手間とコストがかかってしまう。
For example, Patent Document 1 describes a soap composition containing a palm kernel fatty acid salt and a palm stearin fatty acid salt in a specific ratio and further improving foaming by adding a higher fatty acid. However, this soap composition improved lathering, but when used at a low temperature, the soap surface was rough.
Patent Document 2 describes a method for producing soap that can produce a rough soap. However, the soap obtained by this method is improved in roughness, but requires special production equipment, and takes time and cost.
本発明は、特別な製造設備等を必要とせず、製造の手間がかからず、泡立ちに優れ、使用時にざらつきのない、高い硬度を有する石鹸の製造方法に関する。 The present invention relates to a method for producing a soap having a high hardness that does not require special production equipment and the like, does not require time for production, is excellent in foaming, and is not rough during use.
本発明者らは、炭素数8〜22の脂肪酸ナトリウム塩に、ラウリン酸を80質量%以上含む炭素数12〜18の飽和脂肪酸を加熱溶融して加えることにより、泡立ちに優れ、使用時にざらつきのない、高い硬度を有する石鹸が得られる機械練石鹸の製造方法を見出した。 The present inventors are excellent in foaming by adding a saturated fatty acid having 12 to 18 carbon atoms containing 80% by mass or more of lauric acid to a fatty acid sodium salt having 8 to 22 carbon atoms. The present inventors have found a method for producing a mechanically kneaded soap that can obtain a soap having a high hardness.
本発明は、以下の工程を有する、機械練石鹸の製造方法に関する。
(1)(A)ラウリン酸を80質量%以上含む炭素数12〜18の飽和脂肪酸を加熱溶融する工程、
(2)工程(1)で得られた加熱溶融物と、(B)炭素数8〜22の脂肪酸ナトリウム塩を80質量%以上含む組成物とを混合して、成分(B)に成分(A)を被覆する工程、
(3)工程(2)で得られた混合物を混練する工程。
The present invention relates to a method for producing a machined soap having the following steps.
(1) (A) a step of heating and melting a saturated fatty acid having 12 to 18 carbon atoms containing 80% by mass or more of lauric acid,
(2) The heated melt obtained in step (1) and (B) a composition containing 80% by mass or more of a fatty acid sodium salt having 8 to 22 carbon atoms are mixed, and component (B) is mixed with component (A )
(3) A step of kneading the mixture obtained in step (2).
本発明によれば、特別な製造設備等を必要とせず、簡便に石鹸を製造することができ、低温及び高温での泡立ちに優れ、使用時にざらつきがなく、硬度が高く、経時での外観の白色度の低下が小さく、石鹸表面に結晶の析出がないなどの保存安定性に優れ、水で濡れた後の膨潤を抑えた石鹸を得ることができる。 According to the present invention, it is possible to easily produce soap without the need for special production equipment, etc., excellent foaming at low and high temperatures, no roughness during use, high hardness, and appearance over time. It is possible to obtain a soap having a small decrease in whiteness, excellent storage stability such as no crystal precipitation on the soap surface, and suppressing swelling after being wet with water.
[工程(1)]
本発明の工程(1)は、(A)ラウリン酸を80質量%以上含む炭素数12〜18の飽和脂肪酸を加熱溶融する工程である。
成分(A)は、洗浄時の泡立ちを高めるために用いられ、パーム核油、ヤシ油等の植物性油脂から得られるものを用いることもできる。低温での泡立ちの向上、経時での外観の白色度の低下を小さくさせる観点から、成分(A)中のラウリン酸の含有量は、83質量%以上が好ましく、85質量%以上がより好ましく、90質量%以上がさらに好ましく、95質量%以上がさらにより好ましく、99質量%以上が特に好ましく、実質100質量%が最も好ましい。
[Step (1)]
Step (1) of the present invention is (A) a step of heating and melting a saturated fatty acid having 12 to 18 carbon atoms containing 80% by mass or more of lauric acid.
A component (A) is used in order to raise foaming at the time of washing | cleaning, and what can be obtained from vegetable oils and fats, such as palm kernel oil and palm oil, can also be used. From the viewpoint of improving foaming at low temperature and reducing the decrease in whiteness of the appearance over time, the content of lauric acid in the component (A) is preferably 83% by mass or more, more preferably 85% by mass or more, 90 mass% or more is further more preferable, 95 mass% or more is further more preferable, 99 mass% or more is especially preferable, and substantially 100 mass% is the most preferable.
成分(A)は、後記成分(B)と混合される前に、予め加熱溶融される。加熱溶融することで、成分(B)と均一に混合され、低温及び高温での泡立ちに優れ、使用時にざらつきのない、経時での外観の白色度の低下が小さく、石鹸表面に結晶の析出がない石鹸を得ることができる。
成分(A)を加熱溶融する際の温度は、40℃以上が好ましく、41〜80℃がより好ましく、42〜60℃がさらに好ましい。この加熱溶融は、成分(A)を、加熱器の設置された容器に投入し、前記温度範囲に加熱器の温度を設定して行うことができる。
The component (A) is heated and melted in advance before being mixed with the component (B) described later. By heating and melting, it is uniformly mixed with the component (B), has excellent foaming at low and high temperatures, has no roughness during use, has a small decrease in whiteness of appearance over time, and crystals are deposited on the soap surface. You can get no soap.
40 degreeC or more is preferable, as for the temperature at the time of heat-melting a component (A), 41-80 degreeC is more preferable, and 42-60 degreeC is further more preferable. This heating and melting can be carried out by putting the component (A) into a container provided with a heater and setting the temperature of the heater within the temperature range.
本発明において、成分(A)は、不飽和脂肪酸を含んだ状態で用いても良い。不飽和脂肪酸としては、炭素数16〜18のものが挙げられ、炭素数18のものがより好ましい。
本発明により得られる石鹸において、不飽和脂肪酸の含有量は、低温での泡立ち、石鹸硬度を向上させる観点から、0.4質量%以下が好ましく、0.01〜0.3質量%がより好ましく、0.01〜0.25質量%がさらに好ましい。
In the present invention, the component (A) may be used in a state containing an unsaturated fatty acid. As unsaturated fatty acid, a C16-C18 thing is mentioned, A C18 thing is more preferable.
In the soap obtained by the present invention, the content of unsaturated fatty acid is preferably 0.4% by mass or less, more preferably 0.01 to 0.3% by mass from the viewpoint of improving foaming at low temperature and soap hardness. 0.01 to 0.25% by mass is more preferable.
[工程(2)]
本発明の工程(2)は、工程(1)で得られた成分(A)の加熱溶融物と、(B)炭素数8〜22の脂肪酸ナトリウム塩を80質量%以上含む組成物とを混合して、成分(B)に成分(A)を被覆する工程である。
成分(B)において、低温及び高温の泡立ちを向上させ、水で濡れた後の石鹸の膨潤を抑える観点から、炭素数8〜22の脂肪酸ナトリウム塩(b1)の含有量は、80質量%以上であり、80〜94質量%が好ましく、82〜92質量%がより好ましく、84〜90質量%がさらに好ましい。
[Step (2)]
In the step (2) of the present invention, the heated melt of the component (A) obtained in the step (1) and (B) a composition containing 80% by mass or more of a fatty acid sodium salt having 8 to 22 carbon atoms are mixed. In this step, the component (B) is coated with the component (A).
In the component (B), the content of the fatty acid sodium salt (b1) having 8 to 22 carbon atoms is 80% by mass or more from the viewpoint of improving low-temperature and high-temperature foaming and suppressing swelling of the soap after being wet with water. 80 to 94 mass% is preferable, 82 to 92 mass% is more preferable, and 84 to 90 mass% is still more preferable.
また、炭素数8〜22の脂肪酸ナトリウム塩(b1)は、得られる石鹸の泡立ちを向上させる観点、石鹸硬度を高め、水で濡れた後の石鹸の膨潤を抑える観点から、ラウリン酸ナトリウム塩、ミリスチン酸ナトリウム塩のいずれか1種を含むことが好ましく、ラウリン酸ナトリウム塩とミリスチン酸ナトリウム塩の両方を含むことがより好ましい。
炭素数8〜22の脂肪酸ナトリウム塩(b1)に含まれる、ラウリン酸ナトリウム塩の含有量は、同様の観点から、5〜28質量%が好ましく、9〜25質量%がより好ましく、14〜22質量%がさらに好ましい。
また、炭素数8〜22の脂肪酸ナトリウム塩(b1)に含まれる、ミリスチン酸ナトリウム塩の含有量は、1〜12質量%が好ましく、3〜10質量%がより好ましく、5〜8質量%がさらに好ましい。
The fatty acid sodium salt having 8 to 22 carbon atoms (b1) is a sodium laurate salt from the viewpoint of improving foaming of the obtained soap, from the viewpoint of increasing soap hardness and suppressing swelling of the soap after being wet with water, It is preferable to include any one of myristic acid sodium salt, and it is more preferable to include both lauric acid sodium salt and myristic acid sodium salt.
From the same viewpoint, the content of sodium laurate contained in the fatty acid sodium salt (b1) having 8 to 22 carbon atoms is preferably 5 to 28% by mass, more preferably 9 to 25% by mass, and 14 to 22%. More preferred is mass%.
The content of myristic acid sodium salt contained in the fatty acid sodium salt (b1) having 8 to 22 carbon atoms is preferably 1 to 12% by mass, more preferably 3 to 10% by mass, and 5 to 8% by mass. Further preferred.
成分(B)における炭素数8〜22の脂肪酸ナトリウム塩(b1)は、牛脂、ヤシ油、パーム油、パーム核油等の油脂を加水分解して得られる脂肪酸を水酸化ナトリウム水溶液で中和するか、油脂を直接けん化することによって得ることができる。
炭素数8〜22の脂肪酸ナトリウム塩(b1)は、得られる石鹸の泡立ち及び硬度を向上させる観点から、炭素数12以下の脂肪酸ナトリウム塩を主成分とする脂肪酸ナトリウム塩と、炭素数14以上の脂肪酸ナトリム塩を主成分とする脂肪酸ナトリウム塩を含むことが好ましい。本発明において、主成分とは、炭素数12以下の脂肪酸ナトリウム塩を主成分とする脂肪酸ナトリウム塩においては、炭素数12以下の脂肪酸ナトリム塩の含有量が、炭素数13以上の脂肪酸ナトリム塩の含有量よりも多いことを意味し、炭素数14以上の脂肪酸ナトリウム塩を主成分とする脂肪酸ナトリウム塩においては、炭素数14以上の脂肪酸ナトリム塩の含有量が、炭素数13以下の脂肪酸ナトリム塩の含有量よりも多いことを意味する。
炭素数12以下の脂肪酸ナトリウム塩を主成分とする脂肪酸ナトリウム塩としては、パーム核油から得られるパーム核脂肪酸を、炭素数14以上の脂肪酸ナトリム塩を主成分とする肪酸ナトリウム塩はパーム油から得られるパーム脂肪酸を原料としたものを使用することができる。
The fatty acid sodium salt (b1) having 8 to 22 carbon atoms in the component (B) neutralizes fatty acids obtained by hydrolyzing fats such as beef tallow, coconut oil, palm oil, and palm kernel oil with an aqueous sodium hydroxide solution. Alternatively, it can be obtained by directly saponifying oils and fats.
The fatty acid sodium salt (b1) having 8 to 22 carbon atoms is a fatty acid sodium salt mainly composed of a fatty acid sodium salt having 12 or less carbon atoms, and 14 or more carbon atoms from the viewpoint of improving foaming and hardness of the soap obtained. It is preferable that the fatty acid sodium salt which has fatty acid sodium salt as a main component is included. In the present invention, the main component is a fatty acid sodium salt mainly composed of a fatty acid sodium salt having 12 or less carbon atoms, and the content of the fatty acid sodium salt having 12 or less carbon atoms is a fatty acid sodium salt having 13 or more carbon atoms. In the fatty acid sodium salt whose main component is a fatty acid sodium salt having 14 or more carbon atoms, the content of the fatty acid sodium salt having 14 or more carbon atoms is a fatty acid sodium salt having 13 or less carbon atoms. It means that there is more content than.
The fatty acid sodium salt mainly containing a fatty acid sodium salt having 12 or less carbon atoms is a palm kernel fatty acid obtained from palm kernel oil, and the sodium fatty acid salt mainly containing a fatty acid sodium salt having 14 or more carbon atoms is palm oil. What used the palm fatty acid obtained from this as a raw material can be used.
また、同様の観点から、炭素数14以上の脂肪酸ナトリム塩を主成分とする脂肪酸ナトリウム塩の含有量に対する、炭素数12以下の脂肪酸ナトリム塩を主成分とする脂肪酸ナトリウム塩の質量割合([炭素数12以下の脂肪酸ナトリム塩を主成分とする脂肪酸ナトリウム塩]/[炭素数14以上の脂肪酸ナトリム塩]を主成分とする脂肪酸ナトリウム塩)は、成分(B)における炭素数8〜22の脂肪酸ナトリウム塩(b1)中、65/35〜10/90が好ましく、55/45〜15/85がより好ましく、45/55〜25/75がさらに好ましい。 From the same viewpoint, the mass ratio of the fatty acid sodium salt mainly composed of a fatty acid sodium salt having 12 or less carbon atoms to the content of the fatty acid sodium salt mainly composed of a fatty acid sodium salt having 14 or more carbon atoms ([carbon Fatty acid sodium salt whose main component is fatty acid sodium salt having several 12 or less] / [Fatty acid sodium salt whose main component is fatty acid sodium salt having 14 or more carbon atoms] is a fatty acid having 8 to 22 carbon atoms in component (B). In sodium salt (b1), 65 / 35-10 / 90 are preferable, 55 / 45-15 / 85 are more preferable, and 45 / 55-25 / 75 are further more preferable.
成分(B)は、炭素数8〜22の脂肪酸ナトリウム塩を80質量%以上含む組成物であり、これ以外に、例えば、脂肪酸、塩化ナトリウム、水等を含むことができる。工程(1)で得られた加熱溶融された成分(A)との均一な混合を得る観点、得られる石鹸の泡立ち及び使用感を向上させ、高い硬度の石鹸を得る観点から、脂肪酸、塩化ナトリウム、水から選ばれる少なくとも1種を含むことが好ましく、脂肪酸(b2)、塩化ナトリウム(b3)、水(b4)のすべてを含むのがより好ましい。 A component (B) is a composition containing 80 mass% or more of C8-C22 fatty acid sodium salt, and can contain a fatty acid, sodium chloride, water, etc. other than this, for example. From the viewpoint of obtaining uniform mixing with the heated and melted component (A) obtained in step (1), improving the foaming and feeling of use of the resulting soap, and obtaining a high hardness soap, fatty acids, sodium chloride Preferably, at least one selected from water is included, and it is more preferable to include all of fatty acid (b2), sodium chloride (b3), and water (b4).
成分(B)の組成物中に含まれる脂肪酸(b2)は、得られる石鹸の泡立ちを向上させる観点から、炭素数8〜22の脂肪酸を含むのが好ましく、成分(B)中の脂肪酸の含有量は、上記観点に加え、得られる石鹸の硬度を向上させる観点から、成分(B)中に、0.1〜2質量%であるのが好ましく、0.2〜1.8質量%がより好ましく、0.3〜1.5質量%がさらに好ましい。 The fatty acid (b2) contained in the composition of the component (B) preferably contains a fatty acid having 8 to 22 carbon atoms from the viewpoint of improving foaming of the resulting soap, and the fatty acid content in the component (B) In addition to the above viewpoint, the amount is preferably 0.1 to 2% by mass, more preferably 0.2 to 1.8% by mass in the component (B) from the viewpoint of improving the hardness of the resulting soap. Preferably, 0.3 to 1.5 mass% is more preferable.
成分(B)に脂肪酸を含有させる方法としては、炭素数8〜22の脂肪酸ナトリウム塩と脂肪酸とを混合してもよいし、炭素数8〜22の脂肪酸ナトリウムに塩化ナトリムを加え、中和率を調整して、炭素数8〜22の脂肪酸ナトリウム塩と未中和の炭素数8〜22の脂肪酸の混合物として、炭素数8〜22の脂肪酸ナトリウムを80%質量%以上含む成分(B)としてもよい。 As a method of incorporating the fatty acid into the component (B), a fatty acid sodium salt having 8 to 22 carbon atoms and a fatty acid may be mixed, or sodium chloride is added to the fatty acid sodium having 8 to 22 carbon atoms to neutralize the fatty acid. As a mixture of a fatty acid sodium salt having 8 to 22 carbon atoms and an unneutralized fatty acid having 8 to 22 carbon atoms, as a component (B) containing 80% by mass or more of fatty acid sodium having 8 to 22 carbon atoms Also good.
成分(B)の組成物中に含まれる塩化ナトリウム(b3)の含有量は、得られる石鹸の硬度を向上させる観点から、成分(B)中、0.1〜1質量%であるのが好ましく、0.2〜0.8質量%がより好ましく、0.4〜0.6質量%がさらに好ましい。
また、成分(B)の組成物中に含まれる水(b4)の含有量は、石鹸の硬度を向上させる観点から、8〜16質量%であるのが好ましく、9〜15質量%がより好ましく、10〜14質量%がさらに好ましい。
また、成分(B)の組成物は、成分(A)を被覆しやすくするため、ペレット状(粒状)であることが好ましい。
The content of sodium chloride (b3) contained in the composition of component (B) is preferably 0.1 to 1% by mass in component (B) from the viewpoint of improving the hardness of the soap obtained. 0.2 to 0.8 mass% is more preferable, and 0.4 to 0.6 mass% is more preferable.
The content of water (b4) contained in the composition of component (B) is preferably 8 to 16% by mass, more preferably 9 to 15% by mass from the viewpoint of improving the hardness of the soap. 10 to 14% by mass is more preferable.
The composition of component (B) is preferably in the form of pellets (granular) in order to facilitate coating of component (A).
本発明により得られる石鹸は、成分(B)中の炭素数8〜22の脂肪酸ナトリウム塩(b1)と、成分(A)のラウリン酸を80質量%以上含む炭素数12〜18の飽和脂肪酸を含むことで、低温及び高温での泡立ちを向上させることができる。成分(A)に対する成分(b1)の質量割合(b1)/(A)は、7〜60が好ましく、10〜35がより好ましく、12〜30がさらに好ましい。 The soap obtained by the present invention comprises a fatty acid sodium salt (b1) having 8 to 22 carbon atoms in component (B) and a saturated fatty acid having 12 to 18 carbon atoms containing 80% by mass or more of lauric acid of component (A). By including, foaming at low temperature and high temperature can be improved. 7-60 are preferable, as for the mass ratio (b1) / (A) of the component (b1) with respect to a component (A), 10-35 are more preferable, and 12-30 are more preferable.
本発明の工程(2)は、工程(1)で加熱溶融された成分(A)と、成分(B)とを混合して、成分(B)に成分(A)を被覆する工程である。
混合の際、成分(B)を含む系内の温度は、制限されないが、成分(B)と加熱溶融された成分(A)との混合物の温度を抑制し、製造された機械練石鹸での、経時での外観の白色度の低下を小さくさせる点から、20〜40℃であることが好ましく、21〜38℃がより好ましく、22〜35℃がさらに好ましい。
成分(B)と加熱溶融された成分(A)との混合は、混合羽根を有する混合機で混合することが好ましい。混合羽根を有する混合機としては、混合羽根がブレード型であるリボンミキサーやニーダー等の公知の混合機が好ましく、ニーダーを用いるのがより好ましい。また、ニーダーのブレードとしては、具体的には、シグマ(Σ)形、ゼット(Z)形、スパイラル(S)形、マスチケータ形、フィッシュテール形等を用いることができる。混合羽根を有する混合機としては、例えば、「混練装置(1986年9月20日、第1版、株式会社科学技術総合研究所、P.108〜117、P.126〜129)」に記載されている装置などを用いることができる。
The step (2) of the present invention is a step of coating the component (B) with the component (B) by mixing the component (A) heated and melted in the step (1) and the component (B).
During mixing, the temperature in the system containing the component (B) is not limited, but the temperature of the mixture of the component (B) and the heat-melted component (A) is suppressed, The temperature is preferably 20 to 40 ° C., more preferably 21 to 38 ° C., and further preferably 22 to 35 ° C., from the viewpoint of reducing the decrease in whiteness of the appearance over time.
Mixing of the component (B) and the component (A) that has been heated and melted is preferably performed by a mixer having a mixing blade. As a mixer having a mixing blade, a known mixer such as a ribbon mixer or a kneader in which the mixing blade is a blade type is preferable, and it is more preferable to use a kneader. Further, as the blade of the kneader, specifically, a sigma (Σ) shape, a zet (Z) shape, a spiral (S) shape, a masticator shape, a fishtail shape, or the like can be used. As a mixer having a mixing blade, for example, it is described in “kneading apparatus (September 20, 1986, first edition, Science and Technology Research Institute, P.108-117, P.126-129)”. Can be used.
このように、成分(B)と加熱溶融された成分(A)を混合することにより、成分(B)に成分(A)を被覆することができる。
ここで、成分(B)に成分(A)を被覆するとは、成分(B)の表面の一部もしくは全てに成分(A)を付着させることを示す。この工程を行うことで、次に行う工程(3)で、成分(A)と成分(B)を均一に混練しやすくすることができる。
Thus, a component (A) can be coat | covered with a component (B) by mixing a component (B) and the component (A) fuse | melted by heating.
Here, covering the component (B) with the component (A) indicates that the component (A) is adhered to a part or all of the surface of the component (B). By performing this step, it is possible to easily knead the component (A) and the component (B) uniformly in the next step (3).
[工程(3)]
工程(3)は、工程(2)で得られた混合物を混練する工程である。本発明において、混練とは、ロール式混練機を用いて、組成物を均一に混合することを示す。
混練には、断面が円のロールを2〜5本を組み合わせたロール式混練機を使用することができ、ロールの数は3〜5本が好ましく、3本ロールを有するロール式混練機がより好ましい。ロール式混練機としては、3段ロールミル等公知の機械式混練機を用いることができる。
また、ロール間隔(ロール間の隙間)は、均一な石鹸を得る点から、0.1〜2mmが好ましく、0.2〜1.5mmがより好ましい。
[Step (3)]
Step (3) is a step of kneading the mixture obtained in step (2). In the present invention, kneading means that the composition is uniformly mixed using a roll kneader.
For the kneading, a roll kneader in which 2 to 5 rolls having a circular cross section are combined can be used. The number of rolls is preferably 3 to 5, and a roll kneader having three rolls is more preferable. preferable. As the roll kneader, a known mechanical kneader such as a three-stage roll mill can be used.
Moreover, 0.1-2 mm is preferable and the roll space | interval (gap between rolls) from the point which obtains uniform soap, 0.2-1.5 mm is more preferable.
本発明においては、工程(2)で得られた混合物に、前記成分のほか、通常の石鹸組成物に用いられる成分、例えば、非イオン性界面活性剤、成分(A)、(B)以外のアニオン界面活性剤、両性界面活性剤、抗菌剤、香料、殺菌剤、キレート剤、酸化防止剤、顔料、ポリエチレングリコール、染料、油剤等をさらに混合して、混練してもよい。 In the present invention, the mixture obtained in the step (2) is added to the components other than the above components, as well as components used in ordinary soap compositions, such as nonionic surfactants, components (A) and (B). Anionic surfactants, amphoteric surfactants, antibacterial agents, fragrances, bactericides, chelating agents, antioxidants, pigments, polyethylene glycol, dyes, oils and the like may be further mixed and kneaded.
本発明においては、得られる石鹸の全組成中において、低温及び高温での泡立ち、石鹸硬度を向上させ、水で濡れた後の石鹸の膨潤を抑える観点から、ラウリン酸の含有量が、8〜25質量%であるのが好ましく、14〜23質量%がより好ましく、18〜21質量%がさらに好ましい。また、同様に、ミリスチン酸の含有量が、2〜7質量%であるのが好ましく、4〜6.5質量%がより好ましく、5〜6質量%がさらに好ましい。
なお、ラウリン酸、ミリスチン酸は、それぞれ、成分(A)、成分(B)の(b1)及び(b2)中に含まれる。
In the present invention, in the total composition of the soap obtained, the content of lauric acid is 8 to 8 from the viewpoint of improving foaming at low and high temperatures, improving the soap hardness, and suppressing the swelling of the soap after wetting with water. It is preferably 25% by mass, more preferably 14-23% by mass, and even more preferably 18-21% by mass. Similarly, the myristic acid content is preferably 2 to 7% by mass, more preferably 4 to 6.5% by mass, and even more preferably 5 to 6% by mass.
In addition, lauric acid and myristic acid are contained in (b1) and (b2) of component (A) and component (B), respectively.
工程(3)で混練後、通常の機械練製法により、機械練石鹸を製造することができる。
例えば、混練後、混練物をプロッダー(押出機)で棒状に押出した後、1個の大きさに切断し、型打ちすることにより、石鹸を得ることができる。
After kneading in the step (3), a mechanical soap can be produced by a normal mechanical kneading method.
For example, after kneading, the kneaded product is extruded into a rod shape with a pudder (extruder), then cut into a single size and stamped to obtain soap.
石鹸の硬度は、製造成形時に、金型に石鹸の破片などが残らず、外観を損なうことなく製造できる点から、46以上が好ましく、47以上がより好ましく、49以上がよりさらに好ましい。なお、硬度の測定は、石鹸製造時の型打ち前の棒状石鹸押出装置の出口にある、円錐部分のヒーター温度を43℃に設定して石鹸を押出し、ゴム・プラスチック硬度計(GS−701N TYPE C、テクロック社製)で行う。 The hardness of the soap is preferably 46 or more, more preferably 47 or more, and even more preferably 49 or more, from the viewpoint that the soap can be manufactured without damaging the appearance without leaving any soap fragments in the mold at the time of production molding. The hardness is measured by extruding soap with a heater at the conical portion set at 43 ° C. at the outlet of the bar-shaped soap extrusion apparatus before stamping at the time of soap production, and a rubber / plastic hardness meter (GS-701N TYPE). C, manufactured by Teclock Corporation).
実施例1〜4、比較例1〜4
表3に示す組成の機械練石鹸を製造し、10℃及び40℃での泡立ち、10℃での手洗い感触(ざらつきのなさ)、安定性(白色度の低下、表面の結晶の析出)、石鹸硬度並びに膨潤率を評価した。結果を表3に併せて示す。
Examples 1-4, Comparative Examples 1-4
Manufactured mechanical soap with the composition shown in Table 3, foaming at 10 ° C. and 40 ° C., hand washing feeling at 10 ° C. (no roughness), stability (decrease in whiteness, precipitation of crystals on the surface), soap Hardness and swelling rate were evaluated. The results are also shown in Table 3.
(製造方法)
パーム核油及びパーム油を加水分解して、表1に示す脂肪酸組成のパーム核脂肪酸(PK)とパーム油脂肪酸(PO)を得た。パーム核脂肪酸(PK)、パーム油脂肪酸(PO)に塩を加え、水酸化ナトリウム水溶液で中和して、乾燥させた後、押出成形機により直径1cmの棒状に押し出し、さらにペレタイザー(切断機)を用いて、長さ2cm以下のペレット状に切断した、表2に示す組成の組成物(B1)及び(B2)を得た。
次に、25℃の組成物(B1)又は(B2)に、45℃で加熱溶融させた脂肪酸(比較例1では、粉末のままのラウリン酸、比較例3は未添加)を添加した後、香料及びその他の成分を加え(酸化チタンはポリエチレングリコールに分散させた状態で添加した)、ニーダー(ブレードはゼット(Z)型、佐竹社製)で10分間混合し、全成分を均一に混合した。なお、成分(A)及び(B)の混合時温度は、25〜45℃であった。また、得られた実施例1〜4の混合物においては、成分(B)に成分(A)が被覆されていた。
この混合物を、3段ロールミル(日本加工機社製)でロール間隔を0.2mmに設定して混練した。
得られた混練物を、棒状石鹸押出装置(真空2段プロッダー、日本加工機社製)で円柱状の棒状に押出を行った。その際、石鹸押出装置の出口にある、円錐部分のヒーター温度は43℃に設定した。その後型打ちすることにより、石鹸を得た。
(Production method)
Palm kernel oil and palm oil were hydrolyzed to obtain palm kernel fatty acid (PK) and palm oil fatty acid (PO) having the fatty acid composition shown in Table 1. Salt is added to palm kernel fatty acid (PK) and palm oil fatty acid (PO), neutralized with an aqueous sodium hydroxide solution, dried, then extruded into a 1cm diameter rod with an extruder, and a pelletizer (cutting machine) Were used to obtain compositions (B1) and (B2) having the composition shown in Table 2, which were cut into pellets having a length of 2 cm or less.
Next, to the composition (B1) or (B2) at 25 ° C., after adding a fatty acid heated and melted at 45 ° C. (in Comparative Example 1, lauric acid in powder form, Comparative Example 3 is not added), Add perfume and other ingredients (titanium oxide was added in a state of being dispersed in polyethylene glycol), and mixed for 10 minutes with a kneader (blade is Zet (Z type, manufactured by Satake Corporation), and all ingredients were mixed uniformly. . In addition, the temperature at the time of mixing of a component (A) and (B) was 25-45 degreeC. Moreover, in the obtained mixture of Examples 1-4, the component (A) was coat | covered with the component (B).
This mixture was kneaded with a three-stage roll mill (manufactured by Nippon Processing Machine Co., Ltd.) with the roll interval set to 0.2 mm.
The obtained kneaded product was extruded into a cylindrical bar shape with a bar-shaped soap extrusion apparatus (vacuum two-stage prodder, manufactured by Nippon Processing Machinery Co., Ltd.). In that case, the heater temperature of the cone part in the exit of a soap extrusion apparatus was set to 43 degreeC. Then, soap was obtained by stamping.
(評価方法)
(1)40℃での泡立ち:
40℃の水道水でナイロンタオルを濡らした後、石鹸1gをナイロンタオルにこすり付け、10秒間よくタオルを揉みこんで泡立てた。なお、ナイロンタオルに含まれる水の量は、70gとなるようにした。その後、泡のみを集め、メスシリンダーで泡量(mL)を測定した。測定値は、3回の平均値とした。
(Evaluation method)
(1) Foaming at 40 ° C:
After the nylon towel was wetted with tap water at 40 ° C., 1 g of soap was rubbed onto the nylon towel, and the towel was rubbed well for 10 seconds and foamed. The amount of water contained in the nylon towel was set to 70 g. Thereafter, only foam was collected and the amount of foam (mL) was measured with a graduated cylinder. The measured value was an average of three times.
(2)10℃での泡立ち:
水道水に氷を加えて10℃の水を調製し、その水に石鹸を30秒間漬け置きすることで、石鹸の温度を10℃に調整した。その後、石鹸を10℃の水から取出し、両手に石鹸をはさんで10回こすり泡立てを行った。その後、泡を手で集めて泡量(mL)を測定した。測定値は、3回の平均値とした。
(2) Foaming at 10 ° C:
Ice was added to tap water to prepare 10 ° C water, and the soap temperature was adjusted to 10 ° C by immersing the soap in the water for 30 seconds. Thereafter, the soap was taken out from water at 10 ° C. and rubbed 10 times with soap between both hands. Thereafter, the foam was collected by hand and the amount of foam (mL) was measured. The measured value was an average of three times.
(3)10℃での手洗い感触(ざらつきのなさ):
水道水に氷を加えて10℃の水を調製し、その水に石鹸を30秒間漬け置きすることで、石鹸の温度を10℃に調整した。その後、石鹸を10℃の水から取出し、両手に石鹸をはさんで10回こすり、手に感じる石鹸表面のざらつきを、以下の基準で評価した。なお、評価は3人で行い、その合計点で示した。
4:ざらつきを全く感じない。
3:ざらつきをほとんど感じない。
2:ざらつきを感じる。
1:ざらつきを明らかに感じる。
(3) Hand washing feeling at 10 ° C (no roughness):
Ice was added to tap water to prepare 10 ° C water, and the soap temperature was adjusted to 10 ° C by immersing the soap in the water for 30 seconds. Thereafter, the soap was taken out from water at 10 ° C. and rubbed 10 times with soap between both hands, and the roughness of the soap surface felt by the hand was evaluated according to the following criteria. The evaluation was performed by three people, and the total score was shown.
4: I do not feel any roughness.
3: Little roughness is felt.
2: I feel rough.
1: Clearly feel rough.
(4)安定性(白色度の低下):
製造直後の石鹸の色(L,a,b)を色差計(CR−200、ミノルタ社製)で測定した。その石鹸を50℃の恒温に入れ、30日間保存した後、同様に色(L,a,b)を測定した。直後の色と50℃保存品の色の色差(ΔE)を計算することにより、白色度の低下を評価した。
なお、色差(ΔE)は以下の式から計算し、色差(ΔE)が小さいほど、白色度の低下が小さいことを示す。
(白色度の低下、色差(ΔE)の計算)
・製造直後の石鹸のLab:L0、a0、b0
・50℃、30日間保存後の石鹸のLab:L1、a1、b1
・白色度の低下である色差(ΔE)を次の式から計算する。
ΔE={(L1−L0)2+(a1−a0)2+(b1−b0)2}1/2
(4) Stability (decrease in whiteness):
The color (L, a, b) of the soap immediately after production was measured with a color difference meter (CR-200, manufactured by Minolta). The soap was placed at a constant temperature of 50 ° C. and stored for 30 days, and then the color (L, a, b) was measured in the same manner. The decrease in whiteness was evaluated by calculating the color difference (ΔE) between the color immediately after and the color of the product stored at 50 ° C.
The color difference (ΔE) is calculated from the following formula, and the smaller the color difference (ΔE), the smaller the decrease in whiteness.
(Decrease in whiteness, calculation of color difference (ΔE))
・ Lab of soap immediately after production: L 0 , a 0 , b 0
・ Lab of soap after storage at 50 ° C. for 30 days: L 1 , a 1 , b 1
The color difference (ΔE), which is a decrease in whiteness, is calculated from the following equation.
ΔE = {(L 1 −L 0 ) 2 + (a 1 −a 0 ) 2 + (b 1 −b 0 ) 2 } 1/2
(5)安定性(表面の結晶の析出):
得られた石鹸を50℃の恒温槽で30日間保存した後、各石鹸の表面状態を、目視により観察し、以下の基準で評価した。なお、評価は3人で行い、その合計点で示した。
4:結晶の析出が全く見られない。
3:結晶の析出がほとんど見られない。
2:結晶の析出がわずかに見られる。
1:結晶の析出が明らかに見られる。
(5) Stability (precipitation of surface crystals):
After the obtained soap was stored in a thermostatic bath at 50 ° C. for 30 days, the surface state of each soap was visually observed and evaluated according to the following criteria. The evaluation was performed by three people, and the total score was shown.
4: No precipitation of crystals is observed.
3: Almost no precipitation of crystals is observed.
2: Slight crystal precipitation is observed.
1: Crystal precipitation is clearly seen.
(6)石鹸硬度:
型打ち前の棒状石鹸押出装置の出口にある、円錐部分のヒーター温度を43℃に設定して石鹸を押出し、ゴム・プラスチック硬度計(GS−701N TYPE C、テクロック社製)で石鹸硬度を測定した。なお、硬度は数値が高い方が製造時の成型性に優れることを示す。
(6) Soap hardness:
The soap is extruded with rubber heater and plastic hardness meter (GS-701N TYPE C, manufactured by Tecrock Co., Ltd.). did. In addition, it shows that the one where a numerical value is higher is excellent in the moldability at the time of manufacture.
(7)膨潤率:
得られた石鹸を1cm×1cm×5cmの角型に切断し、重量測定後、25℃の水道水中に4時間浸漬を行った。浸漬後、再び重量を測定し、下式に従って膨潤率(%)を求めた。なお、膨潤率が低いほど、水で濡らした後の石鹸の形状が変化しにくいこと示す。
膨潤率(%)=(浸漬後の重量(g)/浸漬前の重量(g))×100
(7) Swell rate:
The obtained soap was cut into a 1 cm × 1 cm × 5 cm square, and after weight measurement, it was immersed in tap water at 25 ° C. for 4 hours. After the immersion, the weight was measured again, and the swelling rate (%) was determined according to the following formula. In addition, it shows that the shape of soap after wetting with water is less likely to change as the swelling rate is lower.
Swelling ratio (%) = (weight after immersion (g) / weight before immersion (g)) × 100
Claims (3)
(1)(A)ラウリン酸を80質量%以上含む炭素数12〜18の飽和脂肪酸を加熱溶融する工程、
(2)工程(1)で得られた加熱溶融物と、(B)炭素数8〜22の脂肪酸ナトリウム塩を80質量%以上含む組成物とを混合して、成分(B)に成分(A)を被覆する工程、
(3)工程(2)で得られた混合物を混練する工程。 The manufacturing method of a mechanical kneaded soap which has the following processes.
(1) (A) a step of heating and melting a saturated fatty acid having 12 to 18 carbon atoms containing 80% by mass or more of lauric acid,
(2) The heated melt obtained in step (1) and (B) a composition containing 80% by mass or more of a fatty acid sodium salt having 8 to 22 carbon atoms are mixed, and component (B) is mixed with component (A )
(3) A step of kneading the mixture obtained in step (2).
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JPS57187400A (en) * | 1981-05-14 | 1982-11-18 | Kao Corp | Detergent composition not for hair |
JPH06511486A (en) * | 1991-09-23 | 1994-12-22 | ザ、プロクター、エンド、ギャンブル、カンパニー | Mild personal cleansing solid composition with balanced surfactants, fatty acids and paraffin wax |
JPH1161198A (en) * | 1997-08-11 | 1999-03-05 | Lion Corp | Transparent solid soap composition by machine kneading |
JP2001003095A (en) * | 1999-06-16 | 2001-01-09 | Kao Corp | Preparation of detergent particles |
JP2001505604A (en) * | 1996-12-06 | 2001-04-24 | ザ、プロクター、エンド、ギャンブル、カンパニー | Coated detergent tablet |
JP2008088085A (en) * | 2006-09-29 | 2008-04-17 | Shiseido Co Ltd | Skin-washing agent |
JP2009029737A (en) * | 2007-07-26 | 2009-02-12 | Shiseido Co Ltd | Skin cleaning preparation |
JP2013185062A (en) * | 2012-03-07 | 2013-09-19 | Kao Corp | Solid detergent composition |
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JPS57187400A (en) * | 1981-05-14 | 1982-11-18 | Kao Corp | Detergent composition not for hair |
JPH06511486A (en) * | 1991-09-23 | 1994-12-22 | ザ、プロクター、エンド、ギャンブル、カンパニー | Mild personal cleansing solid composition with balanced surfactants, fatty acids and paraffin wax |
JP2001505604A (en) * | 1996-12-06 | 2001-04-24 | ザ、プロクター、エンド、ギャンブル、カンパニー | Coated detergent tablet |
JPH1161198A (en) * | 1997-08-11 | 1999-03-05 | Lion Corp | Transparent solid soap composition by machine kneading |
JP2001003095A (en) * | 1999-06-16 | 2001-01-09 | Kao Corp | Preparation of detergent particles |
JP2008088085A (en) * | 2006-09-29 | 2008-04-17 | Shiseido Co Ltd | Skin-washing agent |
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JP2013185062A (en) * | 2012-03-07 | 2013-09-19 | Kao Corp | Solid detergent composition |
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