CN1466942A - Granulating substance used as whitening agent and method for manufacturing the same, bath preparation composition containing the same - Google Patents
Granulating substance used as whitening agent and method for manufacturing the same, bath preparation composition containing the same Download PDFInfo
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- CN1466942A CN1466942A CNA031425046A CN03142504A CN1466942A CN 1466942 A CN1466942 A CN 1466942A CN A031425046 A CNA031425046 A CN A031425046A CN 03142504 A CN03142504 A CN 03142504A CN 1466942 A CN1466942 A CN 1466942A
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- soluble polymer
- anatase
- water soluble
- titanium oxide
- type titanium
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Abstract
To provide a granule usable as a turbidity-forming agent, a method for producing the granule, and to obtain a bathing agent composition containing the granule.The granule contains anatase-type titanium oxide and a water-soluble polymer. The bathing agent composition contains the granule. The method for producing the granule is also provided. By using the granule, the bathing agent composition having high preservation stability can be provided. The bathing agent composition can be packaged and preserved even in a paper container because of the high stability in the preservation. Good solubility and dispersibility can be obtained even in an area where the hardness of tap water is high. (C)2004,JPO.
Description
Technical field
The bath oil composition that the present invention relates to the pelletize thing that uses as the nebulousurine agent and manufacture method thereof and contain this pelletize thing.
Background technology
Nebulousurine agent in the baths generally contains inorganic pigment.Even can not disperse in bath water but directly allocate inorganic pigment into, so the nebulousurine effect is insufficient.Therefore people have carried out various researchs to improving the dispersibility of inorganic pigment in bath water up to now; successively propose to contain baths (the open communique of No. 57516/1988 patent of invention of Japan) with the nebulousurine agent of water soluble polymer coated inorganic pigment; allocate the baths (the open communique of No. 9811/1990 patent of invention of Japan) that is coated the pelletize thing that its surperficial inorganic pigment makes by the surfactant of HLB value 11～18 into as opalizer; the aminoacid that perhaps contains band acidylate N is the water-insoluble and Powdered baths preferably inorganic pigment of white (the open communique of No. 240722/1991 patent of invention of Japan) that surfactant coats; and it is characterized in that containing carbonate and water-insoluble inorganic pigment, also contain the solid-state baths (the open communique of No. 325137/1996 patent of invention of Japan) of polyhydric alcohol etc. simultaneously.
The wherein nebulousurine agent that particularly titanium oxide and water soluble polymer mixing granulation is formed is even from stability and cost consideration, also adopted by most example.
In these patent documentations, though inorganic pigment is to describe with the material form that is coated by water soluble polymer, but, inorganic pigment and water soluble polymer etc. are mixed together because being actually with water, be dried the material that forms, so be recited as the pelletize thing in this manual, much less this and coating have equivalent meanings.
Summary of the invention
But it is strong that the above-mentioned pelletize thing that is made of inorganic pigment and water soluble polymer has hygroscopicity, has the stability of formulation problem that causes curing and preparation overstrike etc. because of moisture absorption.Therefore, these preparations must be kept in the high plastic containers of moisture resistance, can not preserve with paper-made vessel.Environmental problem comes into one's own now, does not preferably use the plastic containers that will directly become rubbish in order to reduce rubbish, replaces the use paper-made vessel.Therefore what must prevent to remember solidifies because of moisture absorption.
What wherein put down in writing in the open communique of Japan's the 57516/1988th equal sign patent of invention is, use sodium carboxymethyl cellulose (CMCNa) as water soluble polymer, with the nebulousurine agent that inorganic pigment coats, this nebulousurine agent does not take place because of suction is solidified, the phenomenon of variable color with it.But nebulousurine agent by CMCNa coated inorganic pigment, in tap water, exist and make under metal ion (calcium ion and the magnesium ion etc.) effect that the dispersibility in bath water worsens, thereby can not particularly directly use in the high geographic tap water of hardness at tap water as the nebulousurine agent of baths.
And the pelletize thing of putting down in writing in the open communique of No. 9811/1990 patent of invention of Japan with the formation of specific surfactant coating anatase-type titanium oxide, not only have the problem of bath water draining on environment because of containing surfactant, but also the dissolubility that has a nebulousurine when preparation is preserved and through the time the problem of reduction.
The inventor etc. further investigate for addressing these problems, found that: a kind ofly wherein contain useful anatase-type titanium oxide as inorganic pigment, itself and water soluble polymer mixing granulation are made the bath oil composition of pelletize thing, can in bath water, dissolve without a doubt and disperse, solidify and discoloration problem nor can produce because of moisture absorption, the perhaps stability in the basic formulations (because of moisture absorption is solidified or variable color) problem, thereby finished the present invention.
That is to say, the present invention includes following invention:
(1) a kind of pelletize thing wherein contains anatase-type titanium oxide and water soluble polymer.
(2) go up the pelletize thing that note (1) is put down in writing, wherein weight ratio X (anatase-type titanium oxide/water soluble polymer) is 4 〉=X 〉=1 between anatase-type titanium oxide and water soluble polymer.
(3) go up the pelletize thing that note (1) or (2) is put down in writing, wherein water soluble polymer is at least a material of selecting from one group of material that gelatin, arabic gum, heal skin ulcer glue, Tragacanth, starch, carboxymethyl cellulose, sodium carboxymethyl cellulose, methylcellulose, hydroxyethyl-cellulose, sodium polyacrylate and polyvinyl pyrrolidone are formed.
(4) go up any one pelletize thing of putting down in writing in note (1)～(3), wherein do not contain surfactant in fact.
(5) a kind of bath oil composition wherein contains any one pelletize thing of putting down in writing in note (1)～(4).
(6) a kind of solid-state bath oil composition wherein contains anatase-type titanium oxide and water soluble polymer, and does not contain surfactant in fact.
(7) remember that upward any one puts down in writing the manufacture method of pelletize thing in (1)～(4), it is characterized in that anatase-type titanium oxide, water soluble polymer and water are mixed, make the pelletize thing after the drying.
Adopt pelletize thing of the present invention can provide a kind of preparation not have fixed and the strong bath oil composition of storage stability variable color.Bath oil composition of the present invention is preserved so can be filled in the paper-made vessel because storage stability is strong.Even and bath oil composition of the present invention also can obtain fine solubility and dispersibility in the high area of tap water hardness.
The specific embodiment
The anatase-type titanium oxide that the present invention uses, for example (leave nothing usable to the invading enemy and learn work, skill newspaper hall publishes and distributes write up at " titanium oxide ", 1991,47～50 pages) on, contain four titanium dioxide unit being equivalent to crystal unit lattice structure cell, have the total chain structure of octahedral four ribs.Can Titanium Dioxide Rutile Top grade and anatase-type titanium oxide be arranged because of crystal structure is different at the titanium oxide of industrial use.Under the general occasion of in baths, using, can use Titanium Dioxide Rutile Top grade.Have been found that the use anatase-type titanium oxide among the present invention, compare during with the use Titanium Dioxide Rutile Top grade, be not subjected to the influence of hardness in the tap water when dissolving disperses in bath water, have the nebulousurine effect.
As the water soluble polymer that uses among the present invention, for example can enumerate gelatin, arabic gum, water soluble polymers such as skin ulcer glue, Tragacanth, starch, carboxymethyl cellulose, sodium carboxymethyl cellulose, methylcellulose, hydroxyethyl-cellulose, sodium polyacrylate and polyvinyl pyrrolidone more, these may be used singly or two or more in combination.These water soluble polymers are from dissolubility bath water and dispersibility viewpoint, preferably carboxymethyl cellulose sodium and polyvinyl pyrrolidone, more preferably sodium carboxymethyl cellulose.As sodium carboxymethyl cellulose, though so long as dissolved with regard to the special restriction of nothing in water, preferred 2% viscosity in aqueous solution is in below the 200mPas, more preferably is in below 1～100mPas.In a single day 2% solution viscosity of this carboxymethyl cellulose is lower than this scope, and the stability of pelletize thing will worsen, and then is difficult to pelletize if surpass this scope.
Using the pelletize thing of the present invention of anatase-type titanium oxide, can weight ratio X (anatase-type titanium oxide/water soluble polymer) be 4 〉=X 〉=1 time pelletize between anatase-type titanium oxide and water soluble polymer.Last note weight ratio X (anatase-type titanium oxide/water soluble polymer) is 4 〉=X 〉=1.5 more preferably.Last note X value is in case be lower than this scope, just can not obtain with the pelletize thing in the corresponding turbidity of the amount of allocating into.And go up note X value in case surpass this scope, and the effect that is coated by water soluble polymer will reduce, and the dispersion stabilization in bath water also can worsen.
Surfactant in the pelletize thing of the present invention, (surfactant is influenced by spice etc. easily and causes dissolubility to reduce the stability of problem, preparation self from the environment of bath water, thereby become the reason of fixed, variable color and fouling) and the cost viewpoint, in the pelletize thing, preferably account for below 1%, more preferably do not contain in fact.
Pelletize thing of the present invention can utilize anatase-type titanium oxide, water soluble polymer and other compositions are in case of necessity mixed with suitable quantity of water, and drying is made the method manufacturing of pelletize thing.
Be not particularly limited for blended orders such as anatase-type titanium oxide, water soluble polymer and water, can in water, add water soluble polymer, after heating makes it dissolving in case of necessity, add anatase-type titanium oxide and mix; Perhaps with anatase-type titanium oxide with after water soluble polymer mixes, add entry, mix, disperse with mixing rolls such as roll-type, kneading types.The ratio of pelletize water and anatase-type titanium oxide and water soluble polymer total amount preferably is in 10: 1～1: 10, more preferably is in 4: 1～1: 8 scope.Pelletize water and titanium oxide and CMCNa total amount in a single day be lower than this scope than, owing to being difficult to the homogenizing pelletize dissolubility of pelletize thing is worsened, otherwise then removes the operating efficiency of moisture content and reduce if surpass this scope.
The example of a kind of pelletize thing manufacture method of the present invention below is described.
Note water soluble polymer on 40 weight portions is added in the 200 weight portion Purified Waters, stir down at 20～80 ℃ and made it dissolving in 0.5～3.0 hour.After wherein adding 60 weight portion anatase-type titanium oxides, room temperature stirred 10～15 minutes down, made it to disperse.
Disperse thing to place the ventilation thermostatic drier this, drying is 10～30 hours under 30～150 ℃.With pulverizers such as small mill, general-purpose ball mill it is crushed to 60～200 orders then.Adopt above method can access purpose pelletize thing.
Pelletize thing of the present invention can be as the nebulousurine agent of baths.The bath oil composition of allocating this pelletize thing into also can be filled in keeping in the paper-made vessel, from the viewpoint that reduces rubbish very big advantage is arranged also.
And go up the amount of allocating into of note pelletize thing in this bath oil composition, preferably allocate into and can make the concentration of nebulousurine agent in the bath water reach 0.15～30ppm, more preferably 1.5～22.5ppm.The amount of allocating into of pelletize thing is lower than this scope, and the tone of baths will reduce, otherwise then adds fashionable dissolubility reduction if surpass this scope in bath water.
Except that anatase-type titanium oxide and water soluble polymer, in the pelletize thing of the present invention, can also in the scope of not damaging effect of the present invention, allocate the various compositions of in bath oil composition, allocating into usually in case of necessity into, for example carbonate, organic acid, inorganic pigment, wetting agent, antiseptic, metal ion sealer, spice, inorganic salts, oiliness composition, extracts from crude drugs, plant extract, vitamins, protease, creeping chill agent, temperature sense agent and other compositions.In pelletize thing of the present invention, allocate under these occasions of selecting composition, preferably account for anatase-type titanium oxide and below 20% of water soluble polymer total amount, more preferably account for below 10%.
In addition, in the bath oil composition of the present invention, except that last note pelletize thing, also can in the scope of not damaging effect of the present invention, allocate the various compositions of in bath oil composition, allocating into usually in case of necessity into, for example carbonate, organic acid, inorganic pigment, wetting agent, antiseptic, metal ion sealer, spice, inorganic salts, oiliness composition, extracts from crude drugs, plant extract, vitamins, protease, creeping chill agent, temperature sense agent and other compositions.Under this occasion, can adopt, put it in the mixer method manufacturing that uniformly mixes at normal temperatures then among the baths composition beyond the pelletize thing adding of the present invention pelletize thing of the present invention.Said mixer is so long as stir, mix can using of usefulness to powder.Specifically can enumerate indoor mixer, powder body mixer, general-purpose stirring mixer, ribbon formula mixer, V-Mixer etc.Incorporation time can be mixed the required time for uniform ingredients, uses under the occasion of above-named mixer, and incorporation time is generally 5～50 minutes.
In addition, the invention provides and a kind ofly contain anatase-type titanium oxide and water soluble polymer, and do not contain the solid-state bath oil composition of surfactant in fact.Solid-state bath oil composition of the present invention as long as this bath oil composition is solid-state, for example can be graininess, bulk, laminar, tablet shape, not necessarily must contain the sort of pelletize thing of note.In the bath oil composition of the present invention, except that anatase-type titanium oxide and water soluble polymer, can also in the scope of not damaging effect of the present invention, allocate the various compositions of in bath oil composition, allocating into usually in case of necessity into, water soluble polymer and other compositions beyond for example carbonate, organic acid, inorganic pigment, wetting agent, antiseptic, metal ion sealer, spice, inorganic salts, oiliness composition, extracts from crude drugs, plant extract, vitamins, protease, creeping chill agent, temperature are felt agent, upward note (3) is put down in writing.
For example can enumerate sodium carbonate, sodium bicarbonate, magnesium carbonate, potassium carbonate, potassium bicarbonate, sodium sesquicarbonate etc. as carbonate; For example can enumerate succinic acid, fumaric acid, malic acid, adipic acid, tartaric acid, citric acid, malonic acid, maleic acid etc. as organic acid.These carbonate and organic acid can use more than one respectively.
As inorganic pigment, for example can enumerate titanium oxide, calcium carbonate, magnesium carbonate, zinc oxide, Talcum, calcium silicates, anhydrous silicic acid, Kaolin, bentonite, odenite etc.
As wetting agent, for example can enumerate saccharides such as Sorbitol, xylitol, maltose alcohol, glucosan, glucose, maltose, lactose, sucrose, xylose, fructose, mannitol, lactose, ethylene glycol, propylene glycol, 3-methyl isophthalic acid, 3-butanediol, glycerol, 1, polyalcohols such as 3-butanediol, amino acidses such as ketopyrrolidine sodium formate, sodium glutamate, carbamide etc.
As antiseptic, for example can enumerate oxo benzoate (for example methyl parahydroxybenzoate), benzoic acid, benzoate, phenyl phenol etc.
As spice, for example can enumerate Essential lavender oil, Flos Jasmini Sambac oil, Fructus Citri Limoniae wet goods natural perfume material, synthetic perfumes such as geraniol, rhodinol, phenethanol.
As inorganic salts, for example can enumerate sodium sulfate, magnesium sulfate, sodium chloride, potassium chloride, sodium carbonate, sodium bicarbonate, sodium sesquicarbonate and sodium thiosulfate.
As the oiliness composition, for example can enumerate Oleum Glycines, Testa oryzae oil, california Simmondsia chinensis oil, American Avocado Tree oil, almond oil, olive oil, cocoa butter, Oleum sesami, almond oil, Semen Ricini oil, Oleum Cocois, ermine oil, Adeps Bovis seu Bubali, leaf fat, solidified oil that these natural HYDROGENATION OF OILS AND FATS obtain and oils such as synthetic glycerides such as myristin, 2 ethyl hexanoic acid glyceride, two glyceride; Brazil wax, spermaceti, Cera Flava, wax classes such as lanoline, Liquid Paraffin, vaseline, paraffin, microcrystalline wax, ceresine, Squalene, hydro carbons such as octadecane, lauric acid, myristic acid, Palmic acid, stearic acid, docosanoic acid, oleic acid, linoleic acid, linolenic acid, lanoceric acid, senior fatty acid such as isostearic acid, lauryl alcohol, spermol, octadecanol, oleyl alcohol, cholesterol, senior alcohols such as 2-hexyl dodecanol, sad cetyl ester, lactic acid myristyl ester, the lactic acid cetyl ester, isopropyl myristate, isopropyl palmitate, the adipic acid isopropyl ester, butyl stearate, decyl oleate, esters such as isostearic acid cholesteryl ester, the quintessence oil class, silicone oils.
Crude drug or plant extract preferably do not influence the proportioning and the form of cooperation with crude drug or plant.The example of crude drug or plant, for example can enumerate Rhizoma Atractylodis, the Rhizoma Atractylodis Macrocephalae, radix valerianae, Herba Schizonepetae, thick pouncing on, Rhizoma Chuanxiong, Pericarpium Citri junoris, Radix Angelicae Sinensis, race, scutellariae,radix, SHANZHIZI, Folium Artemisiae Argyi, Aloe, Radix Ginseng, Cortex cinnamomi japonici (Ramulus Cinnamomi), Radix Paeoniae, Herba Menthae, Poria, Radix Angelicae Pubescentis, Rhizoma Acori Graminei, Fructus Schisandrae Chinensis, the Radix Angelicae Dahuricae, Herba Houttuyniae, Borneolum Syntheticum, Stigma Croci, Cortex Phellodendri, Fructus Foeniculi, Pericarpium Citri Reticulatae, the wild goose skin, Flos Matricariae chamomillae, Herba melissae axillaris, Radix Raphani, willow, Lignum cinnamomi camphorae, Ramulus Sambuci Williamsii Cao Beans is cool, Herba Moslae, Rhizoma et Radix Dysosmae Veitchii, Rhizoma Acori Graminei, Radix Artemisia ordosicae, Herba Hyperici Erecti, Fructus Citri grandis, bitter Citrus, peach tree, Fructus Gleditsia, Folium Eriobotryae, Radix Ophiopogonis, BAIYECAO, Cortex Moutan, Aesculus turbinata B1, common milfoil, hops, Herba Rosmarini Officinalis, birch, lucky grass roots, Aesculus hippocastanum L., Arnica montana, upright certain herbaceous plants with big flowers, Herba Urticae Cannabinae, Radix Hamamelidis Mollis, Radix Curcumae, Radix Scutellariae, wall wood, rice, Rhizoma Paridis, watt shape Radix Artemisia ordosicae, Fructus actinidiae chinensis, Fructus Cucumidis sativi, dizzy grass, Fructus Vitis viniferae, Fructus Gardeniae, Herba Oenanthes Javanicae, Bellis perennis, ZAOCAO, Radix et Caulis Opuntiae Dillenii, Folium Perillae, Betula platyphylla Suk., Herba Equiseti Arvinsis, bodhi tree, Herba Antenoronis Neofiliformis, Chiretta, mulberry, Semen sojae atricolor, Herba thymi vulgaris, big Flos Inulae, Herba Houttuyniae, Fructus Jujubae, Parsley, Semen Coicis, Flos Caraganae Sinicae, Fructus Luffae, Herba Typhae, hop, Herba Saxifragae, Rubus corchorifolius, lavandula angustifolia, Flos Nelumbinis, Flos Rosae Multiflorae, Flos rosae multiflorae, tea, Bulbus Lilii, Fructus Hordei Vulgaris, Semen Tritici aestivi, bright dawn grass, Fructus Pruni, Herba bromi japonici, corn, Qian Kui, Radix Arnebiae (Radix Lithospermi), Fructus Capsici, Rhizoma Zingiberis Recens, Caulis et Folium Lactucae sativae, Fructus Citri Limoniae Fructus cydoniae oblongae tree, orange, Fructus Fragariae Ananssae, Flos Carthami, beech, the Europe Radix Gentianae, Radix Gentianae, Mentha viridis L, the ocean Herba Menthae, Fructus Sapindi Mukouossi, Eucalyptus, thin Herba Solani Septemlobi, Sasa veitchii(Carr.)Rehd., the slender lobule Herba Asari, the stem Herba Asari, the son of leaping up is careless, Fructus Arctii, Bulbus Allii, the plumage Seem Lablab Album, Ceratonia siliqua, pinaster, Caulis Hederae Sinensis, Rodgersia podophylla A. Gray, Radix Sanguisorbae, little Paeonia suffruticosa is climing, Ramulus et Folium Spiraeae Salicifolia, American Avocado Tree, Cordyceps, Urginea maritima, grapefruit, Fructus Pruni salicinae, Citrus aurantium Linn., Mang cattle Seedling, Lentinus Edodes, radix ononidis, tormentil, Rhizoma Coptidis, Cupressaceae, Paeonia suffruticosa, Radix Ophiopogonis Dracaenoidis, Fructus Canarii albi, Helianthi, the california jojoba, macadimia nut, feather palm oil, Flos Camelliae Japonicae, almond, cacao bean, Semen Sesami, late cherry, especially refer to borage etc., these may be used singly or two or more in combination.
Vitamins for example can be enumerated vitamin A, vitamin B, vitamin D, vitamin E, vitaminF, vitamin K, Citrin, vitamin U, carnitine, ferulic acid, oryzanol, thioctic acid, orotic acid and derivant thereof etc.Protease, the protease etc. that for example can enumerate pepsin, trypsin, chymase, cathepsin, papain, bromelain, ficin and antibacterial yeast and derive from the capsule rhzomorph that looses.As the creeping chill agent, for example can enumerate L-menthol, Oleum menthae, Camphora, thymol etc.As temperature sense agent; for example can enumerate capsaicin, Capsaicinoid, dihydroxy capsaicin, capsanthin, capsicum tincture, Fructus Capsici powder, benzyl nicotinate, nicotinic acid Beta-Butoxy ethyl ester, N-acyl group Rhizoma et radix valerianae amide, Vanillyl pelargonic amide, cephrol alkyl ether (specifically cephrol ethylether, cephrol butyl ether, cephrol isobutyl ether, cephrol propyl ether, cephrol isopropyl ether, cephrol amyl ether etc.), n-nonanoic acid vanillyl ether, Rhizoma Zingiberis Recens tincture, butyl-[(3,4-methylene dioxo) benzyl] ether and shogaol etc.
Other compositions can be enumerated sedimentary mineral in sulfur, ore in sand form, the hot spring, neutral clay, yolk powder, stir-fry bran, mica powder, defatted milk powder, Sargassum extract, pigment, antibacterial etc.
The dosage form of bath oil composition of the present invention can be Powdered or solid shape (for example graininess, bulk, laminar, tablet shape etc.).
Embodiment
Below specify the present invention by means of embodiment, but the present invention is not subjected to these
The restriction of embodiment.
(embodiment 1)
(ニ チ リ Application KCC makes, trade name: キ Star コ レ-ト to add 20 weight portion sodium carboxymethyl cellulose in 100 weight portion Purified Waters
TM2% solution viscosity is 10mPas), 30 ℃ are stirred dissolving in 1 hour down.(Ishihara Sangyo Kaisha, Ltd. makes, trade name: イ ペ-Network to wherein adding 80 weight portion anatase-type titanium oxides
TM), room temperature stirs down and made it in 30 minutes to disperse.In ventilation thermostatic drier (ヤ マ ト science society make, DN-81 type) in 105 ℃ with dry 24 hours (diel) of this material.Dry thing is pulverized with small mill (thin river ironworker's manufacturing AP-B type) and is obtained 100 purpose pelletize things.
(embodiment 2)
(テ イ カ Co., Ltd. makes, trade name: TITANIX with 70 weight portion anatase-type titanium oxides
TM) (BASF Japanese firm makes, trade name: Le PVC ス コ-Le) mix, to wherein adding 50 weight portion Purified Waters, mix with Squeezinggranulator, make hydrous powdery with 30 weight account polyethylene base ketopyrrolidines.In ventilation thermostatic drier (ヤ マ ト science society make, DN-81 type) in 105 ℃ with dry 24 hours (diel) of this material.Dry thing is pulverized with small mill (thin river ironworker's manufacturing AP-B type) and is obtained 100 purpose pelletize things.
(embodiment 3)
(Ishihara Sangyo Kaisha, Ltd. makes, trade name: イ ペ-Network with 70 weight portion anatase-type titanium oxides
TM), (ダ イ セ Le chemical industry Co., Ltd. makes 29 weight portion sodium carboxymethyl cellulose, trade name: CMC ダ イ セ Le
TM2% solution viscosity is 10mPas) and the mixing of 1 weight portion spice, to wherein adding 50 weight portion Purified Waters, mediated 30 minutes with mediating mixing roll, make hydrous powdery.In ventilation thermostatic drier (ヤ マ ト science society make, DN-81 type) in 50 ℃ with dry 24 hours (diel) of this material.Dry thing is pulverized with small mill (thin river ironworker's manufacturing AP-B type) and is obtained 100 purpose pelletize things.
(embodiment 4)
(ニ チ リ Application KCC makes, trade name: キ Star コ レ-ト to add 10 weight portion sodium carboxymethyl cellulose in 100 weight portion Purified Waters
TM2% solution viscosity is 10mPas), 30 ℃ are stirred dissolving in 1 hour down.(Ishihara Sangyo Kaisha, Ltd. makes, trade name: イ ペ-Network to wherein adding 90 weight portion anatase-type titanium oxides
TM), room temperature stirs down and made it in 30 minutes to disperse.In ventilation thermostatic drier (ヤ マ ト science society make, DN-81 type) in 105 ℃ with dry 24 hours (diel) of this material.Dry thing is pulverized with small mill (thin river ironworker's manufacturing AP-B type) and is obtained 100 purpose pelletize things.
(embodiment 5)
(ニ チ リ Application KCC makes, trade name: キ Star コ レ-ト to add 29 weight portion sodium carboxymethyl cellulose in 100 weight portion Purified Waters
TM2% solution viscosity is 200mPas) and 1 weight portion polyoxyethylene (10) oleyl ether (Nikko Chemicals Co., Ltd's manufacturing, trade name: NIKKOL
TMBO-10TX), 30 ℃ are stirred dissolving in 1 hour down.(Ishihara Sangyo Kaisha, Ltd. makes, trade name: イ ペ-Network to wherein adding 70 weight portion anatase-type titanium oxides
TM), room temperature stirs down and made it in 30 minutes to disperse.In ventilation thermostatic drier (ヤ マ ト science society make, DN-81 type) in 105 ℃ with dry 24 hours (diel) of this material.Dry thing is pulverized with small mill (thin river ironworker's manufacturing AP-B type) and is obtained 100 purpose pelletize things.
(reference examples 1)
(ニ チ リ Application KCC makes, trade name: キ Star コ レ-ト to add 20 weight portion sodium carboxymethyl cellulose in 100 weight portion Purified Waters
TM), 30 ℃ are stirred dissolving in 1 hour down.(Ishihara Sangyo Kaisha, Ltd. makes, trade name: イ ペ-Network to wherein adding 80 weight portion Titanium Dioxide Rutile Top grades
TM), room temperature stirs down and made it in 30 minutes to disperse.In ventilation thermostatic drier (ヤ マ ト science society make, DN-81 type) in 105 ℃ with dry 24 hours (diel) of this material.Dry thing is pulverized with small mill (thin river ironworker's manufacturing AP-B type) and is obtained 100 purpose pelletize things.
(reference examples 2)
(Ishihara Sangyo Kaisha, Ltd. makes, trade name: イ ペ-Network with 70 weight portion Titanium Dioxide Rutile Top grades
TM) (SongGu Chemical Industrial Co., Ltd makes, trade name: パ イ Application デ Star Network ス) mix, to wherein adding 100 weight portion Purified Waters, room temperature stirs down and made it in 30 minutes to disperse with 30 weight portion soluble starches.In ventilation thermostatic drier (ヤ マ ト science society make, DN-81 type) in 105 ℃ with dry 24 hours (diel) of this material.Dry thing is pulverized with small mill (thin river ironworker's manufacturing AP-B type) and is obtained 100 purpose pelletize things.
(reference examples 3)
(Nikko Chemicals Co., Ltd makes dissolving 30 weight portion polyoxyethylene (10) oleyl ethers, trade name: NIKKOL in 100 weight portion Purified Waters
TMBO-10TX), (Ishihara Sangyo Kaisha, Ltd. makes, trade name: イ ペ-Network to wherein adding 70 weight portion anatase-type titanium oxides
TM), room temperature stirs down and made it in 30 minutes to disperse.In ventilation thermostatic drier (ヤ マ ト science society make, DN-81 type) in 105 ℃ with dry 24 hours (diel) of this material.Dry thing is pulverized with small mill (thin river ironworker's manufacturing AP-B type) and is obtained 100 purpose pelletize things.
Test example 1 (dissolubility of baths and dispersion stabilization test)
Production Example 1 (Powdered baths)
The various compositions that reference examples 4～6 is put down in writing in embodiment 6～10 and the table 2 in pelletize thing that embodiment 1～5 and reference examples 1～3 are obtained and the table 1 add omnipotent stirring mixer, and (three English systems are done manufacturing, 25AM-rr (Qr)) in, mixes after 10 minutes and obtained Powdered baths.Dissolubility and dispersion stabilization test have been carried out with this Powdered bath oil composition.Dissolubility and dispersion stabilization test method are as follows.
The baths of the ampoule just made is dissolved in the 200 liters of tap waters (hardness is that 50 degree and 150 are spent) that are heated to 40 ℃ the dissolubility of visual judgement baths and dispersion stabilization (turbidity).And this baths packed in the paper-made vessel, preserved 30 down in 40 ℃ of room temperatures and 75% relative humidity environment, this baths of ampoule is dissolved in the 200 liters of tap waters (hardness is 50 degree and 150 degree) that are heated to 40 ℃ the dissolubility of visual judgement baths and dispersion stabilization (turbidity).
In this solubility test, by the baths after just making and the product of preserving are tested, can confirm preparation deliquescent through the time variation.Determinating reference as hereinafter described.
Production Example 2 (graininess baths)
Each composition mixing film-making that reference examples 7 is put down in writing in embodiment 11, the table 2 in the pelletize thing that embodiment 1 and reference examples 2 are obtained and the table 1 is pulverized with small mill (thin river ironworker's manufacturing AP-B type) and to be obtained 100 purpose pelletize things.Dissolubility and dispersion stabilization test have been carried out with this graininess bath oil composition.Its test method is identical with the method that Production Example 1 is put down in writing.
Production Example 3 (tablet shape baths)
Each composition that reference examples 8～9 is put down in writing in embodiment 12～13,15, the table 2 in pelletize thing that embodiment 1,4,5, reference examples 1～2 are obtained and the table 1, perhaps each composition that embodiment 14 is put down in writing in the table 1 adds omnipotent stirring mixer (three English systems is done manufacturing, 25AM-rr (Qr)) in, mix and stirred 10 minutes, with having obtained tablet shape baths after the film-making of single-shot pelleter.Dissolubility and dispersion stabilization test have been carried out with this tablet shape bath oil composition.Test method is identical with the method for Production Example 1 record.
Production Example 4 (bulk baths)
Each composition that reference examples 10 in embodiment 16, the table 2 in the pelletize thing of embodiment 3, reference examples 1 and the table 1 is put down in writing; perhaps each composition that embodiment 17 is put down in writing in the table 1 adds omnipotent stirring mixer (three English systems is done manufacturing; 25AM-rr (Qr)) in; mix and stirred 10 minutes, with having obtained the bulk baths after Drygranulatemachine (briquetting machine) pelletize.Dissolubility and dispersion stabilization test have been carried out with this bulk bath oil composition.Test method is identical with the method that Production Example 1 is put down in writing.
Table 1
| Composition | Embodiment (weight portion) | |||||||||||||
| ???6 | ???7 | ???8 | ???9 | ??10 | ??11 | ??12 | ??13 | ??14 | ??15 | ??16 | ??17 | |||
| Powdered | Powdered | Powdered | Powdered | Powdered | Graininess | The tablet shape | The tablet shape | The tablet shape | The tablet shape | Bulk | Bulk | |||
| Sodium sulfate | ??30 | ??30 | ??30 | ??30 | ||||||||||
| Sodium bicarbonate | ??66 | ??63 | ??96 | ??66 | ??66 | ??40 | ??40 | ??38 | ??38 | ??38 | ??38 | ??38 | ||
| Sodium carbonate | ??20 | ??20 | ??20 | ??20 | ??20 | ??20 | ??20 | |||||||
| Malic acid | ??36 | ??36 | ??35 | ??35 | ??35 | ??35 | ??35 | |||||||
| Spice | In right amount | In right amount | In right amount | In right amount | In right amount | In right amount | In right amount | In right amount | In right amount | In right amount | In right amount | |||
| Pigment | In right amount | In right amount | In right amount | In right amount | In right amount | In right amount | ||||||||
| Sodium carboxymethyl cellulose | ??2 | ??2 | ||||||||||||
| Anatase-type titanium oxide | ??5 | ??5 | ||||||||||||
| Pelletize thing (embodiment No.) (weight portion) | ???No.1 | ???No.2 | ???No.3 | ???No.4 | ???No.5 | ???No.1 | ???No.1 | ???No.4 | ???No.5 | ???No.3 | ||||
| ???4 | ???7 | ???4 | ???4 | ???4 | ???4 | ???4 | ???7 | ???7 | ???7 | |||||
| Ampoule (gram) | ??30 | ??30 | ??30 | ??30 | ??30 | ??40 | ??40 | ??40 | ??40 | ??40 | ??40 | ??40 | ||
| Firm manufactured goods | Dissolubility | Hardness 50 | ??○ | ??○ | ??○ | ??○ | ??○ | ??○ | ??○ | ??○ | ??○ | ??○ | ??○ | ??○ |
| Hardness 150 | ??○ | ??○ | ??○ | ??○ | ??○ | ??○ | ??○ | ??○ | ??○ | ??○ | ??○ | ??○ | ||
| Dispersion stabilization | Hardness 50 | ??○ | ??○ | ??○ | ??△ | ??○ | ??○ | ??○ | ??△ | ??○ | ??○ | ??○ | ??○ | |
| Hardness 150 | ??○ | ??○ | ??○ | ??△ | ??○ | ??○ | ??○ | ??△ | ??○ | ??○ | ??○ | ??○ | ||
| The product of preservation | Dissolubility | Hardness 50 | ??○ | ??○ | ??○ | ??○ | ??○ | ??○ | ??○ | ??△ | ??○ | ??△ | ??○ | ??○ |
| Hardness 150 | ??○ | ??○ | ??○ | ??△ | ??△ | ??○ | ??○ | ??△ | ??○ | ??△ | ??○ | ??○ | ||
| Dispersion stabilization | Hardness 50 | ??○ | ??○ | ??○ | ??△ | ??○ | ??○ | ??○ | ??△ | ??○ | ??○ | ??○ | ??○ | |
| Hardness 150 | ??○ | ??○ | ??○ | ??△ | ??○ | ??○ | ??○ | ??△ | ??○ | ??○ | ??○ | ??○ | ||
＜determinating reference 〉
Dissolubility
Zero: dissolving rapidly
△: though dissolving needs some times
*: become white particle and dissolve through several minutes, perhaps do not dissolve fully and produce dissolution residual substance.
Dispersion stabilization
Zero: homogeneous disperses stable muddy (can obtain turbidity) more than 5 minutes.
△: though disperse through homogeneous, can not keep turbidity because of sedimentation slowly.
*: disperse inequality or can not obtain abundant turbidity.
Table 2
| Composition | Reference examples (weight portion) | ||||||||
| ????4 | ????5 | ????6 | ????7 | ????8 | ????9 | ????10 | |||
| Powdered | Powdered | Powdered | Graininess | The tablet shape | The tablet shape | Bulk | |||
| Sodium sulfate | ????30 | ????30 | |||||||
| Sodium bicarbonate | ????66 | ????63 | ????96 | ????40 | ????38 | ????40 | ????40 | ||
| Sodium carbonate | ????20 | ????20 | ????20 | ????20 | |||||
| Malic acid | ????36 | ????35 | ????36 | ????36 | |||||
| Spice | In right amount | In right amount | In right amount | In right amount | In right amount | In right amount | In right amount | ||
| Pigment | In right amount | In right amount | In right amount | In right amount | In right amount | ||||
| Pelletize thing (reference examples No.) (weight portion) | ????No.1 | ????No.2 | ????No.3 | ????No.2 | ????No.1 | ????No.2 | ????No.1 | ||
| ????4 | ????7 | ????4 | ????4 | ????7 | ????4 | ????4 | |||
| Ampoule (gram) | ????30 | ????30 | ????30 | ????40 | ????40 | ????40 | ????40 | ||
| Firm manufactured goods | Dissolubility | Hardness 50 | ????△ | ????△ | ????△ | ????△ | ????△ | ????△ | ????△ |
| Hardness 150 | ????× | ????△ | ????△ | ????× | ????△ | ????△ | ????△ | ||
| Dispersion stabilization | Hardness 50 | ????○ | ????○ | ????× | ????○ | ????○ | ????○ | ????○ | |
| Hardness 150 | ????△ | ????○ | ????× | ????○ | ????× | ????○ | ????△ | ||
| The product of preservation | Dissolubility | Hardness 50 | ????△ | ????× | ????× | ????△ | ????× | ????× | ????× |
| Hardness 150 | ????× | ????× | ????× | ????× | ????× | ????× | ????× | ||
| Dispersion stabilization | Hardness 50 | ????○ | ????○ | ????× | ????△ | ????△ | ????△ | ????△ | |
| Hardness 150 | ????× | ????○ | ????× | ????× | ????× | ????△ | ????× | ||
＜determinating reference 〉
Dissolubility
Zero: dissolving rapidly
△: though dissolving needs some times
*: become white particle and dissolve through several minutes, perhaps do not dissolve fully and produce dissolution residual substance.
Dispersion stabilization
Zero: homogeneous disperses stable muddy (can obtain turbidity) more than 5 minutes.
△: though disperse through homogeneous, can not keep turbidity because of sedimentation slowly.
*: disperse inequality or can not obtain abundant turbidity.
From this dissolubility and dispersion stabilization result of the test, though contain * be the embodiment 9 and 13 of pelletize thing 4 beyond claim 2 scope, and contain the embodiment 10 of the pelletize thing 5 that wherein contains surfactant and 15 preservation product all are judged as △, but other examples all are judged as zero.
In contrast to this, the baths after just having made in the reference examples almost all is judged as △, and the product of preserving almost in all reference examples, all be judged as *.
Test example 2 (preserving fixed, the variable color and the stability test of variation, the preparation of product outward appearance)
The bath oil composition of embodiment 6～17 and reference examples 4～10 is packed in the paper-made vessel, from moisture absorption cause whether preparation fixed, the preparation viewpoint of brown stain and preparation state whether, 40 ℃ of visual examination room temperatures, 75% relative humidity environment are preserved the outward appearance of preparation after 30 days down.
Be not evaluated as zero to have, almost not have, some are arranged or be evaluated as *, whether with regard to fixed and variable color (brownization) is estimated, and the results are shown among the table 3.
Table 3
| Prescription | Preparation fixed | The variable color of preparation |
| Embodiment 6 | ????○ | ????○ |
| Embodiment 7 | ????○ | ????○ |
| Embodiment 8 | ????○ | ????○ |
| Embodiment 9 | ????○ | ????○ |
| Embodiment 10 | ????○ | ????○ |
| Embodiment 11 | ????○ | ????○ |
| Embodiment 12 | ?????- | ????○ |
| Embodiment 13 | ?????- | ????○ |
| Embodiment 14 | ?????- | ????○ |
| Embodiment 15 | ?????- | ????○ |
| Embodiment 16 | ?????- | ????○ |
| Embodiment 17 | ?????- | ????○ |
| Reference examples 4 | ????× | ????○ |
| Reference examples 5 | ????× | ????× |
| Reference examples 6 | ????× | ????× |
| Reference examples 7 | ????× | ????× |
| Reference examples 8 | ?????- | ????○ |
| Reference examples 9 | ?????- | ????× |
| Reference examples 10 | ?????- | ????○ |
This result of the test finds that the baths of embodiment 7～18 does not find that all appearance character changes, and reference examples 4～7 and reference examples 9 find to occur at least fixed or variable color.
Claims (7)
1. a pelletize thing wherein contains anatase-type titanium oxide and water soluble polymer.
2. according to the described pelletize thing of claim 1, wherein the weight ratio X between anatase-type titanium oxide and water soluble polymer (anatase-type titanium oxide/water soluble polymer) is 4 〉=X 〉=1.
3. according to claim 1 or 2 described pelletize things, wherein water soluble polymer is at least a material of selecting from one group of material that gelatin, arabic gum, heal skin ulcer glue, Tragacanth, starch, carboxymethyl cellulose, sodium carboxymethyl cellulose, methylcellulose, hydroxyethyl-cellulose, sodium polyacrylate and polyvinyl pyrrolidone are formed.
4. according to any one described pelletize thing in the claim 1～3, wherein do not contain surfactant in fact.
5. a bath oil composition wherein contains any one described pelletize thing in the claim 1～4.
6. a solid-state bath oil composition wherein contains anatase-type titanium oxide and water soluble polymer, and does not contain surfactant in fact.
7. according to the manufacture method of any one described pelletize thing in the claim 1～4, it is characterized in that anatase-type titanium oxide, water soluble polymer and water are mixed, make the pelletize thing after the drying.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP166869/2002 | 2002-06-07 | ||
| JP2002166869A JP2004010543A (en) | 2002-06-07 | 2002-06-07 | Granule used as turbidity-forming agent, method for producing the same, and bath agent composition containing the granule |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1466942A true CN1466942A (en) | 2004-01-14 |
Family
ID=29996416
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA031425046A Pending CN1466942A (en) | 2002-06-07 | 2003-06-06 | Granulating substance used as whitening agent and method for manufacturing the same, bath preparation composition containing the same |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JP2004010543A (en) |
| CN (1) | CN1466942A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101966129A (en) * | 2010-07-14 | 2011-02-09 | 山东海泽纳米材料有限公司 | Method for preparing artificial carbonated spring preparation |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5285210B2 (en) * | 2006-02-22 | 2013-09-11 | 花王株式会社 | Bath additive |
| JP5072570B2 (en) * | 2007-12-18 | 2012-11-14 | 花王株式会社 | Granular foam bath agent |
-
2002
- 2002-06-07 JP JP2002166869A patent/JP2004010543A/en active Pending
-
2003
- 2003-06-06 CN CNA031425046A patent/CN1466942A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101966129A (en) * | 2010-07-14 | 2011-02-09 | 山东海泽纳米材料有限公司 | Method for preparing artificial carbonated spring preparation |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2004010543A (en) | 2004-01-15 |
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