CN1123336C - Liquid personal cleansing compositions which contain encapsulated lipophilic skin moisturizing agent comprised of relatively large droplets - Google Patents
Liquid personal cleansing compositions which contain encapsulated lipophilic skin moisturizing agent comprised of relatively large droplets Download PDFInfo
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- CN1123336C CN1123336C CN97199040A CN97199040A CN1123336C CN 1123336 C CN1123336 C CN 1123336C CN 97199040 A CN97199040 A CN 97199040A CN 97199040 A CN97199040 A CN 97199040A CN 1123336 C CN1123336 C CN 1123336C
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/11—Encapsulated compositions
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P17/00—Drugs for dermatological disorders
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/10—Washing or bathing preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/41—Particular ingredients further characterized by their size
- A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns
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Abstract
Liquid personal cleansing compositions which comprise from about 1 % to about 35 % of encapsulated lipophilic skin moisturizing agents, from about 0.1 % to about 5 % of a stabilizer, from about 5 % to about 30 % of a lathering surfactant and water are disclosed. The encapsulated lipophilic skin moisturizing agent comprises a lipophilic skin moisturizing agent encapsulated within a complex coascervate comprising a polycation and a polyanion. The lipophilic skin moisturizing agent comprises droplets having a particle size distribution such that at least about 10 % by weight of the droplets have a diameter of at least about 100 microns. The encapsulated lipophilic skin moisturizing agent is essentially free of cross-linking agent.
Description
Technical field
The present invention relates to liquid personal cleansing composition, it provides skin with clinical effective humidification.Liquid personal cleansing composition of the present invention is the emulsion that contains humidification phase and water, and this humidification comprises the lipophilic skin humidizer of sealing mutually, and water comprises surfactant and stabilizing agent.The oleophylic humidizer that constitutes this liquid personal cleansing composition itself constitutes the drop of certain grain size distribution, promptly at least about the diameter of 10% heavy drop greater than about 100 microns.
Background technology
The liquid personal cleaning product becomes more popular in the U.S. and the whole world.Good liquid personal cleaning compositions must meet some standards.For example, accept for making consumer, the liquid personal cleaning product must show favourable cleaning performance, must show good bubbling character, must to skin gentleness (not causing drying or stimulation) and preferably in addition reply skin the benefit of humidification is provided.
The liquid personal cleaning product that contains high concentration lipophilic skin regulator is disclosed.In fact, consumer goods, as Olay humidification body lotion, special when using simultaneously with the Olay foam cleaner, the lipophilic skin regulator is deposited on the skin, is subjected to very much the welcome of consumer.But some consumers wish that more these liquid personal cleansing products have obviously bigger humidification effect.Therefore, be desirable to provide liquid personal cleansing composition with obvious bigger moisturization.
Have now found that if the lipophilic skin humidizer comprises relatively large oil droplet, the deposition of lipophilic skin humidizer on skin can obviously increase.Unfortunately, very difficult preparation contains the personal cleaning compositions of this lipophilic skin humidizer, because during the processing of fluid composition is especially packed, larger oil droplet is easy to destroy and forms than granule.But find again now,, can preserve the integrity of the larger particles that comprises the lipophilic skin humidizer by sealing humidizer with complex coacervate.This complex coacervate must have following character: can preserve the integrity of bulky grain work in-process, but lipophilic skin humidizer wherein is deposited on the skin.
Summary of the invention
The present invention relates to contain the humidification liquid personal cleansing emulsion fluid composition of the aqeous cleansing phase of humidification.Humidification comprise mutually composition weight about 1% to about 35% seal the lipophilic skin humidizer.Aqueous cleaning comprises about 0.1% to about 10% stabilizing agent of composition weight, about 5% to about 30% foaming surface active agent and water mutually.
The lipophilic skin humidizer of sealing comprises the lipophilic skin humidizer that is encapsulated in the complex coacervate, and this coacervate comprises minimum polycation and the polyanion that filters weight (filtrate weight) 10 grams.The hardness of complex coacervate is about 50 to about 1400 gram forces.The lipophilic skin humidizer constitutes drop, and its particle size distribution is at least about the diameter of 10% heavy drop at least about 100 microns.
Specifically, the invention discloses following technical scheme:
1. liquid personal cleansing composition, it comprises:
A) humidification phase comprises the lipophilic skin humidizer of sealing of composition weight 1% to 35%;
Wherein the lipophilic skin humidizer is encapsulated in the complex coacervate, and this coacervate comprises minimum
Filter the polycation and the polyanion of weight 10 grams, wherein said complex coacervate
Hardness be 50 to 1400 gram forces and wherein the agent of lipid skin moisturizing constitute certain particle diameter
The drop that distributes, the diameter that makes at least 10% heavy drop is greater than 100 microns; With
B) water comprises:
I) 0.1% of composition weight to 10% stabilizing agent;
Ii) 5% of composition weight to 30% foaming surface active agent; With
Iii) water, wherein stabilizing agent is the stabilizing agent of crystalline hydroxyl, is selected from:
(i)
Wherein
R1 is
R2 is R1 or H
R3 is R1 or H
R4 is C
0-20Alkyl
R5 is C
0-20Alkyl
R6 is C
0-20Alkyl
R4+R5+R6＝C
10-22
And 1≤x+y≤4 wherein;
(ii)
Wherein
R7 is-R4 (CHOH) xR5 (CHOH) yR6
M is Na+, K+ or Mg++ or H; And
(iii) its mixture.
2. the 1st liquid personal cleansing composition, its deposition value at least 10 microgram/square centimeters.
3. the 2nd liquid personal cleansing composition, wherein at least 10% heavy lipophilic skin humidizer granule of sealing is non-sphere in the finished product.
4. the 3rd liquid personal cleansing composition, wherein complex coacervate comprises 0.1% to 15% polycation and 0.01% to 10% polyanion.
5. the 4th liquid personal cleansing composition, wherein the ratio of polycation and polyanion is 30: 1 to 1: 5 in the complex coacervate.
6. the 5th liquid personal cleansing composition, wherein personal cleaning compositions contains 1% to 30% lipophilic skin humidizer.
7. the 6th liquid personal cleansing composition, wherein the denseness of lipophilic skin humidizer is 5 to 5,000 pools, shearing index is 0.1 to 0.9.
8. the 7th liquid personal cleansing composition, wherein polycation comprises gelatin.
9. the 8th liquid personal cleansing composition, wherein polyanion is selected from Quadrafos, arabic gum, sodium alginate and composition thereof.
10. the 9th liquid personal cleansing composition, wherein the size of at least 50% heavy drop that comprises the lipophilic skin humidizer is greater than 100 microns.
11. the 1st liquid personal cleansing composition, wherein the viscosity of liquid personal cleansing composition is 2,000 to 100,000 centipoises, and wherein the deposition value of liquid personal cleansing composition is at least 30 microgram/square centimeters.
12. the 11st liquid personal cleansing composition, at least 50% the particulate size that wherein comprises the lipophilic skin humidizer is greater than 200 microns.
13. a liquid personal cleansing composition, it comprises:
A) humidification phase comprises the lipophilic skin humidizer of sealing of composition weight 1% to 35%; Wherein the lipophilic skin humidizer is encapsulated in the complex coacervate, this coacervate comprises minimum polycation and the polyanion that filters weight 10 grams, wherein the agent of lipid skin moisturizing constitutes the drop of certain grain size distribution, and promptly the diameter of at least 10% heavy drop is greater than 100 microns; The essentially no cross-linking agent of wherein sealing of lipophilic skin humidizer; With
B) water comprises:
I) 0.1% of composition weight to 10% stabilizing agent;
Ii) 5% of composition weight to 30% foaming surface active agent; With
Iii) water, wherein stabilizing agent is the stabilizing agent of crystalline hydroxyl, is selected from:
(i)
Wherein
R1 is
R2 is R1 or H
R3 is R1 or H
R4 is C
0-20Alkyl
R5 is C
0-20Alkyl
R6 is C
0-20Alkyl
R4+R5+R6＝C
10-22
And 1≤x+y≤4 wherein;
(ii)
Wherein
R7 is-R4 (CHOH) xR5 (CHOH) yR6
M is Na+, K+ or Mg++ or H; And
(iii) its mixture.
14. the 13rd liquid personal cleansing composition, wherein the deposition value is at least 10 microgram/square centimeters.
15. the 14th liquid personal cleansing composition, wherein at least 30% heavy lipophilic skin humidizer granule of sealing is non-sphere in the final products.
16. the 15th liquid personal cleansing composition, wherein complex coacervate comprise 0.1% to
15% polycation and 0.01% to 10% polyanion.
17. the 16th liquid personal cleansing composition, wherein the ratio of polycation and polyanion is 30: 1 to 1: 5 in the complex coacervate.
18. the 17th liquid personal cleansing composition, wherein personal cleaning compositions contains 1% to 30% lipophilic skin humidizer.
19. the 18th liquid personal cleansing composition, wherein the denseness of lipophilic skin humidizer is 5 to 5,000 pools, and shearing index is 0.1 to 0.9.
20. the 19th liquid personal cleansing composition, wherein polycation comprises gelatin.
21. the 20th liquid personal cleansing composition, wherein polyanion is selected from Quadrafos, arabic gum, sodium alginate and composition thereof.
22. the 21st liquid personal cleansing composition, wherein the size of at least 50% heavy drop that comprises the lipophilic skin humidizer is greater than 100 microns.
23. the 13rd liquid personal cleansing composition, wherein the viscosity of liquid personal cleansing composition is 2,000 to 100,000 centipoises, and wherein the deposition value of liquid personal cleansing composition is at least 30 microgram/square centimeters.
24. the 23rd liquid personal cleansing composition, at least 50% the particulate size that wherein comprises the lipophilic skin humidizer is greater than 200 microns.
25. a liquid personal cleansing composition, it comprises:
A) 0.1% to 5% polycation;
B) 0.01% to 1% polyanion;
C) 0.75% to 30% denseness is 5 to 5,000 pools, and shearing index is the lipophilic skin humidizer of 0.1 to 0.9 pool, and wherein the particle size distribution of lipophilic skin humidizer is that the diameter of at least 10% heavy drop is greater than 100 microns;
D) 0.1% to 10% stabilizing agent;
E) 5% to 30% foaming surface active agent; With
F) water;
Wherein the viscosity of personal cleaning compositions is 2,000 to 100,000 centipoises; Wherein polycation is 30: 1 to 1: 5 with the ratio of polyanion; The essentially no cross-linking agent of liquid personal cleansing composition wherein, wherein stabilizing agent is the stabilizing agent of crystalline hydroxyl, is selected from:
(i)
Wherein
R1 is
R2 is R1 or H
R3 is R1 or H
R4 is C
0-20Alkyl
R5 is C
0-20Alkyl
R6 is C
0-20Alkyl
R4+R5+R6＝C
10-22
And 1≤x+y≤4 wherein;
(ii)
Wherein
R7 is-R4 (CHOH) xR5 (CHOH) yR6
M is Na+, K+ or Mg++ or H; And
(iii) its mixture.
26. the 25th liquid personal cleansing composition, wherein the deposition value is greater than 20 microgram/square centimeters.
27. the 26th liquid personal cleansing composition, wherein polycation comprises gelatin.
28. the 27th liquid personal cleansing composition, wherein polyanion is selected from Quadrafos, arabic gum, sodium alginate and composition thereof.
29. the 28th liquid personal cleansing composition, wherein the size of at least 50% heavy drop that comprises the lipophilic skin humidizer is greater than 100 microns.
30. the 25th liquid personal cleansing composition, wherein the size of at least 50% heavy drop that comprises the lipophilic skin humidizer is at least 200 microns.Detailed Description Of The Invention
The invention relates to the liquid personal cleaning emulsion compositions, said composition provides the clinical effective humidification to skin." liquid personal cleaning compositions " of usefulness refers to rinsing type personal cleaning compositions and includes, but not limited to body lotion, liquid hand soaps and shampoo herein.Liquid personal cleaning compositions of the present invention is an emulsion, and this emulsion comprises humidification phase that contains the lipophilic skin humidizer and the aqueous cleaning that contains surfactant, stabilizing agent and water mutually.The drop of forming the oleophylic humidizer formation certain grain size distribution of liquid personal cleansing composition of the present invention itself, promptly at least about the diameter of 10% heavy drop greater than about 100 microns.Among the present invention, particle diameter is meant the size of granule maximum.Find, when comprise the lipophilic skin humidizer at least about the diameter of 10% heavy drop during greater than about 100 microns, the liquid personal cleansing composition that contains the lipophilic skin humidizer can provide skin with clinical effective humidification.
Unfortunately, be difficult to make the personal cleaning compositions that lipophilic skin humidizer wherein has required particle size distribution, even drop initially has required size because in Cleasing compositions processing, especially during the packing big drip to be easy to destroy form droplet.But have now found that; the liquid personal cleansing composition that contains the lipophilic skin humidizer with required particle size distribution can obtain, and method is to form around the complex coacervate of the lipophilic skin humidizer integrity with the big drop of protection during the processing (especially packing) of liquid personal cleansing composition.Yet in order to obtain the humidification effect, the lipophilic skin humidizer must be able to be deposited on the skin.Therefore, the complex coacervate of sealing the lipophilic skin humidizer during liquid personal cleansing composition processing must have this character, and promptly it can make the lipophilic skin humidizer that comprises wherein be deposited on the skin.
The key factor that influences the performance of coacervate is hard relatively/softness and thickness of complex coacervate, and performance wherein is meant during the protection processing particle integrity and still allows humidizer to be deposited on the skin.Especially, complex coacervate must with the integrity of lipophilic skin humidizer during the processing of protection liquid personal cleansing composition, but must enough softly approach so that the lipophilic skin humidizer of sealing can be deposited on the skin enough firmly with thick.
The suitable stiffness of having found complex coacervate is about 50 to about 1400 gram forces, and preferred about 400 to about 1200 gram forces, and more preferably from about 600 to about 1000 gram forces, and the coacervate intensity method that this value is partly described by analytical method is hereinafter tested.Further find again, complex coacervate has suitable thickness under following situation, in finished product at least about 10%, preferably at least about 30%, more preferably at least about 50%, be non-when spherical at least about 70% the lipophilic skin humidizer granule of sealing most preferably, this value is measured by the aspherical particle percentage rate method of analytical method part hereinafter.Among the present invention, as fruit granule draw ratio (long divided by wide) greater than 1.1 o'clock its be non-sphere.Think that particulate non-sphere is directly related with the thickness of complex coacervate, and the thickness of complex coacervate directly with given particle size distribution under deposition proportional.
Below describe the liquid personal cleansing composition that contains the lipophilic skin humidizer in detail, comprise wherein contained material and preparation method thereof, wherein the diameter of at least 10% heavy drop is greater than about 100 microns.I. composition
A. the lipophilic skin humidizer of sealing
1. complex coacervate
The method that a kind of size while of keeping the big drop that contains the lipophilic skin humidizer in the liquid personal cleansing composition processing makes the lipophilic skin humidizer can be deposited on skin again is to form complex coacervate around the lipophilic skin humidizer.The complex coacervate here must have performance like this, oarse-grained integrity during promptly its protection liquid personal cleansing composition is processed, but lipophilic skin humidizer wherein can be deposited on the skin.The complex coacervate here has required performance so that described effect to be provided.
Complex coacervate is the minimum polycation of weight 10 grams and the complex of polyanion of filtering.Complex coacervate generally contains has an appointment 0.1% to about 15%, and preferred about 0.5% to about 10%, and more preferably from about 1% to about 5% polycation and about 0.01% to about 10%, preferred about 0.05% is to about 5%, more preferably from about 0.1% to about 1% polyanion.Polycation is about 30: 1 to about 1: 5 with the ratio of polyanion in the complex coacervate, preferred about 20: 1 to about 1: 2, and more preferably from about 15: 1 to about 1: 1.Each encapsulation of general about 50% to about 95% is made up of the lipophilic skin humidizer.The lipophilic skin humidizer was generally about 5: 1 to about 1: 5 with the ratio of coacervate complex, and preferred about 3: 1 to about 1: 3, more preferably from about 2: 1 to about 1: 2.
Be suitable for minimum that the polycation of complex coacervate of the present invention has and filter weight and be about 10 grams, preferably be about 15 grams, more preferably be about 20 grams, measure by the filtration weight method that analytical method is hereinafter partly illustrated.In order to protect the integrity of lipophilic skin humidizer granule in liquid personal cleansing composition processing, when combining, filter weight and can not form enough thick coacervate less than about 10 polycations that restrain with polyanion.
Mean molecule quantity from about 50 to the preferred polycation of about protein of 1,000,000 for using among the present invention.The preferred protein of Shi Yonging comprises herein, for example, and gelatin, ovalbumin, serum albumin, casein, chitin and composition thereof.
Gelatin is particularly preferred protein as polycation in the present invention.Gelatin can be characterized by bloom strength (bloom strength).Bloom strength is for being 12.7 millimeters flat plunger with a diameter, 4 millimeters required power of gel surface compression (is unit mensuration with the gram) of 63/3% w/w that formed in 10 ℃ of following 16-18 hours.Gauge is the Blume gelometer.Also can use the Blume electronics frozen glue tester of semi-automatic type.The bloom strength of the gelatin that is suitable for herein using is from about 60 to about 300, preferably from about 100 to about 300, and more preferably from about 150 to about 300, most preferably from about 200 to about 300.
Other has the polycation of required filtration weight, also can be suitable for herein use as polyvinylamine and cellulose derivative.
Be applicable to that polyanion herein comprises, for example, Quadrafos, Radix Acaciae senegalis, sodium alginate, carrageenin, cellulose acetate, phthalate, pectin, carboxymethyl cellulose, ethylidene maleic anhydride and composition thereof.
Quadrafos is the particularly preferred polyanion that is applicable to herein.
2. lipophilic skin humidizer
Personal cleaning compositions has herein used the lipophilic skin humidizer.When the lipophilic skin humidizer was deposited on the skin of user, the agent of lipid skin moisturizing provided the benefit of humidification to the user of personal cleansing product.Find, being deposited under the following situation of lipophilic skin humidizer obviously increases, promptly work as at least about 10%, preferably at least about 20%, more preferably at least about 30%, again preferably at least about the diameter of the 50% and most preferably from about 80% heavy drop that comprises the lipophilic skin humidizer greater than about 100 microns, be preferably greater than about 200 microns, more preferably greater than about 300 microns, be preferably greater than about 400 microns and during most preferably greater than about 500 microns again, this value is measured by the described particle size distribution method of following analytical method part.Usually, big particle diameter lipophilic skin humidizer number of particles is many more, and particle grain size is big more, and then the deposition of humidizer on skin is big more.
The lipophilic skin humidizer that has used the explanation of two class rheological parameters to use herein.The viscosity of lipophilic skin humidizer is with denseness (k) and shear index (n) expression.The denseness (k) that usually has of the lipophilic skin humidizer of Shi Yonging is from about 5 to about 5,000 pools herein, preferably from about 10 to about 3,000 pools, more preferably from about 50 to about 2,000 pools, measures as denseness (k) method of statement in the analytical method part hereinafter.The shearing index (n) that the suitable lipophilic skin humidizer that herein uses has in addition is from about 0.01 to about 0.9, preferably from about 0.1 to about 0.5, more preferably from about 0.2 to about 0.5, measures as the shearing index method of statement in the analytical method part hereinafter.
When not being subjected to the restriction of any theory, it is believed that the rheological equationm of state is different from herein the lipophilic skin humidizer of explanation or is easy to very much emulsifying thereby can not deposits, perhaps too " firmly " is to such an extent as to can not adhere to or be deposited on the skin and the benefit of humidification is provided.In addition, the rheological equationm of state of lipophilic skin humidizer is also very important to the sensation of user.Some lipophilic skin humidizers, be deposited on the skin after, be considered to too sticking for user not preferred.
Under some situation, the lipophilic skin humidizer can be existed as Vaughan by its solubility parameter
Cosmetics and washing product, the 103rd volume, the definition in the 47-69 page or leaf (in October, 1988) desirably illustrates.Vaughan solubility parameter (VSP) is from about 5 to 10, preferably is applicable to herein liquid personal cleaning compositions from about 5.5 to 9 lipophilic skin humidizer.
A large amount of lipid feedstocks and raw mix are suitable for being used as the lipophilic skin humidizer in personal cleaning compositions of the present invention.Preferably, the lipophilic skin regulator is selected from hydrocarbon ils and wax, polysiloxanes, derivative of fatty acid, cholesterol, cholesterin derivative, diglyceride and triglyceride, vegetable oil, vegetable oil derivatives, stodgy liquid oil, as authorize the United States Patent (USP) 3 of Mattson on August 17th, 1971,600,186, it all is the patent 4 of authorizing people such as Jandacek on January 25th, 1977,005,195 and 4,005, illustrate in 196, all these are incorporated herein by reference, or the blend of easy digestive fluid oil or nondigestible liquid oil and solid polyalcohol polyester, as authorize the United States Patent (USP) 4 of Jandacek on January 10th, 1989,797,300; It all is the United States Patent (USP) 5 of authorizing Letton on April 26th, 1994,306,514,5,306, illustrate in 516 and 5,306,515, all these are incorporated herein by reference, and aceto-glyceride, Arrcostab, alkenyl esters, lanoline and its derivant, emulsus triglyceride, wax ester, Cera Flava derivant, sterol, phospholipid and composition thereof.Fatty acid, fatty acid soaps and water-soluble polyol will be got rid of from our scope of lipid skin moisturizing agent especially.
Hydrocarbon ils and wax: some examples have vaseline, mineral oil, microwax, polyolefin (as hydrogenation and non-hydrogenated polybutene and poly decene), alkane, azo-bordeaux, ceresine, polyethylene and perhydro-squalene.Vaseline also is applicable to herein lipid skin moisturizing agent to the blend of ratio from about 90: 10 to about 40: 60 vaseline and hydrogenation and non-hydrogenation high-molecular-weight poly butylene of polybutene.
Silicone oil: some examples have dimethicone copolyol, dimethyl polysiloxane, diethyl polysiloxanes, high molecular polydimethylsiloxane, C1-C30 alkyl polysiloxane mixture, phenyl polydimethylsiloxane, dimethiconol and composition thereof.Be more preferably the nonvolatile polysiloxanes that is selected from polydimethylsiloxane, dimethiconol, C1-C30 alkyl polysiloxane mixture and composition thereof.The example of useful herein nonrestrictive polysiloxanes has explanation in people's such as mandate on April 30th, 1991 Ciotti United States Patent (USP) 5,011,681, be incorporated herein by reference.
Diglyceride and triglyceride: some examples have Oleum Ricini, soybean oil, deutero-soybean oil such as maleic acid soybean oil, safflower oil, Oleum Gossypii semen, Semen Maydis oil, walnut oil, Oleum Arachidis hypogaeae semen, olive oil, cod liver oil, almond oil, American Avocado Tree oil, Petiolus Trachycarpi oil and Oleum sesami, vegetable oil and vegetable oil derivatives, Oleum Cocois and the Oleum Cocois of deriving, Oleum Gossypii semen and the Oleum Gossypii semen of deriving, Jojoba oil, cocoa butter or the like.
Used
Aceto-glycerideAnd an example is an acetylated monoglyceride.
LanolineFor preferred and some examples lanoline, lanolin oil, lanolin wax, lanolin alcohol, lanolin fatty acid, isobutylated lanolin ester, acetylated lanolin, Acetylated lanolin alcohols., linoleic acid lanoline alcohol ester, ricinoleic acid (riconoleate) lanoline alcohol ester are arranged with its derivant.
Lipophilic skin regulator that most preferably ought at least 75% is made up of lipid, lipid is selected from: vaseline, the blend of vaseline and high molecular polybutene, mineral oil, the blend of stodgy liquid oil (as liquid cotton seed sucrose octaester) or the easy digestion of liquid or nondigestible oil and solid polyalcohol polyester (as sucrose octaester) by the preparation of C22 fatty acid, wherein liquid easily digestion or nondigestible oil to the ratio of solid polyalcohol polyester from about 96: 4 to about 80: 20, hydrogenation or non-hydrogenated polybutene, microwax, polyolefin, alkane, azo-bordeaux, ceresine, polyethylene, perhydro-squalene, polydimethylsiloxane, alkyl polysiloxane, polymethyl siloxane, methyl phenyl silicone and composition thereof.When using the blend of vaseline and other lipid, vaseline to the ratio of other lipid of choosing (hydrogenation and non-hydrogenated polybutene or poly decene or mineral oil) preferably from about 10: 1 to about 1: 2, more preferably from about 5: 1 to about 1: 1.
3. preparation method
This liquid personal cleansing composition comprises about 1% to about 35%, and preferred about 5% to about 30%, more preferably from about 10% to about 25% the lipophilic skin humidizer of sealing.The amount that is contained in the lipophilic skin humidizer of sealing in the liquid personal cleansing composition of the present invention should make compositions contain about 1% to about 30%, preferred about 3% to about 25%, more preferably from about 5% to about 25% lipophilic skin humidizer.General personal cleaning compositions contains has an appointment 0.1% to about 5%, preferred about 0.3% to about 3%, more preferably from about 0.5% to about 1.5% polycation and about 0.01% is to about 1%, and preferred about 0.02% to about 0.5%, more preferably from about 0.03% to about 0.2% polyanion.
The preparation method of the lipophilic skin humidizer that this is sealed is as follows: the aqueous solution of the heat of preparation polycation and polyanion under the temperature that is higher than lipophilic skin humidizer fusing point, under low shearing condition, sneak into the lipophilic skin conditioner, and do not adopt cross-linking agent.When polycation was gelatin, pH regulator was to about 3.5 to about 5.0.Polycation and polyanion are compounded to form coacervate then, and during cooling, coacervate separates the barrier that the lipophilic skin humidizer is sealed in formation.
Importantly, the mixture of polycation, polyanion and lipophilic skin humidizer must be substantially free of cross-linking agent, to guarantee complex coacervate required hardness is arranged.When adopting the cross-linking agent of obvious content, complex coacervate can't make lipophilic skin humidizer wherein be deposited on the skin too firmly.Here " be substantially free of cross-linking agent " and be meant that mixture contains is lower than about 0.25% cross-linking agent.Cross-linking agent is element, group or the chemical compound of two polymer molecular chains of bridging, and bridging is by main chemical bond interchain certain carbon atom to be linked together.Cross-linking agent for example comprises glutaraldehyde, urea, formaldehyde, phenol, tannic acid and composition thereof.
The particle diameter of lipophilic skin humidizer is the function of the rheological property of the composition of rotating speed, aqueous solution of blender and aqueous solution.Generally speaking, the rotating speed of blender is low more, and the particle diameter of lipophilic skin humidizer is big more.And in order to obtain the lipophilic skin humidizer of bigger particle diameter, aqueous solution does not preferably contain emulsifying agent, as surfactant, and has Newtonianism and non-viscid rheologic behavio(u)r basically.
B. stabilizing agent
Liquid personal cleaning compositions of the present invention usually also contains from about 0.1% to about 10%, preferably from about 0. 25% to about 8%, and from about 0.5% to about 5% stabilizing agent more preferably.
It is coalescent and divide mutually in product to prevent lipophilic skin humidizer drop that stabilizing agent is the stabilizing network that is used for forming crystal form in emulsion.This network shows the viscosity recovery (as thixotropy) according to the time after shearing.
The stabilizing agent of Shi Yonging is not a surfactant herein.Stabilizing agent provides the storage and the stress stability of improvement, separates but can make O/w emulsion pass through foaming, thereby the sedimentary increase on skin of lipophilic skin humidizer is provided.When together using, the sponge of oil-in-water cleaning emulsion of the present invention and aggretion type diamond-mesh particularly like this,, is incorporated herein by reference as authorizing the net silk floss that illustrates in the United States Patent (USP) 5,144,744 of Campagnoli on the 8th JIUYUE in 1992.
In one embodiment of the invention, the stabilizing agent of using in the personal cleaning compositions herein contains the stabilizing agent of the hydroxyl of crystal form.This stabilizing agent can be fatty acid, fatty ester or the fatty soap of hydroxyl, water-insoluble wax or the like.
The stabilizing agent of the hydroxyl of crystal form is selected from:
(i)
Wherein
R2 is R1 or H
R3 is R1 or H
R4 is C
0-20Alkyl
R5 is C
0-20Alkyl
R6 is C
0-20Alkyl
R4+R5+R6＝C
10-22
And 1≤x+y≤4 wherein;
(ii)
Wherein
R7 is-R4 (CHOH) xR5 (CHOH) yR6
M is Na+, K+ or Mg++ or H; Reach (iii) its mixture;
The stabilizing agent of some preferred hydroxyls comprises 12-hydroxy stearic acid, 9,10-dihydroxystearic acid, 9,10-dihydroxy glycerol three stearic acid and 12-hydroxyl glycerol three stearic acid (the castor oil hydrogenated major part is 12-hydroxyl glycerol three stearic acid).12-hydroxyl glycerol three stearic acid are the most preferred emulsion compositions that is used for herein.
When the stabilizing agent of the hydroxyl that uses these crystal forms in the personal cleaning compositions herein, their content be typically liquid personal cleaning compositions from about 0.5% to 10%, preferably from 0.75% to 8%, more preferably from 1.25% to about 5%.Stabilizing agent arrives under the condition near room temperature water insoluble in room temperature.
Additionally, the stabilizing agent that uses in the personal cleaning compositions herein can contain polymeric thickening agent.When using used as stabilizers in the polymeric thickening agent personal cleaning compositions herein, their content be typically composition weight from about 0.01% to about 5%, preferably from about 0.3% to about 3%.Polymeric thickening agent is preferably anion, nonionic, cation or hydrophobically modified polymers, it is 1 that this polymer is selected from molecular weight, 000 to 3,000, the cationic polysaccharide of 000 cationic guar gum class, derive from the anion of acrylic acid and/or methacrylic acid, cation and nonionic homopolymer, anion, cation and non-ionic cellulose resin, dimethyl dialkyl ammonium chloride and acrylic acid cation copolymer, the cationic homopolymer of dimethyl alkyl ammomium chloride, cation polyalkylene and ethyoxyl polyalkyleneimine, molecular weight is from 100,000 to 4,000, Polyethylene Glycol of 000 and composition thereof.Preferably, polymer be selected from sodium polyacrylate, hydroxyethyl-cellulose, cetyl hydroxyethyl cellulose and season hydroxyethyl-cellulose 10.
Additionally, the stabilizing agent that uses in the personal cleaning compositions herein can contain the glycol fatty acid ester of C10-C22.The glycol fatty acid ester of C10-C22 also can together use with the aggretion type thickening agent that above illustrates aptly.This ester is preferably diester, is the diester of C14-C18 more preferably, is most preferably glycol distearate.When using used as stabilizers in the glycol fatty acid ester personal cleaning compositions herein of C10-C22, their content be typically personal cleaning compositions from about 3% to about 10%, preferably from about 5% to about 8%, more preferably from about 6% to about 8%.
The another kind of stabilizing agent that can be used for personal cleaning compositions of the present invention contains dispersive amorphous silica, and this silicon dioxide is selected from fumed silica and precipitated silica and composition thereof.The term of Shi Yonging " dispersive amorphous silica " is meant that little, the average coacervate particle diameter that separates in small, broken bits is less than about 100 microns amorphous silicas herein.
Fumed silica, the arc light silicon dioxide known to being exactly is to make by the vapour phase hydrolysis of Silicon chloride. in oxyhydrogen flame.It is believed that combustion process has generated condensation and formed particulate silicon dioxide molecules.Granule collides, adheres to also clinkering together.The result of this process is the aggregation that has produced three-dimensional branched chain.Aggregation be cooled to the fusing point (about 1710 ℃) of silicon dioxide following after, further collision causes the mechanical interlocking of chain to form coacervate.Precipitated silica and silica dioxide gel generally prepare in aqueous solution.See that title is the Cabot technical data handbook TD-100 of the character and the function of fumed silica " the CAB-O-SIL be untreated ", in October, 1993 and title are the Cabot technical data handbook TD-104 of " the CAB-O-SIL fumed silica among cosmetics and the personal care product ", in March, 1992, both are incorporated herein by reference.
Fumed silica preferably has average coacervate particle diameter from about 0.1 micron to about 100 microns, preferably from about 1 micron to about 50 microns, more preferably from about 10 microns to about 30 microns.Coacervate,,, most preferably is made up of to about 0.3 micron aggregation from about 0.2 micron more preferably from about 0.1 micron to about 5 microns preferably from about 0.05 micron to about 10 microns from about 0.01 micron to about 15 microns mean diameter.This silicon dioxide preferably has specific surface area greater than 50 meters squared per gram, more preferably greater than about 130 meters squared per gram, most preferably greater than about 180 meters squared per gram.
When amorphous silica was used used as stabilizers herein, their content in emulsion compositions was usually from about 0.1% to about 10%, preferably from about 0.25% to about 8%, and more preferably from about 0.5% to about 5%.
Operable the 4th class stabilizing agent contains the dispersive terre verte that is selected from Bentonite, hectorite and composition thereof in the personal cleaning compositions of the present invention.Bentonite is colloidal aluminum sulfate clay.See the Merck index, the 11st edition, 1989,1062,164 pages of clauses and subclauses were quoted as a reference.Hectorite is the clay that contains sodium, magnesium, lithium, silicon, oxygen, hydrogen and fluorine.See the Merck index, the 11st edition, 1989,4538,729 pages of clauses and subclauses were incorporated herein by reference.
When terre verte was used used as stabilizers in personal cleaning compositions of the present invention, its content was usually from about 0.1% to about 10%, preferably from about 0.25% to about 8%, and more preferably from about 0.5% to about 5%.
C. lathering surfactant
Personal cleaning compositions of the present invention also comprises the lathering surfactant that is selected from anion surfactant, non-ionic surface active agent, cationic surfactant, amphoteric surfactant and composition thereof.
Lathering surfactant is defined as surfactant or surfactant mixture herein, the equilibrium surface tension of measuring down in 25 ℃ of critical micelle concentrations (CMC) after it mixes is between 15 and 50 dynes per centimeter, preferably between 25 and 40 dynes per centimeter.The surface tension of some surfactant mixtures is lower than the surface tension of its indivedual compositions.
Personal cleaning compositions herein contains from about 5% to about 30%, preferably from about 5% to about 25%, and from about 10% to about 25% lathering surfactant most preferably.
The anion surfactant of Shi Yonging comprises herein: acyl-hydroxyethyl sulfonate; acyl sarcosinates; alkyl glyceryl ether sulfonate; alkyl sulfate; alkyl sulfate; acyl-lactate; methyl-acyl taurine salt; paraffin sulfonate; linear alkyl benzene sulfonate salt; the N-acyl glutamate; alkyl sulfo succinate; alpha-sulfo fatty acid ester; the alkyl ether carboxy acid salt; alkyl phosphate; ethoxylated alkyl phosphate ester; alpha-olefin sulfate; alkyl ether sulfate (having 1 to 12 ethyoxyl group) and composition thereof, wherein this surfactant contains C8 and is selected to the alkyl chain of C22 and equilibrium ion wherein: Na; K; NH
4, N (CH
2CH
2OH)
3Be preferred when anion surfactant is selected from acyl-hydroxyethyl sulfonate, acyl sarcosinates, acyl-lactate, alkyl sulfo succinate, alkyl glyceryl ether sulfonate, methyl-acyl taurine salt, alkyl ether sulfate, alkyl sulfate, alkyl phosphate and composition thereof, wherein this surfactant contains alkyl chain and the content from about 8% to about 20% of C8 to C14.
Amphoteric synthetic surfactant can not be as independent surfactant in this product, but can be under the lower content of about 10% weight content preferably as cosurfactant from about 1%, preferred type is selected from the single and diacetin of alkyl both sexes, alkyl betaine, alkyl dimethyl amine oxide, alkyl sulfobetaines, alkylamide propyl-betaine, alkylamide propyl hydroxyl sulfo betaine and composition thereof, and wherein this surfactant contains the alkyl chain of C8 to C22.
Non-ionic synthetic surfactant can not be as independent surfactant in this product, but can be preferably as cosurfactant under the lower content of about 15% weight content from about 1%.Preferred type is selected from the ester of polyoxyethylene ester, oxygen ethylene-oxypropylene block copolymer such as the polyoxamine of alkyl glucose amide, alkyl glucose ester, polyoxyethylate amide, fatty alkane amide, alkyl amine oxide, alkyl polyglucoside, polyoxyethylene alkylphenol, fatty acid and poloxamers, anhydrosorbitol and alcohol ester and composition thereof.
Cationic synthetic surfactant can not be as independent surfactant in this product, but can be preferably as cosurfactant under the lower content of about 6% weight content from about 0.5%.More preferably the cationic surfactant of type is selected from alkyl trimethyl ammonium chloride (alkyl trimonium chloride) and dimethyl sulfate, dialkyl dimethyl ammonium chloride and Methylsulfate, zephiran (alkyl alkonium chloride) and Methylsulfate and composition thereof.Each alkyl chain of these surfactants contains C12 to C24 carbon atom.Most preferred cation is selected from stearyl dimethyl benzyl ammonium chloride, stearyl trimethyl ammonium chloride, VARISOFT TA100 and composition thereof.Cationic surfactant also can be used as the lipidosis auxiliary agent.
Except the foam synthetic surfactant, liquid emulsion compositions herein also can not necessarily contain the fatty acid soaps of C8-C14, and wherein the equilibrium ion of soap is selected from K and N (CH
2CH
2OH)
3And composition thereof.In an embodiment preferred of the present invention, liquid personal cleaning compositions contains and is less than approximately 5%, preferably is less than approximately 4%, more preferably is less than approximately 3%, most preferably is less than the fatty acid soaps of about 2% composition weight.
D. water
Contain water as basis in the individual humidification Cleasing compositions of the present invention.Water usually content is from about 30% to about 80%, preferably from about 40% to about 75%, and from about 40% to about 65% personal cleaning compositions of the present invention most preferably.
E. nonessential composition
Personal cleaning compositions of the present invention also can contain some nonessential compositions.
For example, liquid personal cleaning compositions of the present invention can not necessarily comprise the polymer of the formation gel of aqueous dispersion.This polymer is preferably anion, nonionic, cation or hydrophobically modified polymers, it is 1 that this polymer is selected from molecular weight, 000 to 3,000, the cationic polysaccharide of 000 cationic guar gum class, derive from anion, cation and the nonionic homopolymer of acrylic acid and/or methacrylic acid, anion, cation and non-ionic cellulose resin; Dimethyl dialkyl ammonium chloride and acrylic acid cation copolymer, the cationic homopolymer of dimethyl dialkyl ammonium chloride, cation polyalkylene and ethyoxyl polyalkyleneimine, molecular weight from 100,000 to 4,000, Polyethylene Glycol of 000 and composition thereof.Preferably, polymer be selected from sodium polyacrylate, hydroxyethyl-cellulose, cetyl hydroxyethyl cellulose and season hydroxyethyl-cellulose 10.
The content of this polymer in compositions of the present invention is preferably from about 0.1% to 1%, and more preferably 0.1% to 0.5%.This polymer can improve the sensory feel of lipid on skin except product stability is provided.The sensory feel of improvement comes from viscosity and butyrous minimizing and soft and smooth increase.Particularly preferred embodiment is for using mixture of polymers, and some of them are preferred to product stability, and some are to improving sensory feel for preferred.Being used to improve the preferred polymer of sensory feel is selected from: Polyethylene Glycol, hydroxypropyl melon ear, Rhaball Gum CG-M 8M, polyquaternary ammonium salt 3,5,6,7,10,11 and 24 and composition thereof.
Another nonessential composition very preferably of the present invention is one or more wetting agents and solute.Can use multiple wetting agent and solute and its content can be from about 0.5% to about 25%, more preferably from about 3.0% to about 20%.Wetting agent and solute are that nonvolatile dissolubility in 10% aqueous solution is at least 5% Organic Ingredients.Preferred water miscible Organic Ingredients is selected from has structural formula:
R1-O (CH
2-CR
2HO)
nThe polyhydric alcohol of H, wherein R1=H, C1-C4 alkyl; R2=H, CH
3And n=1-200; The alkanediol of C2-C10; Guanidine; Glycol acid and glycol hydrochlorate (as ammonium salt and alkyl quaternary ammonium salts); Lactic acid and lactate (as ammonium salt and alkyl quaternary ammonium salts); Poly-hydroxyl alcohol is as Sorbitol, glycerol, hexanetriol, propylene glycol, hexanediol or the like; Polyethylene Glycol; Sugar and starch; Sugar and starch derivant (as alkoxylate glucose); Pantothenylol (comprising D-, L-and D, the L-type); The 2-pyrrolidone-5-carboxylic acid; Hyaluronic acid; The lactamide monoethanolamine; The acetamide monoethanolamine; Carbamide; Has general structure (HOCH
2CH
2)
xNH
yEthanolamine, x=1-3 wherein; Y=0-2, and x+y=3, and composition thereof.Most preferred polyhydric alcohol is selected from glycerol, polyoxypropylene (1) glycerol and polyoxypropylene (3) glycerol, Sorbitol, butanediol, propylene glycol, sucrose, carbamide and triethanolamine.
Preferred water solublity Organic Ingredients is selected from glycerol, polyoxypropylene (1) glycerol and polyoxypropylene (3) glycerol, Sorbitol, butanediol, propylene glycol, sucrose, carbamide and triethanolamine.
The use of oiliness thickening polymer is listed among EP 0 547897 A2 as the Hewitt that announces on June 23rd, 93, is incorporated herein by reference, and also can be included in the aqueous phase of emulsion of the present invention.
Can comprise a large amount of supplementary elements in the compositions of the present invention.These raw materials comprise, but be not limited to, liquid appearance auxiliary agent, salt and hydrate thereof and the United States Patent (USP) 5 of authorizing people such as Kacher on August 23rd, 1994,340,492 and the United States Patent (USP) 4 of authorizing people such as Deckner April 24 nineteen ninety, other that list in 919,934 " packing material " is incorporated herein by reference.
The nonrestrictive example of other of these supplementary elements comprises vitamin and its derivant (as ascorbic acid, vitamin E, Tocopherol acetate ester or the like); Sunscreen; Thickening agent (as the polyhydric alcohol alkoxy ester, for the Crothix of the content height to 2% that derives from Croda and content high) to about 2% HANSHENGJIAO; In order to keep the antiseptic of the antibiotic integrity of compositions; Anti-acne medicament (resorcinol, salicylic acid or the like); Antioxidant; Comfortable and consolidant of skin such as Aloe vulgaris extractum, allantoin or the like; Chelating agen and sequestering agent; Be suitable for the reagent of sensory effects such as fragrance, quintessence oil, dermal sensation agent (skin sensate), pigment, pearling agent (as Muscovitum and titanium dioxide), in order to the additive (as fumed silica) that produces lax rinse feel, strengthen sedimentary additive (as the maleic acid soybean oil of content height to 3%), color lake, coloring agent or the like (as cloves oil, menthol, Camphora, eucalyptus oil and acetaminol).
II. the preparation method of liquid personal cleaning compositions of the present invention
In order to prepare liquid personal cleansing composition of the present invention, prepare the lipophilic skin humidizer of sealing as previously mentioned.Then the lipophilic skin humidizer of sealing is sneaked into personal cleanliness's substrate, contain foaming surface active agent, stabilizing agent, water and any nonessential composition in the substrate.When the lipophilic skin humidizer of sealing was sneaked in personal cleanliness's substrate, the stress intensity that applies on it should make that at least about 10% heavy encapsulated particles be non-sphere.Prepare the liquid personal cleansing substrate of having added the lipophilic skin humidizer of sealing according to traditional method for preparing liquid personal cleansing composition.III. the performance of liquid personal cleansing composition of the present invention
In order to obtain described deposition effect and to be accepted by consumer, importantly, liquid personal cleansing composition of the present invention has certain rheological characteristic.Especially, the viscosity of liquid personal cleansing composition of the present invention is about 2,000 to about 100,000 centipoise, preferred about 5,000 to about 70,000 centipoises, and more preferably from about 10,000 to about 40,000 centipoise, this value are measured by the viscosity method of following analysis method part and its yield point is about 5 to about 90 dynes/cm, preferred about 7 to about 50 dynes/cm, more preferably from about 9 to about 40 dynes/cm, and most preferably from about 11 to about 30 dynes/cm, and this value is measured by the yield point method of following analysis method part.
Liquid personal cleansing composition of the present invention provides clinical effective humidification effect to skin.Think deposition that this obviously increases owing to the lipophilic skin humidizer, lipophilic skin humidizer wherein is made up of big drop, this be with by the lipophilic skin humidizer of forming than droplet Comparatively speaking.The deposition value of liquid personal cleansing composition of the present invention is at least about 10 microgram/square centimeters, and preferably at least about 20 microgram/square centimeters, more preferably at least about 30 microgram/square centimeters, this value is to be measured by the deposition process of the part of analytical method hereinafter.Analytical method
Carry out quantitative assay by concrete experiment analytical method to being used for representing some parameters of key element of the present invention.These methods specifically describe as follows:
1. the denseness of lipophilic skin humidizer (k) and shear index (n)
Use the shearing index n and the denseness k of the lipophilic skin humidizer that Carrimed CSL100 proof stress rheometer measurement adopts herein here.Measure with 4 centimetres 2 ° the cone measuring system that generally is set at 51 microns gaps down at 35 ℃, mensuration is to be undertaken by shear stress application program (usually from about 0.06 dynes/cm to about 5,000 dynes/cm) in time.If the damage of this stress guide test sample, how much strains of promptly measuring are at least 10-4 rad/second, and this strain rate will be registered as shear rate.These data are used to make the flow curve of the viscosity, mu of material to shear rate γ '.Then this flow curve modelling to be provided at the mathematic(al) representation of describing the behavior of material in certain shear stress and the range of shear rate.The exponential model (for example seeing: the Chemical Engineering of Coulson and Richardson, Pergamon, nineteen eighty-two or Bird, the transport phenomenon of Stewart and Lightfoot, Wiley, nineteen sixty) of these results and following fine acceptance conforms to:
Viscosity, μ=k (γ ')
N-1
2. the viscosity of liquid personal cleaning compositions
Measure the viscosity of liquid personal cleaning compositions herein with Wells-Brookfield awl/board-like DV-II+ viscosity apparatus.Measure 25 ℃ of 2.4 centimetres ° cone (Spindle CP-41) measuring systems that have 0.013 millimeter gap between down with two little pins on each cone and the plate.By measuring injecting 0.5 milliliter sample to be analyzed between cone and plate and cone is rotated under the speed of 1 revolutions per.The resistance that rotates has produced and the proportional torque of the shear stress of liquor sample.Read torque value and on the basis of cone geometric constant, slewing rate and the torque relevant, calculate and be converted into absolute centipoise unit (milli handkerchief * second) by viscometer with stress.
3. the deposition of lipophilic skin humidizer
A. preparation method
Clean arm to reduce ambient interferences, suck dry moisture then as much as possible with the product that does not contain soap and lipid.Use about 5 seconds of whole surface of interior forearm of the tap water humidification tester of 95-100F then.Then as Campagnoli described in the United States Patent (USP) 5144744 (1992 on JIUYUE 8, authorize), the tester is saturated with powder puff, and allows 10 seconds of powder puff draining.The 1 milliliters of liquid personal cleaning compositions that will contain the lipophilic skin humidizer puts on tester's the forearm, with powder puff product is rubbed 10 seconds to bubble then.Allow foam continue 15 seconds at forearm, then water from interior elbow to wrist cleaning down 15 seconds.Pat dry forearm with napkin, allow air-dry about 30 seconds of forearm.
B. sedimentary record-sebum meter
The deposition of lipophilic skin humidizer adopts the sebum meter SM810 of Courage and Khazaka GmbH to measure.Sebum instrumentation amount has been deposited on the amount of the lipophilic skin humidizer on the skin, by the photometry of specific plastic zone, and this band bleach when absorbing the lipophilic skin humidizer.Plastic zone stretches on the minute surface that is connected on the spring.The measuring head (being made up of spring, mirror and plastic zone) of device is pressed in skin last 30 second.Deposition value (microgram/square centimeter) is the sign of lipophilic skin humidification dosage on the skin; The deposition value increases along with the increase of lipophilic skin humidification dosage.This method is insensitive to humidity.Along the length bark fetching fat meter reading (3 times) of forearm, the deposition value is the meansigma methods of 3 readings, divided by conversion factor so that sebum meter reading converts actual deposition level (microgram/square centimeter) to.
Sebum is in respect of following restriction:
1. sebum meter band is also measured the sebum of nature.The standard of this test is that the test body reference value that the sebum instrumentation gets before cleaning is less than or equal to 3 micrograms/square centimeter skin of forearm.
2. measure as drawing on other surface, the sebum meter can not record all sedimentary lipophilic skin humidizers; If skin shape is concavo-convex, may do not absorbed by sedimentary lipophilic skin humidizer by sebum meter band.
3. in the deposition value during greater than about 300 micrograms/square centimeter, sebum meter band is saturated; So this method only can be tested the value that is no more than about 300 microgram/square centimeters.
4. different lipophilic skin humidizers have different conversion factors.For the non-vaseline lipid of test, need new calibration curve.
C. calibration
For the sebum counting certificate with above-mentioned acquisition converts the deposition data to, must produce a conversion factor.In order to produce this conversion factor, every kind of lipid system is drawn, with the sample of gas chromatographic analysis absorption.Draw with sebum meter reading and carry out simultaneously, and take from identical forearm.The absorption program is as follows:
1) glass column (2 inch diameter) with opening places tester's interior forearm, and fixes.
2) Xiang Zhuzhong adds 5 milliliters of absorption solvents.
3) with round end glass stirring rod liquid was stirred 30 seconds on tester's arm.The whole surface of the forearm that comprises with solvent processing.
4) with disposable pipet liquid is gone in the 6 dram bottles.
Twice of 5 repeating step 2-5 (amount to 3 samples, collected 15 milliliters of solvents).
The sample of using the following analysis of gas chromatogram to draw then.The equipment gas chromatogram is equipped with the HP of capillary inlet system and flame ionic detector
5890 and instrument integration system PEN Turbochrom V4.0 data system of equal value, or
HP3396 series II integrator, or have the peak grouping
The similar system of ability.Post DB-5ht, 30M * 0.32mmI.D.,
0.10 μ m thickness, J﹠amp; W Scentific catalog number (Cat.No.) 123-
5731。Analytical balance can claim to 0.0001g.Pipet 1ml, the A level.Volumetric flask 1000ml, 100ml, glass stopper.The automatic probe tube of glass syringe 100 μ l capacity has the cap type bottle air bath of crooked top and transfers to 80-85 ℃ of pipet reason device and have the Ependorf Repeator agitator disk of 12.5ml storage tank and the stirring rod reagent heptane ACS level squalane Aldrich catalog number (Cat.No.) 23 that stirring rod Teflin coats, 431-1 or the analog lipid reference material ultra-pure helium of GC conditions carrier gas or with the routine of main and oxygen scrubber purification
The level helium.Exist with 25ml/min shunting regulated fluid pressure
25psi。Annotating the original mold formula does not have 100 ℃ of beginnings of branch multiple abscess sample volume 310 ℃ of furnace temperature patterns of 2 μ l injector temperature, 10℃/min rises to 350 ℃, kept 6 fens
Clock.350 ℃ of hydrogen of detector temperature and air optimization are suitable for the analytical balance weighing in the 100ml of clean dried volumetric flask of the used gas chromatogram fluid pack factor 2 solution inner mark solutions
0.1g squalane claims to 0.0002g.Be diluted to appearance with heptane
Long-pending, jump a queue and stirring and dissolving.(dilution in 1: 1000 of this solution
Liquid can be used as to be drawn solvent and produces sample) the lipid liquid storage puts into analytical balance and claims in the 100ml of clean dried volumetric flask
The 0.5g lipid reference material of amount claims to 0.0002g.Use heptan
Alkane is diluted to volume, jumps a queue and stirs mixed.3 automatic sampling phials of the following labeling of lipid work: " 100 μ g ", titer " 300 μ g " and " 500 μ g ".Use glass syringe, will
15 μ l inner mark solutions move in each phial.Dash with heptane
Wash syringe, the lipid liquid storage that pipettes following amount with it extremely then
Phial:
Titer liquid storage volume (μ l)
100μg 20
300μg 60
500μg 100
Be diluted to about 0.5ml with heptane, add upper cover then and shake up operation 1. calibrations and move each standard under these conditions.From correcting travel, select
Get 10-14 maximum peak and peak grouping in calibration steps.Will
The lipid amount belongs to the group of each calibrated horizontal in the standard solution. exists
Y axle subscript goes out the area ratio.Do not allow line cross initial point or comprise initial point.
The r2 value should be at least 0.9990.Per 10 or 12 samples and
When the sample end of run, detect calibration.2. sample analysis is being done evaporate to dryness sample under the nitrogen current.Rehydration in the 0.5ml heptane.
Lid is tight and placed air bath 5 minutes; Shake to molten fully
Separate.Move to automatic sampling phial and on calibration instrument, use suitable
Addition analysis as ISTD.Attention: because baseline is mixed, for
Correct identification peak, answer each result of manual detection.
Data from gas chromatography and sebum counting are according to carrying out curve tracing.Slope of a curve is a conversion factor.Conversion factor is 0.56 for vaseline.
4. the filtration weight of polycation
The filtration weight of polycation is measured with the filter plant that leaches the polycation coacervate effectively by having mechanical aspirator.
Polycation by mixed dissolution and dissolved sodium hexameta phosphate are (from the Glass H-P of FMC Corp.
2O
5Average chain length is 21) the formation complex coacervate.The total amount of blended polycation and hexametaphosphate is 12 grams.The polycation of using to the ratio of hexametaphosphate under this ratio, can form sedimentary ratio.When polycation was gelatin, the gelatin of application was 11: 1 (as 11 gram gelatin and 1 a gram hexametaphosphate) to the ratio of hexametaphosphate.
After calculating the suitable amount of polycation to be mixed and hexametaphosphate as mentioned above, in heating with stir a following polycation and hexametaphosphate is dissolved in the deionized water.The total amount that is used to dissolve the water of polycation and hexametaphosphate is 286 grams.Hexametaphosphate is dissolved in the water of 19 times of weight.Polycation is dissolved in remaining water.
After polycation and hexametaphosphate dissolve respectively, two solution are mixed.When polycation is gelatin, under agitation drips glacial acetic acid and regulate pH value to 3.7.Final mixture is cooled to polycation/hexametaphosphate/water complex coacervate that room temperature is separated with generation, and this coacervate can be filtered and weigh.By the device of forming by No. 0 filter paper of Whatman class 4 of the mesopore/middle flow velocity of 1000 milliliters conical flask, 100 millimeters Buchner buchner funnel and 90 millimeters complex coacervate is filtered out from solution.Gast vacuum pump by 1/6 horsepower provides mechanical aspirator.Complex coacervate after filtering is weighed and with the filtration weight of gram record weight as polycation.
5. lipophilic skin humidizer particle grain size distribution
Estimate lipophilic skin humidizer particle grain size distribution by the commercial scanned-laser microscope of producing by Lasentec (Lasentec M100F).It is to measure by cross the granule that floats on a liquid and move through probe window with the scanning focused laser post of a constant speed that Lasentec M100F measures particle.When focus and granule intersected, some light are scattered to be got back to probe and is converted into electronic impulse, and this pulse can be passed through correlation: d=v*t is converted into particle diameter.The persistent period of pulse is represented the time (t) that granule is illuminated at the focus place.Because (v) be known, (d) be exactly that particulate distance is crossed in scanning to the speed at focus place.This is apart from the particulate chord length of expression.Chord length distribution is directly measuring accurately grain structure size and grain structure shape on three-dimensional basis.M100 is divided into 38 sections to granule for from 1.9 to 1000 microns.Calculate particle size distribution with a cube length weight average chord length, this calculating provides the estimation (each size particles number relatively) of the amount of substance of each particle diameter:
n
i=at each other measuring section counting
M
iThe mid point of=respective section
The section # (2≤K≤38) that k=is higher
Lasentec each material in the formula range that comprises precipitation and bubble has all been measured particle size distribution.Therefore, use up the data of micro-lipophilic skin humidizer grain diameter measurement technology as a supplement to confirm to obtain by Lasentec M100F.In this technology, observe product with the very low amplification (＜10 times) between base plate and cover slip, estimate the particle diameter of lipophilic skin humidizer by micrometer.
6. the yield point of liquid personal cleaning compositions
Yield point with Carrimed CSL100 proof stress rheometer measurement liquid personal cleaning compositions.Be purpose herein, yield point is to produce 1% the required stress of strain in liquid personal cleaning compositions.Measure with 4 centimetres 2 ° the cone measuring system that is set at 51 microns gaps down at 77 °F.Mensuration is to be undertaken by shear stress application program (usually from about 0.06 dynes/cm to about 500 dynes/cm) in time.If the damage of this stress guide test sample can be made shear stress to strained curve.From this curve, can calculate the yield point of liquid personal cleaning compositions.
7. the intensity of complex coacervate
A. preparation
By being mixed into, the polycation of proper formula amount and polyanion form complex coacervate in the aqueous solution.When polycation is gelatin, regulate pH value to 3.5 to 4.5 scope by dripping glacial acetic acid.Final mixture is cooled off the coacervate that is separated with generation.Pour out supernatant, abundant complex coacervate is transferred to accompanied for formula culture dish (100 * 15 millimeters) to be full of culture dish fully and to form a plane at the top of culture dish.Make sample balance 24 hours at room temperature then.
B. intensity record
Measure the intensity of complex coacervate with stablizing micro-system general TA.XT2 structural analysis instrument and XT.RA sized data acquisition system.The structural analysis instrument uses the compression stress in cylindrical probe (14 * 11.5 millimeters) the mensuration complex coacervate.Probe is set in the 2mm at complex coacervate sample top.Probe pushes to produce the triggering power of 5 grams under the speed of 1 mm/second.Under the population and muzzle velocity of 1 mm/second, compress 4 mm distance subsequently.Data collecting system record required compression stress in time.Maximum compression stress is recorded as the intensity of complex coacervate.
8. measure the aspherical particle percentage rate
Adopt three-dimensional binocular (Zeiss SV8) to measure aspherical particle percentage rate in the finished product.Generally, from amplifying 9.5 to 24 times finished product is made a video recording.From figure, count aspherical particle (as defined above) number.The aspherical particle number has been obtained the aspherical particle percentage rate divided by the total particle number.
The specific embodiment
Embodiment
The bath gel combination of below listing is the non-restrictive example of liquid personal cleaning compositions of the present invention.The granule premix composition that composition #1 #2 #3 #4 seals:A type gelatin; Bloom strength 150 2.21 0.0 0.0 0.0A type gelatin; Bloom strength 100 0.0 2.21 0.0 0.0A type gelatin; An amount of foam (final volume) the 450 450 390 550 deposition values of vaseline particle (coming from pre-composition) 23.57 23.57 16.4 11.0 water that an amount of end formulation Texapon Special 2.14 2.14 2.89 4.3 lauryl ether 3-ammonium sulfate 6.42 6.42 8.66 6.5 lauryl both sexes sodium acetates 3.67 3.67 4.95 4.7 fatty acid soaps 0.0 0.0 0.0 0.0 laurate 1.4 1.4 1.4 1.4 trihydroxy glycerol stearates 0.38 0.38 0.75 0.4 nonessential component 4.53 4.53 4.39 5.0 that adds filtering particle of bloom strength 275 0.0 0.0 2.21 1.98 6 segregation phosphate 0.20 0.20 0.20 0.18 vaseline, 40.16 40.16 40.16 35.42 glacial acetic acid (dropping to pH＜4.4)～0.08～0.08～0.08～0.08 deionized waters (most excessive) is sealed (microgram/centimetre2) 69 43 46 40 particle diameters (granule of at least 50% weight) (micron)＞500＞500＞500＞600 viscosity (centipoise) 13,760-20,100 24,770pH 5.5-6.5 5.5-6.5 5.5-6.5 5.5-6.5 yield point (dynes per centimeter
2) preparation of 10-14 18 granule pre-compositions of sealing: 1. under agitation six inclined to one side Quadrafos are dissolved in 19 times the water.2. in remaining water, dissolve gelatin, and be heated to 50-60 ℃ under in agitator tank, stirring.3. heating oleophylic humidizer is to 50-60 ℃.4. at 50-60 ℃ of oleophylic humidizer that in 50-60 ℃ aqueous gelatin solution, adds heat.5. regulate mixing speed to obtain required particle diameter.6. in gelatin-water-oleophylic humidizer dispersion, add the Quadrafos aqueous solution.7. drip glacial acetic acid to pH be 3.8 to 5.0.8. cooling particulate mixture under agitation before the granule of sealing is added to liquid personal cleansing substrate.In personal cleanliness's substrate, add the granule of sealing
The Kenics static mixer that has 12 elements with 1.5 inches of diameters is sneaked into the lipophilic skin humidizer granule of sealing in personal cleanliness's substrate.Regulate flow velocity until producing required aspherical particle percentage rate (very depending on rheological property).
Claims (30)
1. liquid personal cleansing composition, it comprises:
A) humidification phase comprises the lipophilic skin humidizer of sealing of composition weight 1% to 35%; Wherein the lipophilic skin humidizer is encapsulated in the complex coacervate, this coacervate comprises minimum polycation and the polyanion that filters weight 10 grams, the hardness of wherein said complex coacervate is 50 to 1400 gram forces, wherein the agent of lipid skin moisturizing constitutes the drop of certain grain size distribution, and the diameter that makes at least 10% heavy drop is greater than 100 microns; With
B) water comprises:
I) 0.1% of composition weight to 10% stabilizing agent;
Ii) 5% of composition weight to 30% foaming surface active agent; With
Iii) water, wherein stabilizing agent is the stabilizing agent of crystalline hydroxyl, is selected from:
Wherein
R1 is
R2 is R1 or H
R3 is R1 or H
R4 is C
0-20Alkyl
R5 is C
0-20Alkyl
R6 is C
0-20Alkyl
R4+R5+R6＝C
10-22
And 1≤x+y≤4 wherein;
(ii)
Wherein
R7 is-R4 (CHOH) xR5 (CHOH) yR6
M is Na+, K+ or Mg++ or H; And
(iii) its mixture.
2. according to the liquid personal cleansing composition of claim 1, its deposition value at least 10 microgram/square centimeters.
3. according to the liquid personal cleansing composition of claim 2, wherein at least 10% heavy lipophilic skin humidizer granule of sealing is non-sphere in the finished product.
4. according to the liquid personal cleansing composition of claim 3, wherein complex coacervate comprises 0.1% to 15% polycation and 0.01% to 10% polyanion.
5. according to the liquid personal cleansing composition of claim 4, wherein the ratio of polycation and polyanion is 30: 1 to 1: 5 in the complex coacervate.
6. according to the liquid personal cleansing composition of claim 5, wherein personal cleaning compositions contains 1% to 30% lipophilic skin humidizer.
7. according to the liquid personal cleansing composition of claim 6, wherein the denseness of lipophilic skin humidizer is 5 to 5,000 pools, and shearing index is 0.1 to 0.9.
8. according to the liquid personal cleansing composition of claim 7, wherein polycation comprises gelatin.
9. liquid personal cleansing composition according to Claim 8, wherein polyanion is selected from Quadrafos, arabic gum, sodium alginate and composition thereof.
10. according to the liquid personal cleansing composition of claim 9, wherein the size of at least 50% heavy drop that comprises the lipophilic skin humidizer is greater than 100 microns.
11. according to the liquid personal cleansing composition of claim 1, wherein the viscosity of liquid personal cleansing composition is 2,000 to 100,000 centipoises, wherein the deposition value of liquid personal cleansing composition is at least 30 microgram/square centimeters.
12. according to the liquid personal cleansing composition of claim 11, at least 50% the particulate size that wherein comprises the lipophilic skin humidizer is greater than 200 microns.
13. a liquid personal cleansing composition, it comprises:
A) humidification phase comprises the lipophilic skin humidizer of sealing of composition weight 1% to 35%; Wherein the lipophilic skin humidizer is encapsulated in the complex coacervate, this coacervate comprises minimum polycation and the polyanion that filters weight 10 grams, wherein the agent of lipid skin moisturizing constitutes the drop of certain grain size distribution, and promptly the diameter of at least 10% heavy drop is greater than 100 microns; The essentially no cross-linking agent of wherein sealing of lipophilic skin humidizer; With
B) water comprises:
I) 0.1% of composition weight to 10% stabilizing agent;
Ii) 5% of composition weight to 30% foaming surface active agent; With
Iii) water, wherein stabilizing agent is the stabilizing agent of crystalline hydroxyl, is selected from:
Wherein
R1 is
R2 is R1 or H
R3 is R1 or H
R4 is C
0-20Alkyl
R5 is C
0-20Alkyl
R6 is C
0-20Alkyl
R4+R5+R6＝C
10-22
And 1≤x+y≤4 wherein;
(ii)
Wherein
R7 is-R4 (CHOH) xR5 (CHOH) yR6
M is Na+, K+ or Mg++ or H; And
(iii) its mixture.
14. according to the liquid personal cleansing composition of claim 13, wherein the deposition value is at least 10 microgram/square centimeters.
15. according to the liquid personal cleansing composition of claim 14, wherein at least 30% heavy lipophilic skin humidizer granule of sealing is non-sphere in the final products.
16. according to the liquid personal cleansing composition of claim 15, wherein complex coacervate comprises 0.1% to 15% polycation and 0.01% to 10% polyanion.
17. according to the liquid personal cleansing composition of claim 16, wherein the ratio of polycation and polyanion is 30: 1 to 1: 5 in the complex coacervate.
18. according to the liquid personal cleansing composition of claim 17, wherein personal cleaning compositions contains 1% to 30% lipophilic skin humidizer.
19. according to the liquid personal cleansing composition of claim 18, wherein the denseness of lipophilic skin humidizer is 5 to 5,000 pools, shearing index is 0.1 to 0.9.
20. according to the liquid personal cleansing composition of claim 19, wherein polycation comprises gelatin.
21. according to the liquid personal cleansing composition of claim 20, wherein polyanion is selected from Quadrafos, arabic gum, sodium alginate and composition thereof.
22. according to the liquid personal cleansing composition of claim 21, wherein the size of at least 50% heavy drop that comprises the lipophilic skin humidizer is greater than 100 microns.
23. according to the liquid personal cleansing composition of claim 13, wherein the viscosity of liquid personal cleansing composition is 2,000 to 100,000 centipoises, wherein the deposition value of liquid personal cleansing composition is at least 30 microgram/square centimeters.
24. according to the liquid personal cleansing composition of claim 23, at least 50% the particulate size that wherein comprises the lipophilic skin humidizer is greater than 200 microns.
25. a liquid personal cleansing composition, it comprises:
A) 0.1% to 5% polycation;
B) 0.01% to 1% polyanion;
C) 0.75% to 30% denseness is 5 to 5,000 pools, and shearing index is 0.1 to 0.9
The lipophilic skin humidizer of pool, wherein the particle size distribution of lipophilic skin humidizer is at least
The diameter of 10% heavy drop is greater than 100 microns;
D) 0.1% to 10% stabilizing agent;
E) 5% to 30% foaming surface active agent; With
F) water;
Wherein the viscosity of personal cleaning compositions is 2,000 to 100,000 centipoises; Wherein poly-sun from
Son is 30: 1 to 1: 5 with the ratio of polyanion; Liquid personal cleansing composition base wherein
Cross-linking agent-free on the basis, wherein stabilizing agent is the stabilizing agent of crystalline hydroxyl, is selected from:
(i)
Wherein
R1 is
R2 is R1 or H
R3 is R1 or H
R4 is C
0-20Alkyl
R5 is C
0-20Alkyl
R6 is C
0-20Alkyl
R4+R5+R6＝C
10-22
And 1≤x+y≤4 wherein;
(ii)
Wherein
R7 is-R4 (CHOH) xR5 (CHOH) yR6
M is Na+, K+ or Mg++ or H; And
(iii) its mixture.
26. according to the liquid personal cleansing composition of claim 25, wherein the deposition value is greater than 20 microgram/square centimeters.
27. according to the liquid personal cleansing composition of claim 26, wherein polycation comprises gelatin.
28. according to the liquid personal cleansing composition of claim 27, wherein polyanion is selected from Quadrafos, arabic gum, sodium alginate and composition thereof.
29. according to the liquid personal cleansing composition of claim 28, wherein the size of at least 50% heavy drop that comprises the lipophilic skin humidizer is greater than 100 microns.
30. according to the liquid personal cleansing composition of claim 25, wherein the size of at least 50% heavy drop that comprises the lipophilic skin humidizer is at least 200 microns.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US08/717,521 | 1996-09-23 | ||
| US08/710,833 US5716920A (en) | 1996-09-23 | 1996-09-23 | Method for preparing moisturizing liquid personal cleansing compostions |
| US08/717,521 US5932528A (en) | 1996-09-23 | 1996-09-23 | Liquid personal cleansing compositions which contain an encapsulated lipophilic skin moisturizing agent comprised of relatively large droplets |
| US08/710,833 | 1996-09-23 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1237900A CN1237900A (en) | 1999-12-08 |
| CN1123336C true CN1123336C (en) | 2003-10-08 |
Family
ID=27108535
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97199040A Expired - Fee Related CN1123336C (en) | 1996-09-23 | 1997-09-22 | Liquid personal cleansing compositions which contain encapsulated lipophilic skin moisturizing agent comprised of relatively large droplets |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP0929291A1 (en) |
| CN (1) | CN1123336C (en) |
| WO (1) | WO1998011870A1 (en) |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1149149B1 (en) | 1999-02-02 | 2002-11-13 | Quest International B.V. | Detergent composition |
| MXPA03003739A (en) † | 2000-10-27 | 2003-07-28 | Procter & Gamble | Stabilized liquid compositions. |
| CA2435735C (en) * | 2002-07-31 | 2008-10-14 | Rohm And Haas Company | Triggered response compositions |
| US7915214B2 (en) | 2006-01-12 | 2011-03-29 | Amcol International Corporation | Compositions containing benefit agent composites pre-emulsified using colloidal cationic particles |
| CN103120627A (en) * | 2012-12-14 | 2013-05-29 | 吴江市德佐日用化学品有限公司 | Healthcare hand sanitizer |
| US9540489B2 (en) | 2013-07-29 | 2017-01-10 | The Procter & Gamble Company | Blocky cationic organopolysiloxane |
| US9611362B2 (en) | 2013-07-29 | 2017-04-04 | The Procter & Gamble Company | Cationic organopolysiloxanes |
| US9701929B2 (en) | 2013-07-29 | 2017-07-11 | The Procter & Gamble Company | Consumer product compositions comprising organopolysiloxane emulsions |
| US10414873B2 (en) | 2013-07-29 | 2019-09-17 | The Procter & Gamble Company | Organopolysiloxane polymers |
| US9993418B2 (en) | 2013-07-29 | 2018-06-12 | The Procter & Gamble Company | Benefit agent emulsions and consumer products containing such emulsions |
| US9963470B2 (en) | 2013-07-29 | 2018-05-08 | The Procter & Gamble Company | Branched blocky cationic organopolysiloxane |
| US9580670B2 (en) | 2013-07-29 | 2017-02-28 | The Procter & Gamble Company | Consumer product compositions comprising organopolysiloxane conditioning polymers |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3697437A (en) * | 1970-05-27 | 1972-10-10 | Ncr Co | Encapsulation process by complex coacervation using inorganic polyphosphates and organic hydrophilic polymeric material |
| IT1079004B (en) * | 1976-05-11 | 1985-05-08 | Rubinstein Inc H | COMPOSITION OF WASHING AND CONDITIONING OF HAIR |
| US5089269A (en) * | 1987-11-07 | 1992-02-18 | Shiseido Company Ltd. | Cosmetic containing fine soft microcapsules |
| US5681801A (en) * | 1995-04-17 | 1997-10-28 | Colgate-Palmolive Company | Stable particle suspended composition |
-
1997
- 1997-09-22 CN CN97199040A patent/CN1123336C/en not_active Expired - Fee Related
- 1997-09-22 WO PCT/US1997/016714 patent/WO1998011870A1/en not_active Application Discontinuation
- 1997-09-22 EP EP97941711A patent/EP0929291A1/en not_active Ceased
Also Published As
| Publication number | Publication date |
|---|---|
| CN1237900A (en) | 1999-12-08 |
| WO1998011870A1 (en) | 1998-03-26 |
| EP0929291A1 (en) | 1999-07-21 |
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