CN1473193A - Reblending of detergent tablets - Google Patents
Reblending of detergent tablets Download PDFInfo
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- CN1473193A CN1473193A CNA018183697A CN01818369A CN1473193A CN 1473193 A CN1473193 A CN 1473193A CN A018183697 A CNA018183697 A CN A018183697A CN 01818369 A CN01818369 A CN 01818369A CN 1473193 A CN1473193 A CN 1473193A
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/02—Floating bodies of detergents or of soaps
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/38—Cationic compounds
- C11D1/65—Mixtures of anionic with cationic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/835—Mixtures of non-ionic with cationic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/86—Mixtures of anionic, cationic, and non-ionic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/88—Ampholytes; Electroneutral compounds
- C11D1/94—Mixtures with anionic, cationic or non-ionic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/0047—Detergents in the form of bars or tablets
- C11D17/0065—Solid detergents containing builders
- C11D17/0073—Tablets
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/0047—Detergents in the form of bars or tablets
- C11D17/0065—Solid detergents containing builders
- C11D17/0073—Tablets
- C11D17/0078—Multilayered tablets
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0052—Gas evolving or heat producing compositions
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/38—Cationic compounds
- C11D1/62—Quaternary ammonium compounds
Abstract
The present invention relates to a multi-phase detergent composition of compressed particulate matter, wherein the geometric mean particle diameter of one phase differs from the geometric mean particle diameter of at least one other phase by at least 300 mum. The phases of the compositions of the present invention are easy to separate and avoid excessive contamination which would cause problems for reblend operations. The present invention also relates to a method of separating the phases of a multi-phase detergent compositions of compressed particulate matter, wherein the geometric mean particle diameter of the first phase differs from the geometric mean particle diameter of the second phase by at least 300 mum, said method comprising the steps: a) breaking up the compressed composition into particles, and b) separating phases on the basis of their particle size.
Description
Technical field
The detergent tablet that the present invention relates to the decomposite method of tablet and be applicable to this method.
Background technology
The detergent tablet composition is known in the art, and known they compare with the detergent composition of particulate form and have several advantages, for example be easy to quantitatively, operation, transportation and storage.The human consumer especially likes the accessibility of shaped detergent composition, because they can be by distributing the ware dispensing.
Heterogeneous tablet has will be the basically incompatible composition of permission and is formulated in advantage in the same dosage device.Can design tablet makes incompatible composition keep physically separating and can discharging those compositions in turn.For example, it is desirable to prepare a kind of composition that comprises tensio-active agent and fabric softener of once used amount.Cause relatively poor cleaning power, relatively poor soft effect but many tensio-active agents commonly used can form title complex with fabric softener and residue may be arranged on fabric.Therefore, any composition that comprises this two classes material must use the compatible material of limited quantity to prepare or be designed to discharge described composition in turn, thereby avoids the non-compatibility problem.
Tablet is prepared as follows usually: be pre-mixed a kind of component of detergent composition, and use any suitable equipment, preferred tabletting machine is made a kind of tablet with the detergent component that has been pre-mixed.Heterogeneous tablet typically is prepared as follows: first kind of composition of compression in tabletting machine is the planar the first layer in fact to form.Then another kind of detergent composition is delivered in the tabletting machine and places on the first layer.Compress this second kind of composition then, be the planar second layer in fact to form another.
Any method all can produce the permission that do not meet of some amount their are loaded and transported the tablet of the quality standard of trade.For example, damaged tablet, inaesthetic tablet, tablet etc. with chemical substance of unacceptable content.For making cost drop to minimum and efficent use of resources, should reclaim underproof tablet.When tablet during, then can simply defective tablet be smashed to pieces and in its pre-composition of particulate matter add-back by even the composition.But, form and comprise the different phase times of differing materials when having two or more by the compressing grains material, it is comparatively complicated that the remix process becomes, because these must be separated and make they and its pre-composition remix separately mutually.
An object of the present invention is to provide a kind of multi-phase detergent composition of compressed microparticles material, said composition designs to such an extent that can improve and the relevant problem of this class tablet of remix.The present invention also provides a kind of method of separating each phase of multi-phase detergent tablet.
Summary of the invention
The present invention relates to a kind of multi-phase detergent composition of compressing grains material, wherein after smashing to pieces, the geometric mean particle diameter of a phase differs at least 300 microns with another geometric mean particle diameter mutually at least.So each is easy to separate mutually, therefore can avoid the excessive soil between each phase, this pollution will bring problem to the remix operation.
The invention still further relates to each phase disengagement method of a kind of multi-phase detergent composition of being made by the compressing grains material, wherein the geometric mean particle diameter of first phase differs at least 300 microns with second mutually the geometric mean particle diameter, and described method comprises the following steps:
(a) make the composition of compression cracked for particle and
(b) separate each phase according to its particle size.
Compressed microparticles material of the present invention can take various forms, and as particle, bead, strip, piller, and mixes.The preferred solid particulate of this particle, but also can be liquid or gel-filled bead.
Embodiment
Multi-phase detergent composition of the present invention is made by the particulate matter of compression, and wherein the geometric mean particle diameter of a phase differs at least 300 microns with another geometric mean particle diameter mutually at least.Preferred each geometric mean particle diameter between mutually differs at least 500 microns, and more preferably at least 750 microns, even more preferably at least 1000 microns, even also more preferably at least 1500 microns.
Used " geometric mean diameter " is meant the particle size determination technology based on quality by any standard among the present invention, preferably how much mass median diameters of a collection of discrete particle of measuring by dry screen.Suitable method for sieving meets ISO 3118 (1976).Suitable device is Ro-Tap testing sieve shaker Model B, uses the selected size of 8 inches sieves.
Detergent composition of the present invention can be any suitable shape, for example sexangle, square, rectangle, cylindrical, sphere etc.Preferred rectangle of composition of the present invention or square use in the distribution ware of automatic washing machine because this is convenient to them.
Of the present invention each can arrange in any suitable mode mutually.EP-A-055,100 have shown some suitable heterogeneous form.Detergent composition of the present invention preferably has two-phase.These are preferably arranged in the mode of layer mutually, are more preferably wherein and one insert mutually in the mould of another phase.If the present composition comprises more than two-phase, then preferred, but and non-essential be that wherein each geometric mean particle diameter mutually of the geometric mean particle diameter and all the other of each phase differs at least 300 microns.
The present invention especially can be used for the heterogeneous tablet made by compressed microparticles.Multi-phase detergent tablet typically is prepared as follows: first kind of composition of compression in tabletting machine, and to form first phase.Then another kind of composition is delivered in the tabletting machine and on first phase and compresses.Preferably use main component to be particulate form.Preferably with less than 10000 newton/square centimeters, more preferably no more than 3000 newton/square centimeters even more preferably no more than the force compresses tablet of 750 newton/square centimeters.In fact, the present invention more embodiment preferred be to use less than the power of 500 newton/square centimeters and compress.Usually, the present composition will use low relatively power to compress, so that its disintegration fast.Suitable sheeting equipment comprises that standard one-shot press or revolver gress (for example can be available from Courtoy
_, Korsch
_, Manesty
_Or Bonals
_) or WO-A-00/10800 described in those.Preferably compression preparation in the tabletting machine that can prepare the tablet that comprises a model of tablet.Heterogeneous tablet can use the known technology preparation.The preferred tabletting method (also being described as the annular punch of the built-in second core drift) of two punching press principles that uses may further comprise the steps:
I) reduce core drift and the core of tablet sent in the formed chamber mutually,
Ii) reduce whole drift and annular sent in the formed chamber mutually,
Iii) make the core drift be promoted to annular punch level (this step can be carried out) during annular is sent into mutually or during compression step.
Iv) facing to two drifts of compressed panel compression.This compression can increase a precompression step mutually.When this method finished, two drifts were in same level.
By punch systems being increased to the turret head level, tablet is deviate from from die cavity then.The order of this step can change according to desired net result.Tablet also can use two punch systems preparations (is lower punch, and is upper punch).
The another kind of preferred form of the present composition is the particulate matter that comprises with a kind of mould material, and this material often is called capsule.Term used herein " capsule " is meant a kind of sealed structure of being made by water-solubility membrane, wherein comprises the above particulate matter of two-phase or two-phase.Capsule can be any form, shape and the material that is suitable for preserving said composition, for example, capsule with do not allow composition substance from capsule to discharge before water contacts.Definite enforcement will be depended on following factor, as the quantity of compartment in the type and the quantity of composition in the capsule, the capsule, preserved, protect and send or discharged each mutually required characteristic by capsule.Preferably, make as a whole capsule and be stretched at the formation and/or the closed period of capsule, the capsule of gained is the part tensile at least like this.
Be used for preferably water soluble film of the present invention and comprise polymkeric substance, multipolymer or derivatives thereof, they are selected from polyvinyl alcohol, Polyvinylpyrolidone (PVP), polyalkylene oxide, acrylamide, vinylformic acid, Mierocrystalline cellulose, ether of cellulose, cellulose ester, cellulose amides, polyvinyl acetate, poly carboxylic acid and salt, polyamino acid or peptide, polymeric amide, polyacrylamide, toxilic acid/acrylic acid multipolymer, the polysaccharide that comprises starch and gelatin, natural gum, for example xanthan gum and carrageenin.More preferably polyvinyl alcohol, polyvinyl alcohol copolymer and Vltra tears (HPMC).Highly preferred water-solubility membrane is the film that comprises the PVA polymkeric substance and have similar performance with following commercially available film: the PT-75 that commodity M8630 that is sold by the Chris-Craft Industrial Products company of U.S.'s Indiana State's Gary and Japanese Aicello company sell.
The particulate material that is used to prepare the present composition can be by any granulating or prilling process preparation.The example of these class methods is spraying drying (in cocurrent flow or Countercurrent Spray Dryer), and spraying drying provides 600 grams per liters or lower bulk density usually.The particulate material of higher bulk density can make by continuous granulation and densifying method (as using Lodige
_CB and/or Lodige
_The KM stirrer).Other method that is fit to comprises bed process, debulking methods (as roll compaction), extrusion molding, and any particulate material that makes as flocculation, crystallization sentering etc. by any chemical process.
Each phase of the present invention can comprise any suitable material.The present invention is particularly useful when each comprises incompatible basically each other composition mutually or has the obvious characteristic of different human consumers such as smell or color, becomes important because this makes to be avoided during the remix polluting.
The material that typically is added in the detergent composition comprises, but be not limited to, tensio-active agent, fabric softener, spices, sequestrant, press down foam system, laking agent, polymeric dye transfer inhibitor, alleviate fabric abrasion polymkeric substance, subtract wrinkle agent, disintegration auxiliary agent, enzyme, SYNTHETIC OPTICAL WHITNER, washing assistant, and mix.These composition more detailed descriptions are as follows.
What preferably have big geometric mean particle diameter comprises one or more medicaments mutually, and this medicament is selected from fabric softener, spices, foam inhibition system, subtract wrinkle agent, sequestrant, laking agent, alleviate the polymkeric substance of fabric abrasion, and composition thereof.What more preferably have big geometric mean particle diameter comprises one or more medicaments mutually, and this medicament is selected from fabric softener, spices, foam inhibition system, and composition thereof.
The present composition preferably comprises tensio-active agent.Can use any suitable tensio-active agent.Preferred surfactants is selected from anion surfactant, amphoterics, zwitterionics, nonionogenic tenside (comprising semi-polar nonionogenic tenside), cats product, and composition thereof.The tensio-active agent gross weight that the present composition comprises preferably accounts for 0.5% to 75%, more preferably 1% to 50%, most preferably 5% to 30% of composition total weight.Detersive surfactant be known and have in the art abundant description (referring to, for example " tensio-active agent and washing composition " (Surface Active Agents andDetergents), Vol.I﹠amp; II, Schwartz, Perry and Beach).Some limiting examples that are applicable to tensio-active agent of the present invention are:
1. any basically nonionogenic tenside that can be used for the decontamination purpose all can be included in the detergent composition of the present invention.Preferably, the non-limiting kind of useful nonionogenic tenside comprises EO/PO and the condenses of propylene glycol, the EO of nonionic and the condensation product of propylene oxide/ethylenediamine adduct of nonionic ethoxylated alcohol surfactant, end capped alkyl alkoxylated surfactants, ether capped poly-(oxyalkylated) alcohols, nonionic ethoxylated/propoxylated fatty alcohol surfactant, nonionic.
In a preferred embodiment of the invention, detergent composition comprises a kind of blended nonionic surfactant system, and this system comprises at least a low cloud point non-ionic surfactants and at least a high cloud point non-ionic surfactants.
" cloud point " that the present invention uses is the known properties of nonionogenic tenside, promptly, temperature causes the surfactant dissolves variation along with raising, thereby can be observed second temperature that occurs mutually and be called " cloud point " (referring to Kirk Othmer ' s Encyclopedia of ChemicalTechnology, 3rd Ed.Vol.22, pp.360-379).
" low cloud point " nonionogenic tenside that the present invention uses be defined as cloud point be lower than 30 ℃, preferably be lower than 20 ℃, most preferably be lower than 10 ℃ nonionic surfactant system composition.
Low cloud point non-ionic surfactants comprises polyoxyethylene, polyoxypropylene block polymer in addition.Polyoxyethylene-the polyoxypropylene polymer of block comprise those based on ethylene glycol, propylene glycol, glycerine, TriMethylolPropane(TMP) and quadrol as initiator for reaction hydrogen compound person.Some of Huaian, the state of Michigan how special BASF-Wyandotte company are called PLURONIC
TM, REVERSED PLURONIC
TM, and TETRONIC
TMBlock polymer class surfactant compounds be suitable for ADD composition of the present invention.Preferred examples comprises REVERSED PLURONIC
TM25R2 and TETRONIC
TM702.This class tensio-active agent typically is used as low cloud point non-ionic surfactants among the present invention.
" high cloud point " nonionogenic tenside that the present invention uses be defined as cloud point be higher than 40 ℃, preferably be higher than 50 ℃, most preferably be higher than 60 ℃ nonionic surfactant system composition.
2. the anion surfactant that is useful on the decontamination purpose basically all is applicable to the present invention.These can comprise anionic property vitriol, sulfonate, carboxylate salt and sarcosinate (comprise, for example sodium salt, sylvite, ammonium salt and substituted ammonium salt is arranged as an alcohol salt, di-alcohol ammonium salt and tri ethanol ammonium salt).The preferred anionic sulfate surfactant.
Other anion surfactant comprises isethionate, as fatty acid amide compound, alkyl succinate and the sulfosuccinate of acyl-hydroxyethyl sulfonate, N-acyl taurine salt, methylamino esilate, the monoesters of sulfosuccinate (especially saturated and undersaturated C
12-C
18Monoesters), the diester of sulfosuccinate (especially saturated and undersaturated C
6-C
14Diester), N-acyl sarcosinate.Resinous acid and hydrogenated resin acid also are suitable, for example rosin, staybelite and be present in the butter or by butter deutero-resinous acid and hydrogenated resin acid.
Secondary alkyl sulfate surfactant also is applicable to the present invention.These comprise US-A-6, in 015,784 disclosed those.Preferred secondary alkyl sulfate surfactant is those materials that have along the sulfate radical part of molecule alkyl " main chain " random distribution.This class material can be described with following array structure:
CH
3(CH
2)
n(CHOSO
3 -M
+) (CH
2)
mCH
3M and n are 2 and greater than 2 integer in the formula, and the m+n sum typically is 9 to 17, and M is a water-soluble cationic.Be used for preferred secondary alkyl surfactants of the present invention and have following structural:
CH
3(CH
2)
x(CHOSO
3 -M
+) CH
3And
CH
3(CH
2)
y(CHOSO
3 -M
+) CH
2CH
3In the formula x and (y+1) be at least 6, be preferably 7 to 20,10 to 16 integer more preferably.M is a positively charged ion, as basic metal, ammonium, alkanol ammonium, alkaline-earth metal or analogue.Typically use sodium salt.The more details that are applicable to secondary alkyl surfactants of the present invention are described among the US-A-6015784.
3. be applicable to that amphoterics of the present invention comprises amine oxide tensio-active agent and alkyl both sexes carboxylic acid.
4. zwitterionics also can be incorporated in the detergent composition of the present invention.These tensio-active agents can broadly be described as the derivative of secondary amine and tertiary amines derived thing, heterocyclic secondary and tertiary amine or the derivative of quaternary ammonium, quaternary phosphonium or uncle's sulfonium compound.Betaine and sulfo group betaine surfactants are the examples that can be used for zwitterionics of the present invention.
Suitable betaine is the compound that meets following formula: R (R
1)
2N
+R
2COO
-, R is a C in the formula
6-C
18Alkyl, each R
1Typically be C
1-C
3Alkyl, and R
2Be a C
1-C
5Alkyl.Preferred betaine is caproic acid C
12-C
18Dimethyl Ammonium and C
10-C
18Amido propane (or ethane) dimethyl (or diethyl) betaine.The betaine surfactants that cooperates also is applicable to the present invention.
5. be used for the water dispersible compound that cationic ester tensio-active agent of the present invention preferably has surfactant properties, this compound comprises at least one ester (promptly-COO-) key and at least one cationic charge group.The cationic ester tensio-active agent that other is suitable comprises the cholinesterase tensio-active agent, for example has been disclosed among US-A-4228042, US-A-4239660 and the US-A-4260529.
Suitable cationic surfactants comprises and is selected from following quaternary ammonium surfactant: single C
6-C
16, preferred C
6-C
10N-alkyl or alkenyl ammonium surfactant, wherein remaining N position have methyl, hydroxyethyl or hydroxypropyl to replace.
Be used for preferred surfactants of the present invention and be selected from anion sulfoacid salt surfactant (especially linear alkylbenzene sulfonate), anion sulfate acid salt surfactant (C especially
12-C
18Alkyl-sulphate), secondary alkyl sulfate surfactant, nonionogenic tenside and composition thereof.
Being used for highly preferred medicament of the present invention is spices.In this context, term " spices " is meant any odoriferous material or any material as the stink counteractant.In general, this class material is characterised in that its vapour pressure is higher than normal atmosphere at ambient temperature.Being used for spices of the present invention or reodorant is liquid at ambient temperature mostly, but also can be known in the industry solid, as various camphors (Camphoraceous) spices.Many chemical substances are well-known owing to using as spices, comprise for example materials such as aldehydes, ketone, ester class and analogue thereof.The most frequently used, naturally occurring plant and animal oil and exudate comprise that the compounding mixture of various chemical compositions is also known to spices, and this class material can be used for the present invention.Spices among the present invention can be relatively simply on it is formed or also can be comprised the mixture of the height elaborate of natural or synthetic chemical components, and all these is selected so that the smell of any needs to be provided.
Perfume composition of the present invention can comprise former, the pure fragrance material of the spices, the spices that incapsulate, and composition thereof.
Normally solid spices also can be used for the present invention.These materials can be mixed together with liquefying agent such as solvent before in mixing particle, and perhaps fusion or mix simply is as long as spices can not distil or decompose when heating.
Spices also comprises the material that uses as the stink counteractant.These materials, though be also referred to as " spices " in the present invention, they self do not have recognizable smell, can cover or reduce any irritating smell.The example of suitable stink counteractant is disclosed in United States Patent (USP) 3,102, in 101.
It is former that perfume composition also can comprise spices.Spices is former to be to discharge the fragrance precursor of spices when for example moisture, pH, chemical reaction interact with outside stimulus.Be applicable to spices of the present invention former comprise known in the industry those.The visible US-A-4 of example, 145,184, US-A-4,209,417, US-A-4,545,705, US-A-4,152,272, US-A-5,139,687 and US-A-5,234,610.
The present composition preferably comprises 0.05% to 15%, preferred 0.1% to 10%, the perfume composition of 0.5% to 5% weight most preferably.
The preferred present composition comprises the disintegration auxiliary agent.The term " disintegration auxiliary agent " that the present invention uses is meant a kind of material of the matrix dispersive effect that has the acceleration present composition when contacting with water or the mixture of material.This can present following form: quicken the material of disintegration itself or composition can be prepared or substances processed in the mode of the disintegration of acceleration water itself.For example, suitable disintegration auxiliary agent comprises swollen clay (thereby matrix of destroying compositions) and Drug coating when contacting with water, this Drug coating allows to use lower pressure with the integrity that improves tablet (thereby make the compactness of tablet relatively poor, and easier dispersion) during processing.Can use any suitable disintegration auxiliary agent, but they are preferably selected from disintegrating agent, Drug coating, effervescent, binding agent, clay, highly soluble compound, binding property compound, and composition thereof.
1. composition of the present invention can comprise a kind of when contacting with water the swollen disintegrating agent.Be used for disintegrating agent of the present invention and comprise those that Handbook of Pharmaceutical Excipients (1986) describes.Suitable disintegrating agent example comprises clay, for example wilkinite; Starch: starch, the starch gluconic acid sodium salt of natural, modification or pre-gelatinization; Resin: agar, guar gum, tracasol, kuteera gum, pectin, tragacanth gum; The crosslinked sodium carboxymethylcellulose pyce that contracts, polyvinylpolypyrrolidone, Mierocrystalline cellulose, carboxymethyl cellulose, alginic acid and salt (comprising sodiun alginate) thereof, silicon-dioxide, polyvinylpyrrolidone, soybean polysaccharide, ion exchange resin, and mixture.
2. composition of the present invention can carry out dressing.Dressing is in the mechanical characteristics that keeps or improve the dissolved while can improve forming composition.This is applicable to multilayer tablet highly beneficially, thereby restricts by the machinery that uses dressing can alleviate heterogeneous processing, thereby improves the mechanical integrity of tablet.Be preferred for Drug coating of the present invention and method and be described in EP-A-846, in 754, the document is introduced the present invention for your guidance.As EP-A-846, described in 754, preferred Drug coating composition such as dicarboxylic acid.Especially the dicarboxylic acid of Shi Heing is selected from oxalic acid, propanedioic acid, succsinic acid, pentanedioic acid, hexanodioic acid, pimelic acid, suberic acid, nonane diacid, sebacic acid, undecane diacid, dodecanedioic acid, undecane dicarboxylic acid and composition thereof.Hexanodioic acid most preferably.Drug coating preferably comprises a kind of disintegrating agent as indicated above, when this disintegrating agent contacts with water with swelling and make dressing be broken into small pieces.Preferred Drug coating comprises a kind of Zeo-karb, as by Purolite company with title Purolite
_C100NaMR is the sodium salt of poly-(vinylbenzene-Vinylstyrene) multipolymer of sulfonated and with title Purolite
_C100CaMR be the calcium salt of poly-(vinylbenzene-Vinylstyrene) multipolymer of sulfonated sell those.
3. the present composition can comprise a kind of effervescent.The effervescent that the present invention uses is meant as the result of chemical reaction between solubility acid source and the alkaline carbonate and produces carbon dioxide, thereby emerge bubble from liquid.In washing composition, add the disintegration time that this effervescent shortens composition.Add-on is preferably 0.1% to 20% of composition weight, and more preferably 5% to 20%.Preferred effervescent should be with the agglomerate of variable grain or with the compact form but as independent particle adding.
4. by using compound such as sodium acetate, nitrilotriacetic acid(NTA) and salt thereof or urea that other dispersing auxiliary can be provided.Suitable dispersing auxiliary inventory is seen Pharmaceutical Dosage Forms:Tablets, the 1st volume, the 2nd edition, editors such as H.A.Lieberman, ISBN 0-8247-8044-2.
5. disperse for helping, non-gelationization binding agent can be added in the particle that forms tablet.They are preferably selected from the synthetic organic polymer, as polyoxyethylene glycol, Polyvinylpyrolidone (PVP), poly-acetic ester, water-soluble acrylic ester multipolymer, and composition thereof.Pharmaceutical Excipients2nd Edition handbook has following binding agent kind: gum arabic, alginic acid, carbomer, Xylo-Mucine, dextrin, ethyl cellulose, gelatin, guar gum, I type hydrogenated vegetable oil, Natvosol, Vltra tears, Liquid Glucose, aluminum magnesium silicate, Star Dri 5, methylcellulose gum, polymethacrylate, polyvidone, sodiun alginate, starch and zein.Most preferred binding agent is in the suds and also has active cleaning function, as cationic polymers.Example comprises ethoxylation hexamethylene-diamine quaternary compound, bis hexamethylene triamine or other is as five amine, ethoxylation polyvinylamine, toxilic acid acrylate copolymer.
6. the present composition also can comprise swellable clay.The term " inflatable " that the present invention uses is meant the clay of (or expansion) ability that has swelling when contact with water.These are three layers of clay normally, as have the silico-aluminate and the Magnesium Silicate q-agent of the loading capacity of at least 50 milligramequivalents/100 gram clays.Three layers of swellable clay that use among the present invention are categorized as the terre verte class on geology.Can be used for clay example of the present invention and comprise montmorillonite, volchonskoite, nontronite, hectorite, saponite, sauconite, vermiculite, and composition thereof.Clay among the present invention can obtain with different trade(brand)names, for example Thixogel#1 and Gelwhite GP (derive from Georgia Kaolin Co., Elizabeth, NJ, USA); Volclay BC and Volclay#325 (derive from American Colloid Co., Skokie, IL, USA); Black Hills Bentonite BH450 (deriving from InternationalMinerals and Chemicals); And Veegum Pro and Veegum F (deriving from R.T.Vanderbilt).Should be realized that the terre verte class mineral that obtain with above-mentioned trade(brand)name can comprise the mixture of various discrete ore entities.The mixture of this class smectite minerals is applicable to the present invention.
7. composition of the present invention can comprise highly soluble mixture.This class mixture can be by mixture or single compound formation.Example comprises acetate, urea, Citrate trianion, phosphoric acid salt, diisobutyl benzene sulfonic acid sodium salt (DIBS), toluenesulfonic acid sodium salt, and composition thereof.
8. the present composition can comprise a kind of compound that has adhesive effect on the detergent base that forms composition.Form adhesive effect on the particulate material of detergent base of this tablet and be in order to the detergent base of investigating of suppressing under the controlled compression condition be foundation, a tablet or the broken required power of one deck are characterized.For given force of compression, high tablet or layer intensity represent that the particle height bonds together when particle compresses, and therefore stronger adhesive effect takes place.The method of tablet or layer intensity (also being called the diameter rupture stress) of estimating is described the Pharmaceutical dosage forms:tablets that people such as seeing H.A.Lieberman edits, published in 1989, volume1.The mensuration of adhesive effect is: will not contain the tablet of original principle powder of the compound with adhesive effect or layer intensity and comprise the tablet or the layer intensity of powdered mixture that 97 parts of original principle powder and 3 parts have the compound of adhesive effect and compare.Compound with adhesive effect preferably is added in the matrix with water-free in fact form (moisture content is lower than 10% (preferably being lower than 5%)).Adding temperature is between 10 to 80 ℃, more preferably between 10 to 40 ℃ of temperature.When under 3000 newton's the setting pressure, to contain 50 gram detergent particles materials and diameters be 55 millimeters tablet owing to exist 3% compound with adhesive effect to make its tablet tensile strength enhancing more than 30% when (preferred 60%, more preferably 100%) in the matrix granule material, this compound just is defined as having adhesive effect according to particulate material of the present invention.An example with compound of adhesive effect is two iso-alkyl benzene sulfonic acid sodium salts.
Another preferred component that is applicable to the present composition is one or more enzymes.Suitable enzyme comprises and is selected from following enzyme: peroxidase, proteolytic enzyme, glucoamylase, amylase, zytase, cellulase, lipase, Phospholipid hydrolase, esterase, at, polygalacturonase, M-Zyme, reductase enzyme, oxydase, phenol oxidase, lipoxygenase, ligninase, Starch debranching enzyme, tannase, pentosanase, malanases, beta-glucanase, arabinofuranosidase/xylosidase, Unidasa, chondroitinase, dextranase, transferring enzyme, laccase, mannase, xyloglucanase enzymes, or its mixture.Detergent composition generally comprises a kind of usual for example mixture of proteolytic enzyme, amylase, cellulase, lipase of enzyme that is suitable for.Enzyme is 0.0001% to 2% to account for composition weight usually, and is preferred 0.001% to 0.2%, and more preferably 0.005% to 0.1% pure enzyme content mixes in the detergent composition.Above-mentioned enzyme can derive from the source of any appropriate, for example plant, animal, bacterium, fungi and yeast source.The source can also be to have a liking for the mesomeric state bacterium or have a liking for extreme condition bacterium (psychrophilic bacteria, fear cold bacterium (psychrotrophic), thermophile bacteria, barophilic bacteria, have a liking for alkali bacterium, acidophilic bacteria, halophilic bacterium etc.).Can use purifying or these enzymes of purified form not.Now, convention is to come the modification wild-type enzyme to optimize its effectiveness of performance in detergent composition of the present invention by albumen/genetic engineering technique.For example, can design varient, the feasible compatibility that can improve the composition commonly used of this enzyme and this based composition.Perhaps, can design varient, make best pH, SYNTHETIC OPTICAL WHITNER or sequestrant stability, the catalytic activity etc. that to adjust this enzyme variant body to be fit to specific cleaning applications.As for the stability of enzyme in liquid washing agent, should concentrate on attention on the amino acid to oxidation-sensitive on (with regard to bleach stability) and the surface charge (with regard to the tensio-active agent compatibility).Can change this zymoid iso-electric point by replacing some charged amino acid.Can also improve sequestrant stability by producing for example additional salt bridge and reinforcement metal binding site, thereby further strengthen the stability of enzyme.In addition, can carry out chemical modification or enzyme catalysis modification to enzyme, for example PEGization, crosslinked and/or can be fixed can be used the enzyme that is attached on the carrier.The enzyme that is incorporated in the detergent composition can be any suitable form, and for example liquid, capsule thing, bead, particle are perhaps according to any other form of mature technology in the industry.
Composition of the present invention preferably comprises washing assistant.Suitable water soluble detergency promoter compound used herein comprises the polycarboxylate of water-soluble monomer or polycarboxylic acid or its salt of its sour form, homopolymerization or copolymerization, wherein polycarboxylic acid comprises at least two separate carboxyl, carbonate, supercarbonate, borate, phosphoric acid salt that are no more than 2 carbon atoms, and composition thereof.Carboxylate salt or polycarboxylic acid salt washing assistant can be monomer or oligomeric type, although the polycarboxylate of monomeric form generally is preferred.The suitable carboxylate salt that contains a carboxyl comprises water-soluble lactic acid salt, glycollate and ether derivant thereof.The polycarboxylate that comprises two carboxyls comprises the water-soluble salt of following material: succsinic acid, propanedioic acid, (ethylenedioxy) oxalic acid, toxilic acid, diglycollic acid, tartrate, tartronic acid and fumaric acid, and ether carboxylate and sulfinyl carboxylate salt.The polycarboxylate that comprises three carboxyls especially comprises water-soluble citrate, aconitate and citraconate and succinate derivative, as GB-A-1,379, the carboxyl methyl oxygen base succinate, the GB-A-1 that describe in 241,389, the aminosuccinic acid salt, the GB-A-1 that describe among the newborn acyloxy succinate of describing in 732, the NL-A-7205873, oxygen Quito unit carboxylate salt material of describing in 387,447.Be applicable to that the polycarboxylate that comprises 4 carboxyls of the present invention comprises GB-A-1, those disclosed in 261,829.Comprise the substituent polycarboxylate of sulfo group and comprise GB-A-1, disclosed sulfo-succinic acid salt derivative in 398,421, GB-A-1,398,422 and US-A-3,936,448, and GB-A-1, the sulfonated pyrolytic Citrate trianion of describing in 439,000.Alicyclic and heterocycle polycarboxylate comprises pentamethylene-cis, cis, cis-tetracarboxylic acid hydrochlorate, 2,5-tetrahydrofuran (THF)--cis-dicarboxylate, 2,2,5,5-tetrahydrofuran (THF)-tetracarboxylic acid hydrochlorate, 1,2,3,4,5, the carboxymethyl derivant of 6-hexane-hexacarboxylic acid salt and polyvalent alcohol such as sorbyl alcohol, mannitol and Xylitol.Aromatic polycarboxylic acid salt comprises GB-A-1, disclosed benzene hexacarboxylic acid, pyromellitic acid and phthalic acid derivatives in 425,343.Preferred polycarboxylate is that per molecule comprises the hydroxycarboxylate that can reach 3 carboxyls, especially Citrate trianion.The mixture of the parent acid of monomeric or oligomeric polycarboxylate sequestrant or itself and its salt also can be considered as washing assistant as citric acid or Citrate trianion/citric acid mixture.The example of carbonate builders is alkaline-earth metal and alkaline carbonate, comprise yellow soda ash and concentrated crystal soda and with the mixture of calcium carbonate superfine powder, DE-A-2 for example, disclosed in 321,001.Be applicable to that portion water dissolubility washing-aid compound of the present invention comprises as EP-A-164, disclosed crystalline layered silicate in 514 and EP-A-293,640.Preferred crystalline layered sodium silicate has following general formula:
NaMSi
xO
2+1.yH
2M is sodium or hydrogen in the O formula, and x is 1.9 to 4 number, and y is 0 to 20 number.This class crystalline layered sodium silicate preferably has the two-dimensional sheet structure, EP-A-164 for example, so-called δ-layer structure of describing in 514 and EP-A-293,640.The preparation method of this class crystalline layered silicate is disclosed in DE-A-3, in 417,649 and DE-A-3,742,043.Preferred crystalline layered sodium silicate compound has formula 5-Na
2Si
2O
5Structure, be called NaSKS-6
TM, can derive from Hoeschst AG.
Be applicable to that basic water-insoluble washing assistant of the present invention comprises sodium silicoaluminate.Suitable silico-aluminate comprises having formula Na
z[(AlO
2)
z(SiO
2)
y] .xH
2The unitary aluminosilicate zeolite of O structure cell, z and y are at least 6 in the formula, the mol ratio of z and y is 1 to 0.5, x at least 5, be preferably 7.5 to 276, more preferably 10 to 264.Alumino-silicate materials be hydrated form and be preferably crystallization, contain 10% to 28%, more preferably the water of 10% to 22% combining form.Aluminosilicate zeolite can be naturally occurring material, but preferred synthetic gained.Synthetic crystal aluminosilicate ion exchange material can obtain with the title of Zeolite A, Zeolite B, Zeolite P, ZeoliteX and Zeolite HS.Preferred aluminosilicate zeolite is the colloidal state aluminosilicate zeolite.When as the component of detergent composition, colloidal state aluminosilicate zeolite, especially colloidal state Zeolite A provide enhanced to help and have washed usefulness, especially show to improve detergency ability, alleviate the fabric fouling and improve fabric whiteness and keep the aspect.The mixture of colloidal state Zeolite A and colloidal state Zeolite Y also is suitable for providing in the present invention the calcium ion and the magnesium ion chelating ability of excellence.
The present invention can use fabric softener.Any suitable softening agent all can be used for the present invention, but preferably quaternary ammonium agent and/or clay softening system.
The term " quaternary ammonium agent " that the present invention uses is meant to have a quaternary nitrogen atoms and have one or morely, preferred two, comprises the compound of group of 6 or 6 above carbon atoms or the mixture of compound.Be used for quaternary ammonium agent of the present invention and be preferably selected from and have a quaternary nitrogen atoms, and this quaternary nitrogen atoms there are two each those self-contained more than 10 or 10, that the group of preferred 12 or 12 above carbon atoms replaces materials.The preferred embodiment that is applicable to the quaternary ammonium compound of the present composition is chlorination N, N-two (canolyl-oxygen base-ethyl)-N, N-Dimethyl Ammonium, methylsulfuric acid N, N-two (canolyl-oxygen base-ethyl)-N-methyl-N-(2-hydroxyethyl) ammonium, chlorination N, N-two (canolyl-oxygen base-ethyl)-N-methyl-N-(2-hydroxyethyl) ammonium and composition thereof.Especially being preferred for of the present invention is methylsulfuric acid N, N-two (canolyl-oxygen base-ethyl)-N-methyl-N-(2-hydroxyethyl) ammonium.Though the quaternary ammonium compound derived from " canolyl " fatty acyl group is preferred; but the example that other of quaternary ammonium compound suits is derived from fatty acyl group; term " canolyl " in the wherein above-mentioned example replaces with term " tallow base, cocoyl, palm oil base (palmyl), lauryl, oleyl, castor oil-base, stearyl, palmityl ", and these are corresponding to deriving the unitary sources of triglycerides of fatty acyl group.These alternative fats acyl group sources can comprise fully saturated or preferably to the undersaturated chain of small part.
Can use any suitable clay softening system, but preferably comprise the clay softening system of clay mineral compound and the clay flocculating agent of choosing wantonly.If exist, forming composition of the present invention preferably comprises the clay softening system that accounts for composition total weight 0.001% to 10%.The preferred a kind of terre verte class clay compound of this clay mineral compound.Terre verte class clay is disclosed in US-A-3, in 862,058, US-A-3,948,790, US-A-3,954,632 and US-A-4,062,647.EP-A-299 in addition, 575 and EP-A-313,146 have described suitable organic polymer clay flocculating agent.
The present composition can comprise sequestrant/heavy metal ion sequestering agent.So-called heavy metal ion sequestering agent is meant the component that is used for sequester (chelating) heavy metal ion in the present invention.These components also can have calcium and magnesium sequestering power, but preferentially to showing selectivity in conjunction with heavy metal ion such as iron, manganese and copper.The heavy metal ion sequestering agent with account for composition weight 0.005% to 20%, preferred 0.1% to 10%, more preferably 0.25% to 7.5%, most preferably 0.5% to 5% amount uses.Be used for suitable heavy metal ion sequestering agent of the present invention and include organic phosphonates, for example poly-(alkylene phosphonic acids salt), basic metal ethane 1-hydroxyl diphosphonate and nitrilo trimethylene phosphonic salt of amino alkylidenyl.Preferably diethylenetriamine five (methylene phosphonic acid salt), quadrol three (methylene phosphonic acid salt), hexamethylene-diamine four (methylene phosphonic acid salt) and hydroxyl-ethylidene-1 in the mentioned kind, the 1-diphosphonate.Other is applicable to that heavy metal ion sequestering agent of the present invention comprises nitrilotriacetic acid(NTA) and polyamino carboxylic acid, as ethylenediamine tetraacetic acid (EDTA), ethylidene pentaacetic acid, ethylenediamine disuccinic acid, quadrol two pentanedioic acids, 2-hydroxyl propylene diamine disuccinic acid or its any salt.Especially preferred is quadrol-N, N '-disuccinic acid (EDDS) or its an alkali metal salt, alkaline earth salt, ammonium salt or substituted ammonium salt is arranged, or its mixture.Preferred EDDS compound is free acid form and its sodium salt, magnesium salts or its title complex.
The present composition can comprise a kind of foam inhibition system.Be applicable to that foam inhibition system of the present invention can comprise all known defoamer compound basically, comprises as siloxanes defoaming compounds, 2-alkyl and alcanol defoaming compounds.Preferred foam inhibition system and defoaming compounds are disclosed among WO-A-93/08876 and the EP-A-705 324.
The present composition can comprise laking agent (fixative).These are known commercially available materials, and they are intended to improve by the dye for fabrics minimization of loss that washing is caused the outward appearance of DYED FABRICS.Many laking agent are cationic, and be based on quaternized nitrogen compound or based on nitrogen compound with strong cation electric charge, described strong cation electric charge forms under working conditions on the spot.Cationic fixing agent can be with different trade names available from the man supplier of number.Representational trade name comprises Tinofix ECO, Tinofix FRD and the Solfin by REWIN SRF, the REWIN SRF-O of SANDOFIX SWE, the CHT-BeitlichGmbH of the SANDOFIX TPS of the INDOSOL E-50 of the CROSCOLOR PMF of Crosfield company and CROSCOLOR NOFF, Sandoz company, Sandoz company, Sandoz company and REWIN DWE, Ciba-Geigy company.
Other cationic fixing agent is described in " Aftertreatments for Improving theFastness of Dyes on Textile Fibres ", Christopher C.Cook, and Rev.Prog.Coloration is among the Vol.XII (1982).The laking agent that is applicable to the present composition comprises ammonium salt compound, as lipid acid-diamines condenses, the particularly hydrochloride of diamines ester, acetate, sulfuric acid one methyl esters salt and benzyl hydrochloride.Limiting examples comprises oil base diethylamino buserelin, sulfuric acid one methyl esters oil base methyl two quadrols, sulfuric acid one methyl esters one stearyl ethylidene diamino-Trimethylamine.The N-oxide compound, the derivative of polymkeric substance alkyl diamine, polyamine mauguinite urine condenses, the amination DCH that comprise tertiary amine in addition, and composition thereof.
The laking agent that is applicable to other kind of the present invention is the cellulolytic activity laking agent.A kind of in order to comprise " laking agent system ", the cellulolytic activity laking agent can suitably be used in combination with one or more above-mentioned laking agent.Among the present invention, term " cellulolytic activity laking agent " be defined as on the spot or by the makers-up heat or during thermal treatment can with the laking agent of cellulosic fibre reaction.The cellulolytic activity laking agent is described in detail among the WO-A-00/15745.
The present composition can comprise the polymeric dye transfer inhibitor.If present, the composition of moulding of the present invention preferably comprises and accounts for total composition weight 0.01% to 10%, preferred 0.05% to 0.5% polymeric dye transfer inhibitor.The polymeric dye transfer inhibitor is preferably selected from multipolymer, polyvinylpyrrolidonepolymers polymers or its combination of polyamine N-oxide pllymers, N-vinyl pyrrolidone and N-vinyl imidazole.
The present composition can comprise the polymkeric substance that alleviates fabric abrasion.Any suitable polymkeric substance that alleviates fabric abrasion all can be used for the present invention.Some case descriptions of suitable polymkeric substance are in WO-A-00/15745.
The present composition can comprise and subtracts the wrinkle agent.Any suitable wrinkle agent that subtracts all can be used for the present invention.Suitable some case descriptions of wrinkle agent that subtract are in WO-A-99/55953.
The another kind of composition that can exist is a bleach systems, as percarbonate especially sodium salt, and/or the organic peroxide acid bleach precursor, and/or the transition metal bleach catalyzer especially comprises those SYNTHETIC OPTICAL WHITNER of Mn or Fe.Have been found that when capsule or compartment are formed by material that comprises free hydroxyl group such as PVA preferred SYNTHETIC OPTICAL WHITNER comprises percarbonate and preferably do not contain any perborate or borate.Have been found that borate and perborate and these hydroxyl matter interactions and reduce its solubleness, also cause performance to reduce.Inorganic perhydrate is a kind of preferred peroxide source.The example of inorganic perhydrate salt comprises percarbonate, superphosphate, persulphate and persilicate.Inorganic perhydrate salt is an alkali metal salt normally.Alkali metal percarbonate, especially SPC-D is the preferred perhydrate of the present invention.Composition of the present invention preferably comprises a kind of peroxy acid or its precursor (bleach-activating agent), preferably comprises a kind of organic peroxide acid bleach precursor.Preferably composition comprises at least two kinds of peroxyacid bleach precursors, and preferred at least a hydrophobicity peroxyacid bleach precursor and at least a wetting ability peroxyacid bleach precursor define as the present invention.Situ reaction by this precursor and hydrogen peroxide cource produces organic peroxide acid then.The hydrophobicity peroxyacid bleach precursor preferably comprises a kind of compound with an oxygen-Phenylsulfonic acid base, preferably NOBS, DOBS, LOBS and/or NACA-OBS as described in the present invention.The wetting ability peroxyacid bleach precursor preferably includes TAED.The alkyl peroxy acids precursor compound that has acid amides to replace can be used for the present invention.The suitable bleach activating immunomodulator compounds that has acid amides to replace is described among the EP-A-0170386.
Composition can comprise a kind of preformed organic peroxide acid.The preferred organic peroxy acid compound of one class is described in EP-A-170, in 386.Other organic peroxide acid comprises diacyl and four acyl peroxides, particularly diperoxy dodecanedioic acid, diperoxy tetradecane diacid and diperoxy Thapsic acid.Undecane dicarboxylic acids crossed by one and two mistake nonane diacids, one and two and N-O-phthalic amido peroxide caproic acid also is applicable to the present invention.
Other composition that can be added in the present composition comprises white dyes, organic polymer, alkalimetal silicate, tinting material and lime soap dispersion agent.
Composition of the present invention is not preferably prepared to such an extent that have a too high pH value.The pH of composition of the present invention is 7.0 to 12.5, more preferably 7.5 to 11.8 when preferably measuring with its distilled water solution of 1%, most preferably is 8.0 to 11.5.
Separation method
The present invention includes two-phase or multiphase separation method of the composition made by compressed microparticles.Said method comprising the steps of:
(a) make the composition of compression cracked for particle and
(b) separate each phase according to its particle size.
The composition of compression can be by the pulverizing of any suitable method, but the particle that obtains must have essentially identical particle size with first phase.That is, breaking method must be each to be reentried mutually initially add the method for fashionable similar geometric mean particle diameter with it.Composition preferably uses a pair of column type rotating cylinder with built-in cutter to carry out fragmentation, and (example of these devices is Telschig shears and Opbouw Messen ' s Cru-cut
_Shears).Afterwards composition is sent on the conventional rotating screen so that the mobile packing of separating plastic is sent to lump breaker (for example, Kemutec K1350 sieve apparatus then
_) in, be not sheared the last tablet fragment of crusher machine with further fragmentation.
After the micronize, can be by any suitable each phase of method composition for separating (every have mutually different particle sizes).Preferably, particle is sent into sieve apparatus, as Rotex Gradex 2000
_In, this sieve apparatus can be available from the Rotex company of the Ohio, USA city of Cincinnati.
In case respectively be separated, just they can be sent in its pre-composition separately and recompression.
Embodiment
Use follow procedure to prepare a kind of composition:
First phase:
Weight %, based on
Composition total weight
Negatively charged ion agglomerate 1 7.1
Negatively charged ion agglomerate 2 17.5
Nonionic agglomerate 9.1
Positively charged ion agglomerate 4.6
Layered silicate 9.7
SPC-D 12.2
Bleach-activating agent agglomerate 6.1
Yellow soda ash 7.27
EDDS/ sulphate particle 0.5
Hydroxyl ethane di 2 ethylhexyl phosphonic acid tetra-na salt 0.6
Soil release polymer 0.3
Fluorescent agent 0.2
Phthalocyanine sulfonic acid zinc encapsulate 0.03
Soap powder 1.2
Suds suppressor 2.8
Citric acid 4.5
Proteolytic enzyme 1
Lipase 0.35
Cellulase 0.2
Amylase 1.1
Sparge the binding agent 3.05 of system
Spray perfume 0.1
DIBS (diisobutyl benzene sulfonic acid sodium salt) 2.1
Negatively charged ion agglomerate 1 comprises 40% anion surfactant, 27% zeolite and 33% carbonate.
Negatively charged ion agglomerate 2 comprises 40% anion surfactant, 28% zeolite and 32% carbonate.
The nonionic agglomerate comprises 26% nonionogenic tenside, 6%Lutensit K-HD 96 (coming from BASF), 40% anhydrous sodium acetate, 20% carbonate and 8% zeolite.
The positively charged ion agglomerate comprises 20% cats product, 56% zeolite and 24% vitriol.
Layered silicate comprises 95%SKS 6 and 5% silicate.
The bleach-activating agent agglomerate comprises 81% tetra acetyl ethylene diamine (TAED), 17% vinylformic acid/maleic acid (acid type) and 2% water.
The EDDS/ sulphate particle comprises 58% quadrol-N, N-disuccinic acid sodium salt, 23% vitriol and 19% water.
Phthalocyanine sulfonic acid zinc encapsulate is 10% effective constituent.
Suds suppressor comprises 11.5% silicone oil (coming from Dow Corning), 59% zeolite and 29.5%H
2O.
The binding agent that sparges system comprises 0.5 part of Lutensit K-HD 96 and 2.5 parts of polyoxyethylene glycol (PEG).
Second phase:
Weight % is based on group
The compound gross weight
Softening agent and fragrance beads 8.4
The fragrance beads composition comprises 56%expancel 091DE80,7% silicon-dioxide, 8% spices, 5% cross-linking polyvinyl alcohol (PVA)-borate, 5% water, 18% cationic softener sulfuric acid, one methyl esters N, the Zeneca Monastral indigo plant of N-two (candyl-oxygen-ethyl)-N-methyl-N-(2-hydroxyethyl) ammonium and 1% laundry compatibility.
Make:
The manufacturing of first phase:
Being prepared as follows of the washing composition active composition of first phase: in mixing tank, grain fraction was mixed 5 minutes, form the homogeneous granules mixture.Between this mixing period, use above-mentioned adhesive composition to spray by nozzle and hot blast.Median size is 560 microns.
The manufacturing of the 2nd phase:
Use has the Braun food-processor of standard agitator, to wherein adding above-mentioned drying composite, makes the bead of second phase.Agitator is run up 1 minute also with in this mixture impouring Fuji Paudal Dome Gran DGL1 (Japan) forcing machine, and this forcing machine has diameter in extruding end plate be 3 millimeters hole and the speed running of changeing with per minute 70.Products therefrom is added among the Fuji Paudal Marumerizer QJ-230, this machine was turned round 5 minutes with the speed that per minute 1000 changes, obtain good spheroidization.
In next step, with the insoluble Drug coating coating of described part bead.Apply as follows: in conventional mixing tank, under 70 ℃ of temperature, use fog nozzle and hot blast, the mixture of being made up of 80% cross-linking polyvinyl alcohol-borate and 20% water with 4% (based on the weight of bead) sprays bead.Then bead was placed the cylindrical blender mixing 60 minutes and injected hot blast, with the part moisture content that contains in the evaporation PVA dressing.Superincumbent bead has been mentioned the final water content in the bead in forming.
The particle diameter of resulting bead is 2110 microns.
The manufacturing of tablet:
Use Instron 4400 trier and manual tablet manufacturing to prepare heterogeneous tablet composition with the standard die head.It is in 2.5 millimeters 41 * 41 millimeters the die head with circular edge that the washing composition active compositions of 35 grams, first phase are sent into ratio.This mixture uses the force compresses of drift with 1,500 newton, and this drift has the suitable shape that can form the spill model of a 25mm diameter and the 10mm degree of depth in this tablet.Take out forming punch carefully, tablet is stayed in this die head.The 4 gram beads that will form second phase import in the model stay in first figure of tablet and use the common drift of planar to apply 1,700 newton's pressure at last, to make heterogeneous tablet.By hand tablet is ejected from die head then.
In next step, will immerse in 170 ℃ of fused Drug coating mixtures with the tablet that aforesaid method makes is manual, make its cool to room temperature then, make dressing sclerosis carrying out dressing.The composition of Drug coating and per-cent are described in the composition of top tablet.
Process the material that is equivalent to 1 kilogram of mobile package troche by Opbouw Messen shears, then it is transferred on the pillar rotating screen with 10 millimeters * 10 millimeters perforates, flow with separating plastic from the tablet of pulverizing and pack.After the packing that flows is separated, this mixture is transferred in the Kemutec K1350 lump breaker, be converted into powder so that tablet is remained fragment.
For the density according to them is classified particle, the laboratory scale device that preparation is made with the transparent plastics post of 10 cm diameters.Vacuum cleaner with a standard links to each other at its top with this post, and the sieve of 50 microns perforates is arranged in the every side of post.By the control device control air-flow of vacuum cleaner self, be returned to the top of post so that have the particle of light density, and the mode that makes fine and close particle be returned to the bottom of post is set up this system.
For the macrobead size is classified mutually with the smaller particles size, flow of powder is transported on the Rhewum WA 8/270 * 180V sieve with 1500 * 1500 microns holes.Adopt this method to be recovered to two kinds of flow of powders: the geometric mean particle diameter is the fine particle fraction that 2137 microns coarse particles fraction and geometric mean particle diameter are 691 microns.
Then the content of these two fractions with 10% weight (in each phase) is mixed in the starting powder stream again, and prepares new composition according to the same program shown in top.
Claims (10)
1. the multi-phase detergent composition of a compressing grains material, wherein the geometric mean particle diameter of a phase differs at least 300 microns with another geometric mean particle diameter mutually at least.
2. detergent composition as claimed in claim 1, wherein the geometric mean particle diameter of a phase differs at least 750 microns with another geometric mean particle diameter mutually at least.
3. detergent composition as claimed in claim 1 or 2, wherein the geometric mean particle diameter of a phase differs at least 1000 microns with another geometric mean particle diameter mutually at least.
4. the described detergent composition of each claim as described above, wherein said composition has two-phase.
5. the described detergent composition of each claim as described above, wherein each is arranged with the stratiform form.
6. the described detergent composition of each claim as described above, wherein each is with a form arrangement that is inserted into mutually in the mould of another phase.
7. the described detergent composition of each claim as described above, wherein composition is tablet form.
8. the phase disengagement method of the multi-phase detergent composition of compressing grains material, wherein the geometric mean particle diameter of first phase differs at least 300 microns with second mutually the geometric mean particle diameter, and described method comprises the following steps:
(a) make compressed compositions cracked for particle and
(b) separate each phase according to their particle size.
9. method as claimed in claim 8, wherein particle separates by sieve apparatus.
10. method will as claimed in claim 8 or 9 turn back in its pre-composition separately and recompression after wherein will separating mutually.
Applications Claiming Priority (10)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP00870252.4 | 2000-10-31 | ||
| EP00870253.2 | 2000-10-31 | ||
| EP00870254.0 | 2000-10-31 | ||
| EP00870254A EP1201743A1 (en) | 2000-10-31 | 2000-10-31 | Detergent compositions |
| EP00870252A EP1201741A1 (en) | 2000-10-31 | 2000-10-31 | Detergent compositions |
| EP00870253A EP1201742A1 (en) | 2000-10-31 | 2000-10-31 | Detergent compositions |
| EP01870013.8 | 2001-01-19 | ||
| EP01870013A EP1201745A1 (en) | 2000-10-31 | 2001-01-19 | Shaped detergent compositions |
| EP01870012A EP1201744A1 (en) | 2000-10-31 | 2001-01-19 | Detergent compositions |
| EP01870012.0 | 2001-01-19 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1473193A true CN1473193A (en) | 2004-02-04 |
Family
ID=27513083
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA018183735A Pending CN1473194A (en) | 2000-10-31 | 2001-10-26 | Reprocessing of detergent tablets |
| CNA018183697A Pending CN1473193A (en) | 2000-10-31 | 2001-10-26 | Reblending of detergent tablets |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA018183735A Pending CN1473194A (en) | 2000-10-31 | 2001-10-26 | Reprocessing of detergent tablets |
Country Status (7)
| Country | Link |
|---|---|
| EP (2) | EP1330508A2 (en) |
| CN (2) | CN1473194A (en) |
| AU (2) | AU2002239794A1 (en) |
| BR (2) | BR0115015A (en) |
| CA (2) | CA2424143A1 (en) |
| MX (2) | MXPA03003818A (en) |
| WO (2) | WO2002042407A2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105670809A (en) * | 2016-02-24 | 2016-06-15 | 奉化市瑶琴生物科技有限公司 | Portable household cleaning agent and preparing and use methods thereof |
Families Citing this family (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1418226B1 (en) * | 2002-11-07 | 2006-10-04 | Unilever N.V. | Detergent composition |
| GB0913808D0 (en) | 2009-08-07 | 2009-09-16 | Mcbride Robert Ltd | Dosage form detergent products |
| EP2588589B2 (en) | 2010-07-02 | 2023-07-19 | The Procter & Gamble Company | Process for the production of a detergent product |
| JP5759544B2 (en) | 2010-07-02 | 2015-08-05 | ザ プロクター アンド ギャンブルカンパニー | Methods for delivering active agents |
| CN114796017A (en) | 2014-04-22 | 2022-07-29 | 宝洁公司 | Composition in the form of a soluble solid structure |
| CN104257624A (en) * | 2014-09-10 | 2015-01-07 | 天津爱勒易医药材料有限公司 | Novel effervescent and disintegrative premix and preparation method thereof |
| WO2018140676A2 (en) | 2017-01-27 | 2018-08-02 | The Procter & Gamble Company | Compositions in the form of dissolvable solid structures |
| CN110167639B (en) | 2017-01-27 | 2022-10-14 | 宝洁公司 | Composition in the form of a soluble solid structure comprising effervescent agglomerated granules |
| MX2019013048A (en) | 2017-05-16 | 2019-12-11 | Procter & Gamble | Conditioning hair care compositions in the form of dissolvable solid structures. |
| JP1629688S (en) | 2018-07-16 | 2019-04-15 | ||
| US11666514B2 (en) | 2018-09-21 | 2023-06-06 | The Procter & Gamble Company | Fibrous structures containing polymer matrix particles with perfume ingredients |
| MX2021013141A (en) | 2019-06-28 | 2021-12-10 | Procter & Gamble | Dissolvable solid fibrous articles containing anionic surfactants. |
| MX2021015391A (en) | 2019-07-03 | 2022-01-24 | Procter & Gamble | Fibrous structures containing cationic surfactants and soluble acids. |
| USD939359S1 (en) | 2019-10-01 | 2021-12-28 | The Procter And Gamble Plaza | Packaging for a single dose personal care product |
| US11597191B2 (en) | 2019-10-14 | 2023-03-07 | The Procter & Gamble Company | Biodegradable and/or home compostable sachet containing a solid article |
| WO2021097691A1 (en) | 2019-11-20 | 2021-05-27 | The Procter & Gamble Company | Porous dissolvable solid structure |
| USD962050S1 (en) | 2020-03-20 | 2022-08-30 | The Procter And Gamble Company | Primary package for a solid, single dose beauty care composition |
| WO2022027067A1 (en) | 2020-07-31 | 2022-02-03 | The Procter & Gamble Company | Water-soluble fibrous pouch containing prills for hair care |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3541146A1 (en) * | 1985-11-21 | 1987-05-27 | Henkel Kgaa | MULTILAYERED DETERGENT TABLETS FOR MACHINE DISHWASHER |
| GB9015503D0 (en) * | 1990-07-13 | 1990-08-29 | Unilever Plc | Detergent composition |
| DE19542688A1 (en) * | 1995-11-16 | 1997-05-22 | Peter Dieckmann | Method and device for separating a good consisting of solid particles of different shape, size and / or density into at least two components |
| GB2324495A (en) * | 1997-04-22 | 1998-10-28 | Procter & Gamble | Multi-layer detergent tablet |
| GB2327949A (en) * | 1997-08-02 | 1999-02-10 | Procter & Gamble | Detergent tablet |
| CA2296354C (en) * | 1997-11-10 | 2003-05-27 | The Procter & Gamble Company | Detergent compositions |
| GB2331994A (en) * | 1997-12-02 | 1999-06-09 | Procter & Gamble | Detergent tablet |
-
2001
- 2001-10-26 MX MXPA03003818A patent/MXPA03003818A/en unknown
- 2001-10-26 CN CNA018183735A patent/CN1473194A/en active Pending
- 2001-10-26 EP EP01987591A patent/EP1330508A2/en not_active Withdrawn
- 2001-10-26 BR BR0115015-4A patent/BR0115015A/en not_active IP Right Cessation
- 2001-10-26 WO PCT/US2001/051378 patent/WO2002042407A2/en not_active Application Discontinuation
- 2001-10-26 BR BR0115022-7A patent/BR0115022A/en not_active IP Right Cessation
- 2001-10-26 CN CNA018183697A patent/CN1473193A/en active Pending
- 2001-10-26 EP EP01987592A patent/EP1330509A2/en not_active Withdrawn
- 2001-10-26 MX MXPA03003816A patent/MXPA03003816A/en unknown
- 2001-10-26 CA CA002424143A patent/CA2424143A1/en not_active Abandoned
- 2001-10-26 WO PCT/US2001/051379 patent/WO2002038722A2/en not_active Application Discontinuation
- 2001-10-26 AU AU2002239794A patent/AU2002239794A1/en not_active Abandoned
- 2001-10-26 AU AU2002239793A patent/AU2002239793A1/en not_active Abandoned
- 2001-10-26 CA CA002424168A patent/CA2424168A1/en not_active Abandoned
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105670809A (en) * | 2016-02-24 | 2016-06-15 | 奉化市瑶琴生物科技有限公司 | Portable household cleaning agent and preparing and use methods thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| MXPA03003818A (en) | 2003-07-28 |
| CA2424143A1 (en) | 2002-05-30 |
| WO2002038722A2 (en) | 2002-05-16 |
| EP1330508A2 (en) | 2003-07-30 |
| AU2002239793A1 (en) | 2002-06-03 |
| AU2002239794A1 (en) | 2002-05-21 |
| BR0115022A (en) | 2003-12-23 |
| WO2002038722A8 (en) | 2003-11-13 |
| WO2002042407A8 (en) | 2003-11-20 |
| WO2002042407A2 (en) | 2002-05-30 |
| CA2424168A1 (en) | 2002-05-16 |
| WO2002042407A3 (en) | 2002-08-29 |
| EP1330509A2 (en) | 2003-07-30 |
| CN1473194A (en) | 2004-02-04 |
| BR0115015A (en) | 2004-02-25 |
| WO2002038722A3 (en) | 2002-08-29 |
| MXPA03003816A (en) | 2003-07-28 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |