CN100544700C

CN100544700C - The dentifrice composition that abrasiveness reduces

Info

Publication number: CN100544700C
Application number: CNB2004800034708A
Authority: CN
Inventors: V·K·加德卡日; V·B·兰迪伊夫; M·R·文卡塔; N·A·贝彻贝特; S·A·卡达姆
Original assignee: FMC Corp
Current assignee: DuPont Nutrition USA Inc
Priority date: 2003-02-05
Filing date: 2004-02-04
Publication date: 2009-09-30
Anticipated expiration: 2024-02-04
Also published as: CN1747709A

Abstract

A kind of dentifrice composition is disclosed, described dentifrice composition comprises binding agent, surfactant, grinding agent, wetting agent and water, wherein, (1) described grinding agent is a silicon oxide, described compositions also comprises silica thickener, and described compositions comprises silica thickener, following silica abrasive, 45-70 weight % water, 0.8-3.0 weight % surfactant, the 0.05-3.0 weight % binding agent of 15 weight % of 1-7 weight %; Perhaps (2) described grinding agent is a silicon oxide, described compositions also comprises silica thickener, described compositions comprises silicon oxide, 0.8-3.0 weight % surfactant, the 0.05-3.0 weight % binding agent of 2-22 weight % altogether, and described compositions also comprises the non-colloid microcrystalline Cellulose of about 0.1-8.0 weight %, colloid microcrystalline Cellulose or their mixture; (3) or described binding agent be the calcio grinding agent, described binding agent is a cellulose gum, described compositions comprises the binding agent of 25-55 weight % calcio grinding agent, 35-60 weight % water, 0.8-3.0 weight % surfactant and 1.0-3.0 weight %.

Description

The dentifrice composition that abrasiveness reduces

The cross reference of related application

The application requires in the priority of the U.S. Provisional Patent Application No.60/445376 of submission on February 5th, 2003, and its reference in content is incorporated in this; And require in the priority of the U.S. Provisional Patent Application No.60/479690 of submission on June 19th, 2003, its reference in content is incorporated in this.

Invention field

The present invention relates to dentifrice composition.More particularly, the present invention relates to the high-moisture dentifrice composition, its water content height, and abrasiveness reduces.

Background of invention

In order to satisfy the needs of consumer, dentifrice composition should have some good physical of consumer's custom.These performances have good cleaning effect for toothpaste provides attracting sense of taste, clean easily, have good mouthfeel, and have physical stability.Dentifrice composition with acceptable physical stability is not easy sclerosis when storing, and can not occur being separated, and separates as water or spice.When allotter is extruded, the outward appearance of described toothpaste is also very important.Should seem smooth, and have pleasant honorable or glossy outward appearance.

In dentifrice composition, must have these character, this concerning consumer in the cost economical and effective.Continue at present to require to provide cost lower dentifrice composition, keep required character simultaneously.Although it has clear and definite benefit to tooth hygiene, this point is even more important to the area of those toothpaste of cannot afford in the world.

The material that dentifrice composition comprises polishing agent or grinding agent, wetting agent, binding agent or thickening agent, surfactant and water usually and treatment or dressing effect are provided is as fluoride, spice and sweeting agent.Described wetting agent and water also are referred to as excipient.Though described water content changes, most dentifrice composition comprises the water of about 10-25 weight %.

Compare the cost of other composition, because water is to so not expensive, so a kind of method that reduces the dentifrice composition cost improves its water content exactly.But in these dentifrice compositions, water content is higher relatively can to produce the problem that viscosity is low and/or be separated usually.In storage process, water can move down, and oil (as spice) then moves up.For high-moisture toothpaste, consumer finds that " wet lid " or spice concentrate on the situation at top, and this depends on that the pipe of adorning toothpaste is to store at lid up or under the situation down.There are adverse influence in the brilliance or the gloss that are separated also to the dentifrice composition extruded.

The dentifrice composition of many routines uses silica-based polishing agent.But, the needs of the abrasiveness of the conventional dentifrice composition of existence this use silicon oxide of reduction and calcio polishing agent in industry.Therefore, require there is the water content height, have favourable physical property and reduce the high-moisture dentifrice composition of abrasiveness.

Summary of the invention

The present invention relates to dentifrice composition.Described dentifrice composition comprises binding agent, surfactant, grinding agent, wetting agent and water, wherein:

(1) described grinding agent is a silicon oxide, described compositions also comprises silica thickener, and described compositions comprises silica thickener, following silica abrasive, 45-70 weight % water, 0.8-3.0 weight % surfactant, the 0.05-3.0 weight % binding agent of 15 weight % of 1-7 weight %; Perhaps

(2) described grinding agent is a silicon oxide, described compositions also comprises silica thickener, described compositions comprises 2-22 weight % silicon oxide, 0.8-3.0 weight % surfactant, 0.05-3.0 weight % binding agent altogether, and described compositions also comprises the non-colloid microcrystalline Cellulose of about 0.1-8.0 weight %, colloid microcrystalline Cellulose or its mixture; Perhaps

(3) described binding agent is the calcio grinding agent, and described binding agent is a cellulose gum, and described compositions comprises the binding agent of 25-55 weight % calcio grinding agent, 35-60 weight % water, 0.8-3.0 weight % surfactant and 1.0-3.0 weight %.

Detailed Description Of The Invention

Unless have in addition described, the term grinding agent in description and claims, polishing agent, wetting agent, binding agent, microcrystalline Cellulose, colloid microcrystalline Cellulose, hydrocolloid, surfactant, spice, aromatic, sweetener, sweeting agent, antilubricant, abrasive (attriting agent) and similarly term also comprise this mixtures of material.Unless have describedly in addition, all percents are in weight %.

Component

Described dentifrice composition comprises grinding agent or polishing agent, wetting agent, binding agent, surfactant, water and other optional material, and the conventional component of dentifrice composition normally is as spice and sweetener.Can have non-colloid microcrystalline Cellulose, colloid microcrystalline Cellulose or their mixture, this has reduced the abrasiveness of dentifrice composition.

The solid and the liquid component of preparation dentifrice composition make product, are extrudable paste material.Described binding agent or thickening agent produce viscosity, and required denseness and thixotropy is provided, and prevent described composition store with use in separate.Suitable thickening comprises cellulose derivative (" cellulose gum "), as carboxymethyl cellulose (CMC), methylcellulose, hydroxyethyl-cellulose, hydroxypropyl emthylcellulose and composition thereof, polyvinyl pyrrolidone, xanthan gum, carrageenin such as ι-carrageenin, κ-carrageenin, κ 2-carrageenin, λ-carrageenin and composition thereof, guar gum, karaya, arabic gum, tragacanth and composition thereof.The toothpaste that comprises carrageenin is as described in the U.S. Patent No. 6162418 of Randive, and its reference in content is incorporated in this.Hydrated silica and colloidal silica can be used as thickening agent.Silica thickener is as described in the U.S. Patent No. 6342205 of Niemi.

Described dentifrice composition comprises grinding agent (being also referred to as polishing agent).Suitable grinding agent or polishing agent comprise water-fast fine powder material, and it does not have water solublity or water solublity very low, and granularity is about 1-40 micron (diameter) usually, are more preferably to be about 2-20 micron (diameter), and have normal particle size distribution.It is active that these materials have polishing, do not have undue wear.General grinding agent comprises the calcio polishing agent, as dicalcium phosphate dihydrate (being known as dicalcium phosphate usually), tricalcium phosphate, calcium carbonate (as limestone, natural whiting or deposition Chalk), calcium pyrophosphate, calcium silicates and calcium aluminate, magnesium carbonate, magnesium phosphate, Polymeric sodium metaphosphate., amorphous silicon oxide, crystal silicon oxide, cvd silicon oxide, Smecta, aluminium hydroxide, aluminosilicate, bentonite, Talcum, aluminium oxide, silicon oxide xerogel and composition thereof.Be that grinding agent is dicalcium phosphate, calcium carbonate and silicon oxide better.

Non-colloid microcrystalline Cellulose, colloid microcrystalline Cellulose or its mixture can be added in the dentifrice composition, to reduce its abrasiveness.These materials reduce the relative quantity (in solid total in the dentifrice composition) of grinding agent in the dentifrice composition, reduce its abrasiveness thus.

Non-colloid microcrystalline Cellulose (being commonly referred to microcrystalline Cellulose or MCC) is the cellulose of the part depolymerization of purification.Hydrolysing step prepares described in U.S. Patent No. 3539365 that this can be by for example Durand and the U.S. Patent No. 2978446 of Battista.In this step, cellulose source (better being the alpha-cellulose that is from the pulp form of fibrous plant) is used mineral acid, better is that hydrochloric acid is handled.Then, the aggregates of crystallites of separating obtained microcrystalline Cellulose from reactant mixture, and the by-product of degraded is removed in washing.The gained material (comprising 40-60 weight % water usually) that wets is called the wet cake of hydrocellulose, microcrystalline Cellulose, microcrystalline Cellulose or is called wet cake simply.Described steam explosion technology (wood flour or other cellulosic material are placed cavity, introduce superheated steam to described cavity) is as described in the U.S. Patent No. 5769934 of Ha.

The particulate granularity of non-colloid microcrystalline Cellulose is usually less than about 100 microns, about usually 20-100 micron.Measure as Horiba Cappa 700 particle size analyzers, the particulate particle mean size of described colloid microcrystalline Cellulose is about the 0.1-8 micron, and better about 0.1 to less than about 1.0 microns, is more preferably about 0.1-0.9 micron, preferably about 0.1-0.6 micron.Usually, particle size distribution all is suitable arbitrarily, as long as particle mean size within the required range, the particle mean size that better is trickle crystalline cellulose element (being colloidal basically) is less than about 10 microns.

Granularity by reducing microcrystalline Cellulose and stable abrasive grains make the colloid microcrystalline Cellulose thus to avoid forming hard aggregation.The technology that reduces the microcrystalline Cellulose granularity is disclosed in the U.S. Patent No. 6391368 of the U.S. Patent No. 6037080 of the U.S. Patent No. 6025037 of the U.S. Patent No. 3539365 of Durand, Krawczyk, Venables and Tuason and WO 03/09676.

In described dentifrice composition, can use the colloid microcrystalline Cellulose of processing together with surfactant.The HLB of " surfactant " (hydrophilic) is about 1-40.The method of the colloid microcrystalline Cellulose that preparation processes with surfactant is disclosed in the U.S. Patent No. 6025007 of the U.S. Patent No. 5736177 of for example McGinley and Krawczyk.Known many surfactants.Useful surfactant comprises for example lecithin; the monoglyceride class; di-glycerides; acetylated monoglycerides; the ethoxylation monoglyceride; sorbitan ester; sucrose ester; the monostearate esters; monoglyceride or di-glycerides; comprise that acid is as acetic acid; the ester of lactic acid and succinic acid; and comprise the diacetyl tartrate of monoglyceride and di-glycerides; propylene glycol monoester; the fatty acid polyglycol glycerine ester; Polysorbate; stearin-based lactate (lactylate) and ethoxylate; the sulfate of sulfate and alkylol ethoxylate (wherein; alkyl comprises about 8-18 carbon atom), as sodium hexadecyl sulfate; sodium lauryl sulfate (SLS) and lauryl disodium sulfosuccinate.Passable with the colloid microcrystalline Cellulose that stearin-based lactate is processed together

SD 1340 buys from FMCCorporation.

The surfactant of processing together with microfibre of the plain and about 5-40 weight % of the trickle crystalline cellulose that the described altogether microcrystalline Cellulose of processing can comprise about 60-95 weight %, all percentage number averages are in the described gross weight that is total to rapidoprint.Be preferably, described microcrystalline Cellulose comprises the common rapidoprint of about 70-95 weight %.Be preferably, described surfactant comprises the common rapidoprint of about 5-30 weight %.Be that described surfactant comprises the common rapidoprint of about 10-30 weight % better.

In dentifrice composition, can use the colloid microcrystalline Cellulose of processing together with hydrocolloid.Suitable hydrocolloid comprises for example cellulose derivative, as carboxymethyl cellulose, hydroxypropyl cellulose, hydroxypropyl emthylcellulose and hydroxyethyl-cellulose, natural gum is as guar gum, Flos Robiniae Pseudoacaciae glue, arabic gum, xanthan gum, tragacanth and POLY-karaya, seaweed extract such as κ-carrageenin, κ 2-carrageenin, ι-carrageenin, λ-carrageenin and alginate, and the frumentum solid and the pectin of starch such as maltodextrin, hydrolysis.

Disclosing in the U.S. Patent No. 4980193 of Tuason and carboxymethyl cellulose (CMC), starch (better being the low starch of amylose content) and diluent, maltodextrin, milk surum or take off the dried milk solids of ester, better is the colloid microcrystalline Cellulose of processing together with maltodextrin.The colloid microcrystalline Cellulose of processing together with alginate is disclosed in the U.S. Patent No. 5366742 of Tuason.The colloid microcrystalline Cellulose of processing together with the low-viscosity alginates complex is disclosed in the U.S. Patent No. 5985323 of Augello.In the U.S. Patent No. 5192569 of McGinley, disclose and colloid microcrystalline Cellulose that galactomannan gum (as locust bean gum or guar gum) is processed together.In the U.S. Patent No. 6391368 of Tuason, disclose and colloid microcrystalline Cellulose that ι-carrageenin is processed together.And the colloid microcrystalline Cellulose processed together of sodium carboxymethyl cellulose (MCC/CMC) with

RC-591 buys from FMC Corporation.

Disclose the colloid microcrystalline Cellulose of processing with hydrocolloid such as carrageenin and water soluble salt in the WO03/096976 of Tuason (PCT/US03/15146), its reference in content is incorporated in this.The described colloid microcrystalline Cellulose of processing together stands high shear forces power by the highly filled mixture that makes microcrystalline Cellulose and hydrocolloid in the presence of antilubricant and prepares.Though described antilubricant can be any water soluble salt basically, preferred antilubricant is as sodium chloride, potassium chloride, calcium lactate, Calcium d-tartrate, calcium citrate or single calcium phosphate, especially calcium chloride.Described hydrocolloid can be used as dry powder and adds.In the course of processing, importantly evenly adding described salt before moistening and the swelling hydrocolloid powder.Described particulate particle mean size is measured as mentioned above less than 10 microns.When described hydrocolloid was carrageenin, the particulate granularity at least about 50% was less than 3.5 microns.When described hydrocolloid was hydrocolloid except that carrageenin, the particulate granularity at least about 30% was less than 3.5 microns.When described hydrocolloid was carrageenin and another colloidal combination, the particulate granularity at least about 20% was less than 3.5 microns.

The colloid microcrystalline Cellulose of can use in dentifrice composition processing with hydrocolloid and abrasive.Suitable hydrocolloid as mentioned above.Suitable abrasive comprises calcium carbonate (limestone, Chalk), dicalcium phosphate, tricalcium phosphate, zinc carbonate, zinc hydroxide, magnesium phosphate, brium carbonate, barium sulfate, ferrous carbonate, aluminium hydroxide, magnesium hydroxide and aluminum magnesium hydroxide.Other material as the friction auxiliary agent comprises silicon oxide, various clay, silicate, silicon dioxide, Talcum, titanium dioxide and partly soluble organic material, as lactose.Preferred abrasive comprises calcium carbonate, dicalcium phosphate and silicon oxide, and they can be as the grinding agent in the dentifrice composition.The method of the colloid microcrystalline Cellulose of processing with hydrocolloid and abrasive has been described in the U.S. Patent No. 6037380 of for example Venable.

The weight ratio of described microcrystalline Cellulose and abrasive is about 85: 15 to 30: 70 usually, is more preferably to be about 70: 30 to 40: 60.Described hydrocolloid is about the 5-30 weight % of microcrystalline Cellulose usually, better 5-15 weight %; The weight ratio that is microcrystalline Cellulose and hydrocolloid is about 95: 5 to 70: 30.

When the granule of abrasive has suitable granularity, and the ratio of microcrystalline Cellulose and abrasive is when dropping in the suitable scope, can by use abrasive and and the mixture of the microcrystalline Cellulose processed together of hydrocolloid reach equal result.As mentioned above, the particulate suitable particle size of described abrasive is the particle mean size of 0.1-8 micron, better is about 0.1 to 8 micron, better about 0.1 arrive less than about 1.0 microns, better about 0.1-0.9 micron, preferably about 0.1-0.6 micron is determined as Horiba Cappa 700 particle size analyzers.For the mixture of microcrystalline Cellulose and abrasive, the approrpiate wts of described microcrystalline Cellulose and abrasive ratio is about 95: 5 to 5: 95, is generally 90: 10 to 30: 70, better normally about 85: 15 to 55: 45.

The excipient of described dentifrice composition is that the oral cavity is acceptable, comprises water and wetting agent.Described wetting agent provides mouthfeel, prevents that also dentifrice composition from becoming dry.General wetting agent is polyhydric alcohol of 3-6 carbon atom and composition thereof, and wherein, each carbon is hydroxylated, for example glycerol, sorbitol, Polyethylene Glycol, polyoxyethylene glycol, mannitol, xylitol and other sugar alcohol.Preferred sorbitol and glycerol.The better deionization of described water, and free from foreign meter.

Dentifrice composition also comprises surfactant, is used for emulsifying or otherwise disperses toothpaste component equably.Described surfactant is anion or non-ionic surface active agent or their mixture normally.The example of suitable surfactant comprises water soluble salt, higher alkyl sulfates, senior alkyl arylsulphonate, the senior alkyl sulfosalicylic acetate, 1 of sulfate mono higher fatty acids monoglyceride; basically the saturated higher aliphatic acyl group amide-type of the high-grade aliphatic ester of 2-dihydroxypropane sulfonate, lower aliphatic amino carboxylic acid compounds (as having those of 12-16 carbon atom in fatty acid, alkyl or the acyl group), higher alkene sulfonate, poly-lower alkoxy (3-100 alkoxyl) sulfate of senior alkyl, and fatty acid soaps.These examples of anionic surfactants comprise sodium lauryl sulfate (SLS), hydrogenation fatty acid distribution of coconut oil monoglyceride sulfate mono sodium, dodecylbenzene sodium sulfonate, lauryl sulfoacetate sodium, N-lauryl sarcosine (sarcosinate) sodium and coconut oil (cocate) sodium.Suitable ionic surfactant pack is drawn together rudimentary epoxyalkane, as the chain of oxirane and expoxy propane.Surfactant commonly used is a sodium lauryl sulfate.

Described dentifrice composition can comprise many other optional ingredients.Can there be the reagent that treatment or dressing effect are provided, as enamel sclerosing agent, tartar controlling agent, brightening agent and antibacterial.In order to satisfy consumer, can add one or more sweeteners and spice.Also can there be other material, as opacifier and coloring agent as the conventional component of dentifrice composition.

The example of spice (spice, aromatic material or aromatic) comprises menthol, carvone, anethole, methyl salicylate, and the oil of spearmint, Mentha arvensis L. syn.M.haplocalyxBrig, Ilicis Purpureae, sassafrases, Flos Caryophylli, Salvia japonica Thunb., Eucalyptus, Adeps Bovis seu Bubali, Cortex Cinnamomi, Fructus Citri Limoniae, Citrus aurantium Linn., Fructus Vitis viniferae, Fructus Fortunellae Margaritae, Fructus Kaki and Fructus Citri junoris.The example of sweetener (sweeting agent) comprises sucrose, lactose, maltose, sorbitol, xylitol, ring sodium sulfonate, perillartine, L-aspartyl-L-phenyl methyl lactamine (LaspartylLphenylalanine methylester) and glucide.In dentifrice composition, can exist pyrophosphate (having the anti-calculus effect) as pyrophosphoric acid two alkali metal salts or four alkali metal salts, as Na ₄P ₂O ₇(TSPP), K ₄P ₂O ₇, Na ₂K ₂P ₂O ₇, Na ₂K ₂H ₂O ₇And Na ₂H ₂P ₂O ₇, long-chain polyphosphate such as sodium hexameta phosphate and ring-type phosphate such as sodium trimetaphosphate.The example of sclerosing agent is a fluoride salt, as sodium fluoride, potassium fluoride, calcium fluoride, zinc fluoride, stannous fluoride, ammonium fluoride zinc, sodium monofluorophosphate, single fluorophosphoric acid potassium and hydrofluorination lauryl amine.

In dentifrice composition, also comprise antibacterial.What be particularly useful is non-cationic germicide, it is based on phenol and bisphenol compound, halogenated diphenyl ether, benzoate and diphenylcarbamide such as sodium benzoate, 4-chlorophenol, 2,2 '-three chloro-2-hydroxyl-diphenyl ethers (triclosan), the esters of hydroxy benzoic acid, especially methyl ester, ethyl ester (ethyl parasept), propyl ester (propyl group parasept), butyl ester (butyl parasept) and benzyl ester, 3,4,4 '-neko (carbanalide) and 3,3 ', the 4-neko.Preferred microbicide is a triclosan.Also can use nonionic microbicide such as sesquiterpene alcohols, as merolidol and bisabolol.

In dentifrice composition, there is brightening agent.Useful brightening agent is an oxidant, as calper calcium peroxide, urea peroxide, peracetic acid and SODIUM PERCARBONATE.Can add opacifier such as titanium dioxide, make toothpaste opaque, perhaps improve its opacity.

Described dentifrice composition also comprises other composition, and the conventional component for dentifrice composition comprises the desensitizer that for example is used for dentin hypersensitiveness, as Chile saltpeter; The acceptable pigment in oral cavity is as beta-carotene, chlorophyll, FD﹠amp; C yellow #5, FD﹠amp; C yellow #6, FD﹠amp; C blue #2, FD﹠amp; The red #4 of C, FD﹠amp; The green #6 of C, FD﹠amp; C yellow #10, FD﹠amp; The red #40 of C, D﹠amp; The green #5 of C, D﹠amp; C red #30 lake and FD﹠amp; The blue #1 lake (lake) of C; Therapeutic agent such as rose-seed oil; Chelating agen such as citrate; Vitamin such as vitamin C and vitamin E; Aminoacid; Protein; Antibiotic; Antienzyme; Enzyme; PH controlling agent (buffer agent); Antioxidant and antiseptic.

Compositions

In the gross weight of described dentifrice composition, described dentifrice composition comprises the binding agent of about 0.05-3.0 weight % usually.Compare the situation when using cellulose derivative such as carboxymethyl cellulose, when using carrageenin or xanthan gum, need less binding agent usually as binding agent as binding agent.When using cellulose derivative such as carboxymethyl cellulose as binding agent, described binding agent comprises about 0.25-3.0 weight %, the dentifrice composition of better about 1.0-1.5 weight % usually.When using carrageenin or carrageenin mixture as binding agent, described binding agent comprises the carrageenin of about 0.05-2.5 weight % usually.The method for preparing the low toothpaste of carrageenin content is disclosed in the U.S. Patent No. 6187293 (its reference in content is incorporated in this) of Ballard.

Toothpaste of the present invention is the high toothpaste of water content.The water yield that exists in described " dentifrice composition that water content is high " depends on grinding agent used in the dentifrice composition to a certain extent.In dentifrice composition, can use more high-load calcio grinding agent, as dicalcium phosphate and calcium carbonate and the silicon oxide of low content more.Therefore, the silica-based dentifrice composition that water content is high comprises more water than the dentifrice composition that comprises the calcio grinding agent usually.Illustrated to comprise ι-carrageenin as high toothpaste of the water content of binding agent and preparation method thereof in the U.S. Patent No. 6159446 of for example Randive, its reference in content is incorporated in this.

In dentifrice composition, can use two kinds of silicon oxides.Silicon oxide is as grinding agent.Example is 113,

115, 124 Hes

623 (J.M.Huber Co., Edison, NJUSA).Silicon oxide is also as viscosifier.Example is

165,

163 Hes

153 (J.M.Huber Co., Edison, NJ USA).In the U.S. Patent No. 6342202 of Niemi, provided the proportional difference between these two kinds of materials, especially in table B and C.The disclosure of U.S. Patent No. 6342202 is with reference to being incorporated in this.

Have been found that to prepare the high toothpaste of water content, it comprises less than 8%, and 7 weight % or following normally are more preferably the silica thickener of 1-7 weight %.The abrasiveness of this dentifrice composition is lower than the dentifrice composition that comprises 8-15 weight % silica thickener.In addition, described dentifrice composition comprises less than 15%, 1 to less than 15 weight %, is the silica abrasive of 6-10 weight % in some cases.The total amount of the silicon oxide that exists is 2-22 weight %, in some cases, 8-18 weight %, the silicon oxide total amount is 10-14% in other cases.

The abrasiveness that comprises the dentifrice composition of silicon oxide can usually reduce by microcrystalline cellulose, and described dentifrice composition includes but not limited to the above-mentioned high dentifrice composition of water content that comprises silicon oxide.When existing, gross weight in described dentifrice composition, have about 0.1-8.0 weight % in the described dentifrice composition, normally about 0.2-4 weight % is more preferably non-colloid microcrystalline Cellulose, colloid microcrystalline Cellulose or their mixture of about 0.3-2.0 weight % and 0.4-1.6 weight %.This has reduced the relative quantity of grinding agent in the dentifrice composition, in the solid amount in the dentifrice composition, reduces its abrasiveness thus.

Water accounts for the 45-70 weight % of the high dentifrice composition of the water content that comprises silicon oxide.Described water content can be the 50-70 weight % and the 60-70 weight % of described dentifrice composition gross weight.

" gained " viscosity (that is, the viscosity of compositions or " initial viscosity " after being cooled to room temperature but before leaving standstill more than several hours) that comprises the high dentifrice composition of the water content of silica abrasive is usually less than 200000cp.The viscosity of gained dentifrice composition is about 80000 to 180000cp usually, is more preferably about 100000 to 165000cp, even is about 120000 to 155000cp usually.This scope is usually used in the automatic stuffing apparatus.

When using dicalcium phosphate (DCP) as grinding agent, described dentifrice composition comprises about 25-55 weight % usually, is more preferably the dicalcium phosphate of about 35-53 weight %.When using calcium carbonate as grinding agent, described compositions comprises about 25-55 weight % usually, is more preferably the calcium carbonate of about 35-50 weight %.Therefore, because abrasive levels is higher, so the water yield in the high dentifrice composition of these water contents is less than the dentifrice composition that comprises silicon oxide.The dentifrice composition that these water contents are high comprises 35-60 weight % water, better 40-60 weight % water.Described binding agent is a cellulose gum, better is carboxymethyl cellulose, about usually 1.0-3.0 weight %.There is silica thickener, for example about at the most 7 weight %, as 1.0-7.0 weight %, usually under the situation of about 1.0-4.0 weight % silica thickener, perhaps there are silica thickener and microcrystalline Cellulose, for example 0.5-7.0 weight %, silica thickener and the 0.5-10.0 weight % of 0.5-2.0 weight % usually, usually under the situation of the non-colloid microcrystalline Cellulose of 1.0-3.0 weight %, colloid microcrystalline Cellulose or its mixture, can reduce the amount of described binding agent.

As calculated after grinding agent, water, binding agent and other composition, wetting agent just occupies the surplus of material.Usually, when the water yield increased, the amount of wetting agent just reduced in the dentifrice composition.Described dentifrice composition comprises about 8-45 weight % wetting agent, and about usually 10-25 weight % is in absolute quantity.Prepared the dentifrice composition that comprises 10-15 weight % wetting agent (in absolute quantity).Sorbitol for example can 70% sorbitol/30 weight % water mixture buy." in absolute quantity " is meant the amount of wetting agent, gets rid of all water that exist in the wetting agent.

Described dentifrice composition comprises about 0.8-3.0 weight %, the surfactant of better about 1.0-2.0 weight % usually.When having spice, described dentifrice composition comprises about 0.1-2.0 weight % usually, is more preferably the spice of about 0.5-1.5 weight %.When having sweetener, described dentifrice composition comprises the sweetener of about 0.1-2 weight % usually.When having anticalculus agents, the anticalculus agents of the about usually 0.5-8.0 weight of described dentifrice composition %.When having antibacterial, described dentifrice composition comprises the antibacterial of 0.03-1 weight % usually.When having brightening agent, described dentifrice composition comprises about 0.1-5 weight % usually, better about 0.5-2 weight % brightening agent.When having pyrophosphate, described dentifrice composition comprises about 0.5-8.0 weight %, the pyrophosphate of better about 1.5-3 weight % usually.When having sclerosing agent, it accounts for about 0.1-5 weight % of described dentifrice composition usually.When existing, other composition exists with effective dose, as dyestuff and opacifier, promptly exist to obtain each composition of its concrete application purpose institute necessary amounts.

The preparation of toothpaste

Described dentifrice composition uses thermal process or environmental technology to prepare, and can use discontinuous method or continuation method.Described environmental technology is sometimes referred to as cold technology.For example, described described thermal process in the U.S. Patent No. 6,187,293 of the U.S. Patent No. 4,353,890 of Scott and Ballard, its reference in content is incorporated in this.For example, in the U.S. Patent No. 6,187,293 of Ballard, the continuous preparation method of toothpaste is especially disclosed in Fig. 1 and the adnexa, its reference in content is incorporated in this.The continuation method of preparation toothpaste is disclosed in the U.S. Patent No. 5236696 of Catiis.The example that can be used to prepare the thermal process of dentifrice composition provides as embodiment.The step (2) of the technology that provides and (3) are carrying out under about 25 ℃ in embodiment, and described environmental technology is identical with thermal process.

Industrial applicability

Dentifrice composition of the present invention can be used for oral hygiene.

Advantage character of the present invention illustrates with reference to following examples, but this is used to limit the present invention anything but.

Embodiment

Nomenclature

CL611 colloid microcrystalline Cellulose and sodium carboxymethyl cellulose, ratio are 85/15 (weight

Amount), (FMC Philadelphia PA USA)

The non-colloid microcrystalline Cellulose of PH102, (FMC Philadelphia PA USA)

The non-colloid microcrystalline Cellulose of PH105, (FMC Philadelphia PA USA)

The colloid microcrystalline Cellulose that RC-591 and sodium carboxymethyl cellulose are processed together, ratio is

89/11 (weight), (FMC Philadelphia PA USA)

Commercially available other carboxymethyl cellulose of medium-viscosity level of CMC

The DCP dicalcium phosphate dihydrate often is called dicalcium phosphate

MCC

PH101, particle mean size is the non-colloid crystallite of 50-100 micron

Cellulose powder, (FMC Philadelphia PA USA)

MCC/CMC The colloid that RC-591 and sodium carboxymethyl cellulose are processed together is little

The crystalline cellulose element, (FMC Philadelphia PA USA)

The colloid microcrystalline Cellulose that MCC/SLS and sodium lauryl sulfate are processed together

MCC/CMC/CaCO ₃The colloid microcrystalline Cellulose of processing together with carboxymethyl cellulose and calcium carbonate

The SLS sodium lauryl sulfate

The SMFP sodium monofluorophosphate

TP 399 mainly comprises the binding agent of ι-carrageenin mixture, and Brookfield viscosity is

20-50cp (in 75 ℃ of following deionized waters, measuring under 1.5% solid), (FMC

Philadelphia PA USA)

113 amorphous silicon oxide (J.M.Huber, Edison NJ as grinding agent

USA)

165 amorphous silicon oxide (J.M.Huber, Edison NJ as thickening agent

USA)

General step

Raw material

In using the embodiment of sorbitol, described sorbitol is 70% aqueous solution, make the water content of dentifrice composition equal to show shown in water add the total amount of 30% water in the sorbitol.

Sample preparation

Use full-boiled process to prepare described dentifrice composition according to following steps:

(1) with high speed agitator binding agent and colloid microcrystalline Cellulose are distributed in the wetting agent, and stir about 10 minutes for example, gel formed.

(2) then, described water can be heated to about 80 ℃, and is continuing to add wetting agent and binding agent/colloid microcrystalline cellulose mixt under 15 minutes the condition of stirring, and described temperature remains on 60-70 ℃ simultaneously.

(3) do mixed described dried composition, as (eliminating grinding agents) such as saccharin sodium, sodium benzoate.Described doing mixed in the thing stirring adding binding agent serosity, and stirs 15 minutes, and simultaneous temperature remains on 60-70 ℃.

(4) gained gel (elixir) is transferred to the low speed Ross with vacuum accessory ^TMIn the blender.Described Ross ^TMBlender is two oar mixture of dual planetary gear, operation under per minute 20-100 changes, and can operate in a vacuum.

(5) described grinding agent (polishing agent) adds in the elixir successively, and mixes 15 minutes down at vacuum condition (720mmHg at least).

(6) spice is added in the elixir, and in the Ross blender, under the vacuum condition, mixed 10 minutes.

(7) described surfactant is added as sodium lauryl sulfate (SLS) as described in the mixture, and under vacuum condition, continue to mix 20 minutes.

(8) sample is extracted out, tested, batch of material is discharged to fills in pipe or other disperser.

Viscosity measurement

The Brookfield DVII viscometer that the Helipath adnexa is equipped with in use is according to the viscosity of measuring dentifrice composition with the T-E spindle at 5rpm as described below: in method A, described sample is in the following balance of ambient temperature (23 ℃), in method B then 25 ℃ of following balances.By spindle is directly put into the dentifrice composition that comprises 30-40g, and measure viscosity according to method A according to the paste that method B infiltrates in the pipe spindle.

Method A: fixed spindle is placed sample.Open described viscometer, and in 1 minute, write down reading, obtain totally 6 readings, be averaged then every 10 seconds.

Method B: spindle is placed the top slightly of sample surfaces, and allow it to move down Helipath to enter in the sample.Observe described reading, further enter with spindle and begin in the sample to increase.When spindle still moved down can observe stable reading in the process time, write down the viscosity of described sample in 30 seconds.

The Cuban test

In Cuban test (being also referred to as " frame " test), under the condition that spacing increases, paste is extruded from pipe by fixing hole through the grid of parallel bars.Described result of the test is expressed as maximum space-number (number of 1-12), the ultimate range between the rod that expression support toothpaste ribbon can not rupture.Described is about 300 millimeters, wide about 100 millimeters.The spacing of described stainless steel bar increases gradually, and from 3mm (spacing number 1) between the rod 1 and 2, spacing increases 3mm at every turn between rod.Therefore, the spacing of rod between 2 and 3 is 6mm, and the distance between the 12nd and 13 rod (spacing number 12) is 39mm.For the not high toothpaste of water content, the grade of 1-2 and 9-12 is unacceptable, and 3 and 8 is acceptables, and 4-7 is good.

In order to carry out the Cuban test, carry out following steps:

(1) nozzle is fixed to be equipped with and waits to test in the dentifrice tube of dentifrice composition.

(2) pipe that the test dentifrice composition will be housed and have a nozzle with 45 ° fixed angle on rack device.Exerting pressure in bottom at pipe, extrudes uniform pasty state band from described pipe.When from pipe, extruding the pasty state band, described pipe with straight line across whole shelf.Usually about 2-4 of time second of pasty state band on the top of the shelf stretches.If band ruptured, then want repeating said steps before traversing whole shelf.

(3) band was left standstill 30 seconds.At this moment, the point of record band fracture is as shelf grade or Cuban value.

(4) carry out described exerting pressure 5 times, and the record average reading, be rounded to immediate integer.

Embodiment 1-3 and Comparative Examples 1 and 2

These embodiment show that microcrystalline Cellulose makes the high dentifrice composition of water content, and have good storage stability.Comparative Examples 1 is based on the standard toothpaste preparation of dicalcium phosphate polishing agent (DCP) and carrageenin binding agent.Its water content is lower, and does not have microcrystalline Cellulose.The dicalcium phosphate of Comparative Examples 2 is less, but does not have the dicalcium phosphate of microcrystalline Cellulose, embodiment 1-3 less, and comprises microcrystalline Cellulose.

Table 1

The toothpaste that comprises carrageenin and MCC

^aIdentical with water content

Dentifrice composition as described in described in general step, estimating.Measured viscosity is as shown in table 2.

Table 2

The toothpaste that comprises carrageenin and MCC

Storage stability	Comparative Examples 1 standard DCP	Comparative Examples 2 low DCP	Embodiment 1 low DCP	Embodiment 2 low DCP	Embodiment 3 low DCP
Storage stability	Comparative Examples 1 standard DCP	Comparative Examples 2 low DCP	Embodiment 1 low DCP	Embodiment 2 low DCP	Embodiment 3 low DCP	25℃
Initially						25℃
Initially						Cuban ^a	5	7	5	5	5
Cp	ND	155000	169000	ND	115000	Cuban ^a	5	7	5	5	5
Cp	ND	155000	169000	ND	115000	1 day
Cuban	5	5	4	5	5	1 day
Cuban	5	5	4	5	5	3 weeks
Cuban	ND	5	4	ND	5	3 weeks
Cuban	ND	5	4	ND	5	6 weeks
Cuban	ND	5	4	ND	5	6 weeks
Cuban	ND	5	4	ND	5	12 weeks
cp/Cuban	5	5	3	5	4	12 weeks
cp/Cuban	5	5	3	5	4	cp ^b	ND	141000	89000	ND	129000
Outward appearance	Well	Well	Thin	Well	Well	cp ^b	ND	141000	89000	ND	129000
Outward appearance	Well	Well	Thin	Well	Well	June
Cuban	5	5	2	5	3	June
Cuban	5	5	2	5	3	Outward appearance	Well	Well	Thin	Well	Thin
1 year						Outward appearance	Well	Well	Thin	Well	Thin
1 year						Cuban	5	ND	ND	4	ND
Outward appearance	Well	ND	ND	Well	ND	Cuban	5	ND	ND	4	ND
Outward appearance	Well	ND	ND	Well	ND	50℃
3 weeks						50℃
3 weeks						Cuban	ND	5	4	ND	4
6 weeks						Cuban	ND	5	4	ND	4
6 weeks						Cuban	ND	5	4	ND	4
12 weeks						Cuban	ND	5	4	ND	4
12 weeks						cp/Cuban	6	5	3	5	5
cp ^b	ND	131000	88000	ND	129000	cp/Cuban	6	5	3	5	5
cp ^b	ND	131000	88000	ND	129000	Outward appearance	Well	Well	Thin	Well	Well

The ND=undetermined

^aThe viscosity of the dentifrice composition of representing with Cuban

^bDentifrice composition viscosity in cp

Comparative Examples 2 shows that the toothpaste that abrasiveness is less and water content is high that does not contain microcrystalline Cellulose is reduced to 5Cuban one day medium viscosity from 7cuban.Embodiment 1-3 shows that the preparation that comprises microcrystalline Cellulose makes the dentifrice composition of low abrasiveness, its water content height, and have good long-time stability.

As the MCC/CMC/CaCO that uses 50: 50 ₃Can obtain identical result when replacing MCC in embodiment 1-3 with the mixture of MCC.

Embodiment 4 and 5 and Comparative Examples 3

This embodiment has proved the ability with the high silicon oxide dentifrice composition of microcrystalline Cellulose preparation water content.Dentifrice composition shown in the table 3 prepares as mentioned above.The result is as shown in table 4.

Table 3

The silica-based toothpaste that comprises carrageenin and MCC

Table 4

The silica-based toothpaste that comprises carrageenin and MCC

Storage stability	Comparative Examples 3	Embodiment 4	Embodiment 5
Storage stability	Comparative Examples 3	Embodiment 4	Embodiment 5	25℃
Initial				25℃
Initial				Cuban ^a	4	2	2
1 day				Cuban ^a	4	2	2
1 day				Cuban	4	3	3
12 weeks				Cuban	4	3	3
12 weeks				Cuban	5	7	8
Outward appearance	Well	Well	Well	Cuban	5	7	8
Outward appearance	Well	Well	Well	June
Cuban	4	5	5	June
Cuban	4	5	5	Outward appearance	Well	Well	Well
50℃				Outward appearance	Well	Well	Well
50℃				12 weeks
Cuban	5	7	8	12 weeks
Cuban	5	7	8	Outward appearance	Well	Well	Well

As the MCC/CMC/CaCO that uses 50: 50 ₃Can obtain identical result when replacing MCC in embodiment 4 with the mixture of MCC.

Embodiment 6 and 7 and Comparative Examples 4

This embodiment has proved the ability with the higher silicon oxide ointment composition of microcrystalline Cellulose preparation water content.Dentifrice composition shown in the table 5 prepares as mentioned above.The result is as shown in table 6.

Table 5

The silica-based toothpaste that comprises carrageenin and MCC

Dentifrice composition shown in the embodiment 5 and 6 is the high compositions of water content, and it comprises 14% silicon oxide.

Embodiment 8 and 9 and Comparative Examples 5

This embodiment has proved the ability with the high silicon oxide dentifrice composition of microcrystalline Cellulose preparation water content.Dentifrice composition shown in the table 6 prepares as mentioned above.

Table 6

The silica-based toothpaste that comprises CMC and MCC

^aThe viscosity of dentifrice composition is in cuban.

Embodiment 10-15

These embodiment are presented at can various binding agents in the dentifrice composition of the present invention.Prepare following dentifrice composition, and estimate as mentioned above.Embodiment 10-15 is the dentifrice composition that also comprises carrageenin, carboxymethyl cellulose or xanthan gum/carboxymethyl cellulose as binding agent respectively except that microcrystalline Cellulose.Embodiment 10,12 and 14 also comprises microcrystalline Cellulose.

Table 7

The silica-based toothpaste that comprises carrageenin/CMC

Table 8

The silica-based toothpaste that comprises CMC

Table 9

The silica-based toothpaste that comprises xanthan gum/CMC

Embodiment 16-18

These embodiment have illustrated microcrystalline Cellulose and have processed the application of colloid microcrystalline Cellulose in the high dentifrice composition of water content altogether.Use the above step, the dentifrice composition shown in preparation and the evaluation table 10.

Table 10: the dentifrice composition that water content is high

Embodiment 19

The application of the colloid microcrystalline Cellulose that this embodiment explanation and hydrocolloid and abrasive are processed together in the high dentifrice composition of water content.Except using 0.5%MCC/CMC/CaCO ₃Replacement 0.5%

Beyond the PH 105, prepare dentifrice composition as described in example 16 above.The preparation initial viscosity is about the dentifrice composition of 12000-140000cps.When storing 6 months down for 25 ℃, described dentifrice composition is stable.

Embodiment 20

The application of colloid microcrystalline Cellulose in the high dentifrice composition of water content that this embodiment explanation and surfactant are processed together.Except using 0.5%MCC/SLS to replace 0.5% Beyond the PH 105, prepare dentifrice composition as described in example 16 above.The preparation initial viscosity is about the dentifrice composition of 12000-140000cps.When storing 6 months down for 25 ℃, described dentifrice composition is stable.

Embodiment 21 and 22

The application of colloid microcrystalline Cellulose in the high dentifrice composition of water content that this embodiment explanation and carrageenin are processed together.Except using 0.5% and the colloid microcrystalline Cellulose processed together of carrageenin (described in the U.S. Patent No. 6391368 of Tuason) replacement 0.5%

When using and colloid microcrystalline Cellulose replacement 0.5% that carrageenin (as the WO03/096976 of Tuason) is processed together

Can obtain identical result during PH 105.

Embodiment 23

The microcrystalline Cellulose that this embodiment explanation is processed with carrageenin and the application of mixture in the high dentifrice composition of water content of colloid microcrystalline Cellulose.Except using 0.25% and the colloid microcrystalline Cellulose processed together of carrageenin (described in the U.S. Patent No. 6391368 of Tuason) and 0.25%

PH 105 replacements 0.5%

When using 0.25%MCC/CMC/CaCO ₃With 0.25%

PH 105 replacements 0.5%

During PH 105, when using 0.25%MCC/SLS and 0.25%

PH 105 replacements 0.5%

During PH 105, and when using the 0.25% colloid microcrystalline Cellulose and 0.25% with carrageenin (as the WO03/096976 of Tuason) processing

PH 105 replacements 0.5%

Can obtain identical result during PH 105.

Embodiment 24-26

These embodiment have illustrated microcrystalline Cellulose and the application of colloid microcrystalline Cellulose in the high dentifrice composition of water content of processing altogether.Use above-mentioned steps, can prepare and the dentifrice composition shown in the evaluation table 11.

Table 11

The dentifrice composition that water content is high

Embodiment 27

Beyond the PH 105, prepare dentifrice composition as described in example 24 above.The preparation initial viscosity is about the dentifrice composition of 15000-160000cps.When storing 6 months down for 25 ℃, described dentifrice composition is stable.

Embodiment 28

The application of colloid microcrystalline Cellulose in the high dentifrice composition of water content that this embodiment explanation and surfactant are processed together.Except using 0.5%MCC/SLS to replace 0.5%

Embodiment 29 and 30

Can obtain identical result during PH 105.

Embodiment 31

The microcrystalline Cellulose that this embodiment explanation is processed with carrageenin and the application of mixture in the high dentifrice composition of water content of colloid microcrystalline Cellulose.Except using 0.25% and the colloid microcrystalline Cellulose processed together of carrageenin (described in the U.S. Patent No. 6391368 of Tuason) and 0.25% PH 105 replacements 0.5%

When using 0.25%MCC/CMC/CaCO ₃With 0.25%

PH 105 replacements 0.5%

During PH 105, when using 0.25%MCC/SLS and 0.25% PH 105 replacements 0.5%

PH 105 replacements 0.5%

Can obtain identical result during PH 105.

Embodiment 32

The present invention has illustrated the application of κ-carrageenin in the high dentifrice composition of the water content with silicon oxide.

Table 12

In this dentifrice composition, can use

PH 105 microcrystalline Cellulose replace The PH102 microcrystalline Cellulose.

Embodiment 33 and 34

This embodiment has said the application of mixture in the high dentifrice composition of water content of xanthan gum and carboxymethyl cellulose.

Table 13

The silica-based toothpaste that comprises carrageenin

Embodiment 35-40

These embodiment have illustrated the Chalk (calcium carbonate) that comprises as grinding agent and as the high toothpaste of water content of the carboxymethyl cellulose of binding agent.

Table 14

The toothpaste that comprises calcium carbonate

Table 15

The toothpaste that comprises calcium carbonate

Table 16

The toothpaste that comprises calcium carbonate

The present invention has been described, now our claimed the following stated and content of equal value thereof.

Claims

1. dentifrice composition, described compositions comprises:

Binding agent, surfactant, grinding agent, wetting agent and water; Wherein,

Described grinding agent is a silica abrasive; Described compositions also comprises silica thickener, and described compositions comprises the silica thickener of 1-7 weight %, the silica abrasive that is less than 15 weight %, 45-70 weight % water, 0.8-3.0 weight % surfactant, 0.05-3.0 weight % binding agent, and described binding agent is not a microcrystalline Cellulose; Described compositions also comprises non-colloid microcrystalline Cellulose, colloid microcrystalline Cellulose or its mixture of 0.1-8.0 weight %.

2. compositions as claimed in claim 1 is characterized in that described compositions comprises the water of 50-70 weight %.

3. compositions as claimed in claim 1 is characterized in that described compositions comprises the water of 60-70 weight %.

4. as each described compositions of claim 1-3, it is characterized in that, described compositions make viscosity less than 200,000cp.

5. compositions as claimed in claim 4 is characterized in that, the viscosity that makes of described compositions is 80,000-180,000cp.

6. compositions as claimed in claim 5 is characterized in that, the viscosity that makes of described compositions is 120,000-155,000cp.

7. as each described compositions of claim 1-3, it is characterized in that described binding agent is selected from carrageenin, cellulose gum and xanthan gum.

8. as each described compositions of claim 1-3, it is characterized in that the content of described non-colloid microcrystalline Cellulose, colloid microcrystalline Cellulose or its mixture is 0.2-4.0 weight %.

9. compositions as claimed in claim 5 is characterized in that, the content of described non-colloid microcrystalline Cellulose, colloid microcrystalline Cellulose or its mixture is 0.2-4.0 weight %.

10. compositions as claimed in claim 6 is characterized in that, the content of described non-colloid microcrystalline Cellulose, colloid microcrystalline Cellulose or its mixture is 0.2-4.0 weight %.

11. compositions as claimed in claim 7 is characterized in that, the content of described non-colloid microcrystalline Cellulose, colloid microcrystalline Cellulose or its mixture is 0.2-4.0 weight %.

12., it is characterized in that described compositions also comprises spice and sweetener as claim 1,2 or 3 described compositionss.