CN1105139C - Dispersible water-soluble or water-swellable polymers and process for making toothpastes containing them - Google Patents
Dispersible water-soluble or water-swellable polymers and process for making toothpastes containing them Download PDFInfo
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- CN1105139C CN1105139C CN97121750A CN97121750A CN1105139C CN 1105139 C CN1105139 C CN 1105139C CN 97121750 A CN97121750 A CN 97121750A CN 97121750 A CN97121750 A CN 97121750A CN 1105139 C CN1105139 C CN 1105139C
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Abstract
The present invention provides a composition comprising a granular water-soluble or water-swellable polymer which is processed by at least one kind of polylol and is partially agglomerated at least. The content of the polylol is higher than about 10 wt% by measuring the total weight of the composition. Compared with a water-soluble or water-swellable polymer which is not processed, the granular water-soluble or water-swellable polymer which is processed by the polylol and is partially agglomerated at least can be quickly hydrated into a water containing solvent, and can not form polymer agglomerate. The present invention also provides an improved method for preparing a toothpaste composition comprising at least one dry water-soluble or water-swellable polymer, and the method is improved by that the granular water-soluble or water-swellable polymer which is processed by the polylol and is partially agglomerated at least is used for replacing dry water-soluble or water-swellable polymers.
Description
The present invention relates to contain through polyvalent alcohol and handle and by the composition of agglomerant water-soluble or water-swellable polymer, and the application of this composition in preparation toothpaste.
Usually contain the acceptable abrasive of tooth, wetting agent, water in the formulation of tooth-paste and as the thickening material of said components and the water-soluble polymers of tackiness agent.Also use a spot of other various components, for example flavouring agent, sweeting agent, sanitas and fluorochemical.Glycerol and sorbyl alcohol (the normally aqueous solution) are the most frequently used toothpaste wetting agents, and simultaneously required according to product characteristic also can add polyoxyethylene glycol or propylene glycol.That generally produces has two types toothpaste: 1) paste or opaque gel; 2) transparent or semitransparent gel.
It is the most frequently used that what make toothpaste thickening material or tackiness agent is carboxymethyl cellulose (CMC), Natvosol (HEC), silicon-dioxide and neusilin.Also can use carrageenin, xanthan gum and polyacrylic ester, but general inadequately.
In the process of preparation toothpaste, often encounter difficulties when being incorporated into the water-soluble binder polymkeric substance of doing in the composition, because the polymkeric substance of doing adds and when being distributed in the water solution system, form agglomerate easily.This has increased hydrated body or the required time of dispersion that obtains uniform binder polymer.Therefore, in a kind of method of mixing the water-soluble binder polymkeric substance of industrial needs, this method can obtain not have the product of agglomerate, can make the rapid time of rising and can shorten batch preparations of viscosity, can handle tackiness agent easily simultaneously.
Japanese patent application No.73036167B discloses a kind of composition, said composition comprises: 1) carboxymethyl cellulose, alginic acid, polyacrylic acid or its salt, these materials are through following processing: a) apply with glycerol or alcohol, or b) after a) going on foot processing, apply with paste, lac, gelatin and agar, or c) use a) in material and b) in the mixture coating of material; 2) an alkali metal salt of alkaline carbonate, two carbonate, phosphoric acid salt, polyphosphate or EDTA, these materials optionally use above-mentioned a), b) and method c) handle; And optionally comprise 3) glucose, sucrose, fructose, barley-sugar, mannitol and salt.When adding water in the said composition, its is very fast wetted and disperse, and can obtain the solution of alginic acid, polyacrylic acid or carboxymethyl cellulose rapidly.
Japanese patent application No.72044335B has instructed by improve the deliquescent method of water-soluble polymers coated with fused polyvalent alcohol, sugar or latex auxiliary agent.Wherein water-soluble polymers comprises methylcellulose gum, CMC, polyvinyl alcohol, alginate, polyacrylic acid and salt thereof and polyacrylamide.Polyvalent alcohol comprises sorbyl alcohol, barley-sugar, inositol, and steamed bun stuffed with sugar is drawn together glucose, sucrose and lactose.With respect to polymkeric substance, the consumption of coating substance is 0.5～10% (weight), is preferably 3～5% (weight).
The U.S. Patent No. 3850838 that licenses to people such as Guckenberger discloses a kind of preparation can disperse pure insoluble hydrogenation colloidal method with the dissolved agglomerate rapidly; this method comprises hydrogenation colloid and not only water soluble but also dissolves in the carbohydrate tackiness agent of alcohol and aqueous alcohol solvent that should sugar is closely linked; the mixture that granulation obtains, the dry then agglomerate granule that obtains.
Above-mentioned patent is not all instructed polyvalent alcohol-the agglomerant water-soluble or application of water-swellable polymer in dentifrice composition.
The present invention relates to contain the composition of the water-soluble or water-swellable polymer of granulous, polymkeric substance wherein is by at least by partial coalescence, wherein with total restatement of composition, the content of polyvalent alcohol is higher than about 10% (weight) with at least a polyvalent alcohol processing.Compare with corresponding undressed water-soluble or water-swellable polymer, said composition can be scattered in the solvent fasterly, and does not form polymer clump.
Another aspect of the present invention also relates to the improved method that a kind of manufacturing contains the dentifrice composition of at least a dried water-soluble or water-swellable polymer, and its improvement comprises with handling through polyvalent alcohol that at least by the granulous of partial coalescence water-soluble or water swellable polymer replaces the water-soluble or water-swellable polymer of doing.Thisly handle and compared with corresponding undressed water-soluble or water-swellable polymer by the granular water soluble of partial coalescence or water-swellable polymer at least through polyvalent alcohol, hydration in water or in the water-containing solvent fasterly, and do not form polymer clump.
Composition of the present invention contains through at least a polyvalent alcohol to be handled and at least by the granular water soluble of partial coalescence or water-swellable polymer, wherein in the gross weight of composition, the content of polyvalent alcohol is higher than about 10% (weight).Agglomeration is in the gathering that is defined as the individual particle that causes the increase of granulated material particle size in addition.
Any natural or synthetic is water-soluble or water-swellable polymer all can be used for preparing composition of the present invention.Preferred water-soluble or water-swellable polymer is a polysaccharide.The available polysaccharide comprises, but be not limited to ether of cellulose, guar gum, guar gum derivatives, Viscogum BE, psyllium, Sudan Gum-arabic, gum ghatti, Indian tragacanth (gum karaya), Tragacanth, carrageenin, agar, ammonium alginate, xanthan gum, Sclerotium gum (scleroglucan), dextran, pectin, starch, chitin and chitosan.
Preferred polysaccharide is ether of cellulose, carrageenin, guar gum, guar gum derivatives and pectin.
Be used for ether of cellulose of the present invention and comprise Natvosol (HEC), hydroxypropylcellulose (HPC), water-soluble Type 3U (EHEC), carboxymethyl cellulose (CMC), carboxymethyl hydroxyethyl cellulose (CMHEC), hydroxypropyl Natvosol (HPHEC), methylcellulose gum (MC), methylhydroxypropylcellulose (MHPC), methyl hydroxyethylcellulose (MHEC), carboxy methyl cellulose (CMMC), the carboxymethyl cellulose of hydrophobically modified (HMCMC), the Natvosol of hydrophobically modified (HMHEC), the hydroxypropylcellulose of hydrophobically modified (HMHPC), the Type 3U of hydrophobically modified (HMEHEC), the carboxymethyl hydroxyethyl cellulose of hydrophobically modified (HMCMHEC), the hydroxypropyl Natvosol (HMHPHEC) of hydrophobically modified, the methylcellulose gum of hydrophobically modified (HMMC), the methylhydroxypropylcellulose of hydrophobically modified (HMMHPC), the methyl hydroxyethylcellulose of hydrophobically modified (HMMHEC), the carboxy methyl cellulose of hydrophobically modified (HMCMMC), cationic hydroxyethyl cellulose (positively charged ion HEC), and the Natvosol of cation hydrophobic modification (positively charged ion HMHEC).Preferred ether of cellulose is carboxymethyl cellulose and Natvosol.
Be used for guar gum derivatives of the present invention and comprise carboxymethyl guar gum (CM guar), hydroxyethyl guar gum (HE guar), Rhoximat RH 148 (HP guar), carboxy-methyl hydroxy propyl guar gum (CMHP guar), cationic guar gum, the guar gum of hydrophobically modified (HM guar), the carboxymethyl guar gum of hydrophobically modified (HMCM guar), the hydroxyethyl guar gum of hydrophobically modified (HMHE guar), the Rhoximat RH 148 of hydrophobically modified (HMHP guar), the Rhoximat RH 148 of cation hydrophobic modification (positively charged ion HMHP guar), the cationic guar gum (HM positively charged ion guar) of carboxy-methyl hydroxy propyl guar gum of hydrophobically modified (HMC MHP guar) and hydrophobically modified.
The polysaccharide that more preferably is used to prepare the present composition is carboxymethyl cellulose, carrageenin and pectin, or their mixture.Carboxymethyl cellulose most preferably.
Be used to make water-soluble or the agglomerant polyvalent alcohol of water-swellable polymer includes, but not limited to sugar, sugar alcohol, glycerol, polyoxyethylene glycol, propylene glycol and their mixture.
The example of sugar is sucrose, glucose, lactose, fructose and wood sugar, or their mixture.The example of sugar alcohol is sorbyl alcohol, inositol, mannitol, melampyrum, arabitol, ribitol, Xylitol and their mixture.
Being used for preferred polyhydric alcohols of the present invention is sorbyl alcohol and polyoxyethylene glycol, or their mixture.The molecular weight that is used for polyoxyethylene glycol of the present invention is not crucial.The molecular weight of polyoxyethylene glycol is preferably about 200 to about 5000,000, and is more preferably about 600 to 25,000, and most preferred is about 1,000 to about 10,000.
In composition of the present invention, in the gross weight of composition, the content that is used for agglomerant polyvalent alcohol is greater than about 10% (weight).The high-content of polyvalent alcohol is preferably 90% (weight), and more preferably about 50% (weight) most preferably is about 30% (weight).
Described agglomeration composition can prepare by spraying liquid polyvalent alcohol to granular polymer.Polyvalent alcohol can be a fused or in solution, is preferably the aqueous solution.In a preferable methods, in a fluidized-bed, fused polyvalent alcohol or polyhydric alcohol solutions are ejected on the particle of water-soluble or water-swellable polymer, if polyvalent alcohol is in solution, the while dried particles.Commercially available to the fluidised-bed spray device can be used in the aforesaid operations.
Agglomerant composition of the present invention is compared with corresponding undressed water-soluble or water-swellable polymer, can the hydration of faster ground in or be dissolved in water or the water-containing solvent, and do not form polymer clump.Adopt Haake viscosity test device 501 to measure this hydration or dissolved speed, promptly when polymkeric substance generation hydration and thickening, under the speed of setting (400rpm), be measured as torque (power) value that keeps being located at the rotation of the transmitter in the solution and need.Hydration time be considered to reach final viscosity 95% o'clock required time (minute), wherein final viscosity is meant in two hours the test mean value of viscosity in last 20 minutes.
In this test, 55 ℃ of measurement hydrations in water.For example, under these conditions, undressed carboxymethyl cellulose lumps immediately, needs to reach in about 15 minutes 95% viscosity subsequently; And handle and have some cakings by agglomerant carboxymethyl cellulose through the polyoxyethylene glycol of the sorbyl alcohol or 20% (weight) of 20% (weight), and these agglomerates disperse rapidly and dissolving in less than one minute.
The another one advantage of above-mentioned composition is agglomeration has reduced the flying dust that occurs when handling undressed polymkeric substance a amount.
Toothpaste of the present invention comprises abrasive, wetting agent and water-soluble polymers.Wetting agent is used to keep the moisture content of toothpaste, and particularly at the mouth end of toothpaste tube, toothpaste longer time ground, there contacts with air.Water-soluble polymers is as the thickening material and the tackiness agent of each composition.Can also use a spot of various other composition, for example flavouring agent, sweeting agent, sanitas, washing composition, winestone control agent, thrombocyte control agent and fluorochemical.
The dental abrasive that is used for toothpaste of the present invention is typical silicon-dioxide and insoluble inorganic salt.Preferred inorganic salt are lime carbonate, Lin Suanergai, tricalcium phosphate, calcium sulfate, insoluble sodium-metaphosphate, hydrated aluminum oxide, magnesiumcarbonate and trimagnesium phosphate.Silicon-dioxide and silica xerogel are specially adapted to translucent or transparent toothpaste.
The typical wetting agent that is used for toothpaste of the present invention comprises glycerol, sorbyl alcohol, propylene glycol or their mixture, these wetting agents and a kind of suitable wetting agent vehicle, and for example water mixes.
In toothpaste of the present invention, in by the gross weight of agglomerant water-soluble or water-swellable polymer, can be contained about 0.5% polyvalent alcohol to about 90% (weight) by agglomerant water-soluble or water-swellable polymer.The preferred content of polyvalent alcohol is about 2% to 50% (weight), and preferred content is about 10% to 30% (weight).
For preparing toothpaste of the present invention, will handle through polyvalent alcohol and stirred with following material: a) wetting agent or wetting agent mixture by agglomerant water-soluble or water-swellable polymer; B) wetting agent vehicle is typically water most; C) salt, flavouring agent, colorant, tensio-active agent; And d) abrasive is to form complete formulation of tooth-paste.In a preferred manufacturing procedure, will directly be joined in wetting agent and the vectorial mixture of wetting agent by agglomerant water-soluble polymers, stir and fully dissolve or swelling until polymer beads; Add any salt then, add abrasive subsequently.Abrasive dissolves the back fully at salt and adds.The mixture that stirring obtains is wetted until abrasive particles; Add flavouring agent then, add tensio-active agent then.
The present invention will illustrate that these embodiment only are used for explanation, are not limitations of the present invention with the following example.Unless otherwise noted, all per-cents, umber etc. all are by weight.
Embodiment 1-14 has demonstrated through polyoxyethylene glycol or sorbyl alcohol and has handled and by the preparation of agglomerant carrageenin and carboxymethyl cellulose and test.Used carrageenin is GENU carrageenin (can buy from the Hercules Inc of Wilmington, the Delaware State).Used carboxymethyl cellulose is CMC 7 MF or CMC 7 the MXF Hercules Inc of Wilmington, the Delaware State (can buy).
Above-mentioned polymkeric substance is used polyoxyethylene glycol, PEG4600 and 1450 (union carbide corporation, Carbowax in Glatt fluid bed processor (GPCG-5 type) top jet device
4600 and 1450) the aqueous solution (25,33 and 50%) is handled and is made that the final content of polyvalent alcohol is about 20% (weight).Also can handle and obtain containing the composition of 10% and 20% sorbyl alcohol with 70% sorbitol aqueous solution.
In operating process, all polyatomic alcohol water solutions all are heated to 50 ℃, and measure with calibration pump and balance.All the test in all with the preheating of Glatt fluid bed processor.Use a Schlick945 nozzle, it is 30/3 second that its strainer shakes circulation (filter shake cycle), and after particle size increases, be reduced to 2 fens/3 seconds.Atomization air pressure is made as 2bar.All products all are dried to and contain the 6-8% moisture content of having an appointment, and are cooled to 30-34 ℃ then.The batch of material amount is 3kg.
Employing is furnished with the HaakeVT501 viscometer of a FL10 transmitter and estimates agglomeration sample and dispersive ability and the hydration/dissolution characteristics of undressed contrast in 55 ℃ deionized water thereof.This apparatus measures is when polymkeric substance generation hydration and thickening, and (400rpm) is the size of the required torque (power) of the rotation that keeps the transmitter in the solution under setting speed.These data are converted into viscosity number (CPS) by computer mathematics subsequently.
Hydration time shown in the table 1 is meant that with the viscosity in two hours the test last 20 minutes be at 100% o'clock, reach the required time of 95% viscosity (minute).The viscosity of each sample is being to record in 2% o'clock with the total restatement concentration of solution all.The amount of polyvalent alcohol or moisture content is not calibrated in the sample.
Embodiment 1-8 and comparative example A
These embodiment have illustrated with sorbyl alcohol and polyoxyethylene glycol processing and have made the carrageenin agglomeration.Data are listed in table 1.The comparative example A has shown the hydration time of undressed carrageenin.
| Table 1 is handled with sorbyl alcohol or polyoxyethylene glycol and is made the carrageenin agglomeration | |||||
| Embodiment number | Polyvalent alcohol | Polyvalent alcohol content weight % | Agglomeration method | Reach the time of 95% viscosity, minute | |
| Injection rate g/min | Preparation temperature ℃ | ||||
| 1 2 3 4 1 5 6 7 8 A 2 | Sorbierite (70% aqueous solution) * * PEG 4600 (50% aqueous solution) PEG 4600 (50% aqueous solution) PEG 4600 (50% aqueous solution) sorbierite (70% aqueous solution) * * * *- | 20 10 20 20 20 10 20 20 - | 34 33 35-84 165 9-20 12 8 9 - | 50 48 42-44 38 38-42 56-62 60 40-42 - | 3 2 9 ＜1 11 30 22 23 22 |
1, in this embodiment, before spraying PEG, in the batch of material of 3kg, spray 1200g water and make the pre-agglomeration of carrageenin with the injection rate of 170g/min.
2, undressed carrageenin embodiment 9-14 and Comparative Examples B, C
These embodiment have illustrated with sorbyl alcohol and polyoxyethylene glycol processing and have made the carboxymethyl cellulose agglomeration.Data are listed in table 2.Comparative Examples B and C have shown the hydration time of undressed carboxymethyl cellulose.
These data show, with content be 10% or higher sorbyl alcohol or polyoxyethylene glycol make the carboxymethyl cellulose agglomeration shorten the time of its hydration greatly.
| Table 2 makes the carboxymethyl cellulose agglomeration with sorbyl alcohol or polyoxyethylene glycol | |||||
| Embodiment number | Polyvalent alcohol | Polyvalent alcohol content weight % | Agglomeration method | Reach the time of 95% viscosity, minute | |
| Injection rate g/min | Preparation temperature ℃ | ||||
| 9 1 10 1 11 1 12 1.3 13 2.4 14 1 B 1 C 2 | Sorbierite (70% aqueous solution) * * PEG 1450 (50% aqueous solution) PEG 1450 (50% aqueous solution) PEG 1450 (50% aqueous solution) sorbierite (70% aqueous solution)-- | 20 20 20 20 20 10 - - | 44 8 150 90-100 165 9 - - | 52 41 38 38 38 42 - - | ＜1 6 ＜1 ＜1 ＜1 15 15 10 |
1, carboxymethyl cellulose is CMC 7MF (Hercules Inc)
2, carboxymethyl cellulose is CMC 7MXF (Hercules Inc)
3, in this embodiment, before spraying PEG, in the batch of material of 3kg, spray 800g water and make the pre-agglomeration of carboxymethyl cellulose with the injection rate of 120g/min.
4, in this embodiment, before spraying PEG, in the batch of material of 3kg, spray 1500g water and make the pre-agglomeration of carboxymethyl cellulose with the injection rate of 70g/min.Embodiment 15,16 and Comparative Examples D, E
These embodiment have illustrated to adopt through sorbyl alcohol or polyoxyethylene glycol and have handled and the formulation of toothpaste of agglomerant carboxymethyl cellulose.Comparative Examples has illustrated the prescription of the contrast composition that adopts undressed carboxymethyl cellulose.
Embodiment 15 and 16 illustrated in room temperature, adopt respectively through the polyoxyethylene glycol (PEG 1450) of 9% sorbyl alcohol and 16% handle and agglomeration carboxyl methyl cellulose 7 MF prepare the method for toothpaste.Comparative Examples D has illustrated the wherein undressed similar prescription of CMC 7 MF with E.Composition and component content in every kind of prescription are listed in table 3.
| Table 3 formulation of tooth-paste, weight % | ||||
| Composition | Embodiment 15 | Embodiment 16 | Comparative Examples D | Comparative Examples E |
| CMC 7MF with 9% sorbierite agglomeration CMC 7MF with 16% PEG1450 agglomeration CMC 7MF glycerine sorbierite (70% aqueous solution) distilled water dicalcium phosphate dihydrate tetrasodium pyrophosphate saccharin sodium sodium monofluorophosphate Sodium Benzoate distilled water flavorant NaLS | 1.10 35.43 8.79 45.0 0.42 0.20 0.76 0.50 6.25 0.55 1.00 | 1.10 35.43 8.79 45.0 0.42 0.20 0.76 0.50 6.25 0.55 1.00 | 1.10 13.00 16.88 14.36 45.0 0.42 0.20 0.76 0.50 6.25 0.55 1.00 | 1.10 35.43 8.79 45.0 0.42 0.20 0.76 0.50 6.25 0.55 1.00 |
For the prescription that does not contain glycerol (embodiment 15,16 and Comparative Examples E), take following step:
1. under agitation, in 6.25 parts of water, add tetrasodium pyrophosphate (0.42 part), soluble saccharin (0.20 part), sodium monoflurophosphate (0.76 part) and Sodium Benzoate (0.50 part), be heated to about 60 ℃, dissolve.
2. carboxymethyl cellulose (1.10 parts) is joined (35.43 parts) in the Sorbitol Solution USP in the beaker, stirred 15 minutes or be stirred to abundant dispersion.Add 8.79 parts of water then, the mixture that stirring obtains 15 to 30 minutes is guaranteed the complete hydration of polymkeric substance (gel-free).Under agitation add the warm salts solution in the step 1 then, stir to continue 15 minutes or until system evenly (no agglomerate or gel).Then mixture is transferred in the Luo Si double planetary mixer (Ross double planetary mixer).
3. in mixing tank, add dicalcium phosphate dihydrate (DCP) (45.00 parts), continue to mix 10 minutes with abundant wetting DCP.Open mixing tank then, scrape the mixture on pulping device and bowl limit, close mixing tank then; Apply vacuum tightness; Continue high-speed mixing 20 minutes or smooth until mixture.
4. add sodium lauryl sulphate (1.00 parts) subsequently, do not having to continue low speed mixing 5 minutes under the vacuum tightness situation.Add flavouring agent (0.55 part) then, under low speed, mixed 2 minutes.Open mixing tank, scrape pulping device and the bowl limit mixture after close mixing tank; Apply vacuum tightness; Continuing middling speed mixed 15 minutes.Then mixing tank is cut off, bleed off vacuum tightness, toothpaste is taken out.
In Comparative Examples D, used glycerol, its schedule of operation and above-mentioned basic identical just in step 2, under agitation is scattered in carboxymethyl cellulose in the glycerol.Continue to stir 5 minutes or fully disperseed until carboxymethyl cellulose.Just add Sorbitol Solution USP then and continue and stirred other 10 minutes.Add entry (14.36 parts) and continue and stirred 15 to 30 minutes, guarantee the complete hydration of polymkeric substance (gel-free).Add warm salts solution and continuation stirring 15 minutes or evenly (do not have caking or gel) until system.Then mixture is transferred to and carries out all the other steps in the Luo Si mixing tank.
In embodiment 15 and 16, observe, agglomeration carboxymethyl cellulose in sorbitol aqueous solution, very easily disperse.After about 3 to 4 minutes, polymkeric substance shows the beginning hydration, and carries out slowly, up to adding entry and salts solution.Do not find the caking of carboxymethyl cellulose.
In Comparative Examples D, undressed carboxymethyl cellulose disperses in anhydrous glycerol easily, not caking.But in Comparative Examples E, undressed carboxymethyl cellulose only just can be scattered in the Sorbitol Solution USP under the high speed stirring very much.Demonstrate the beginning hydration at 1 to 2 minute post polymerization thing.In sorbyl alcohol/salts solution, observe some cakings of carboxymethyl cellulose.Embodiment 17,18 and Comparative Examples F, G
These embodiment have illustrated to adopt through sorbyl alcohol or polyoxyethylene glycol and have handled and the formulation of toothpaste of agglomerant carboxymethyl cellulose at 55 ℃.Comparative Examples has illustrated the prescription of the contrast composition that adopts undressed carboxymethyl cellulose.
Embodiment 17 and 18 illustrated at room temperature, adopt respectively through the polyoxyethylene glycol (PEG1450) of 9% sorbyl alcohol and 16% handle and agglomeration carboxyl methyl cellulose 7 MF prepare the method for toothpaste.Comparative Example F has illustrated the wherein undressed similar prescription of CMC 7 MF with G.The composition and the component content of each prescription are listed in table 4.
| Table 4 formulation of tooth-paste, weight % | ||||
| Composition | Embodiment 17 | Embodiment 18 | Comparative Examples F | Comparative Examples G |
| CMC 7MF with 9% sorbierite agglomeration CMC 7MF with 16% PEG1450 agglomeration CMC 7MF glycerine sorbierite (70% aqueous solution) distilled water dicalcium phosphate dihydrate tetrasodium pyrophosphate saccharin sodium sodium monofluorophosphate Sodium Benzoate distilled water flavorant NaLS | 1.00 35.43 8.89 45.00 0.42 0.20 0.76 0.50 6.25 0.55 1.00 | 1.00 35.43 8.89 45.00 0.42 0.20 0.76 0.50 6.25 0.55 1.00 | 1.00 13.00 16.86 14.46 45.00 0.42 0.20 0.76 0.50 6.25 0.55 1.00 | 1.00 35.43 8.89 45.00 0.42 0.20 0.76 0.50 6.25 0.55 1.00 |
For the prescription that does not contain glycerol (embodiment 17,18 and Comparative Examples G), take following step:
1. under agitation in 6.25 parts of water, add tetrasodium pyrophosphate (0.42 part), soluble saccharin (0.20 part), sodium monoflurophosphate (0.76 part) and Sodium Benzoate (0.50 part), be heated to about 60 ℃, dissolve.
2. Sorbitol Solution USP (35.43 parts) is heated to 55 ℃, under agitation carboxymethyl cellulose (1.00 parts) is added wherein then, continue to stir 15 minutes or until obtaining sufficient dispersion.The water (8.89 parts) that will be heated to 55 ℃ then adds wherein, continues to stir 15 to 30 minutes, guarantees the complete hydration (gel-free) of polymkeric substance.Under agitation add salts solution warm in the step 1 then.Continue to stir 15 minutes or up to system evenly (no agglomerate or gel).Mixture is transferred in the Luo Si double planetary mixer then.
3. in mixing tank, add dicalcium phosphate dihydrate (DCP) (45.00 parts), continue to mix 10 minutes with abundant wetting DCP.Open mixing tank then, scrape pulping device and the bowl limit mixture after close mixing tank; Apply vacuum tightness; Continuing middling speed mixed 15 minutes.Then mixing tank is cut off, bleed off vacuum tightness, toothpaste is taken out.
The treatment step of Comparative Examples F only in the 2nd step with above-mentioned different.Carboxymethyl cellulose under agitation is scattered in the glycerol in 55 ℃, continues to stir 5 minutes or until obtaining sufficient dispersion.Add Sorbitol Solution USP then, and continue to stir other 10 minutes.The water that under agitation adds 55 ℃ continue to stir 15 to 30 minutes to guarantee complete hydration (gel-free), under agitation adds the warm salts solution in the step 1 then, continues to stir 15 minutes or up to system evenly (no agglomerate or gel).Mixture is transferred in the Luo Si double planetary mixer then.
Observed by embodiment 17,18 and Comparative Examples F, carboxymethylcellulomaterials materials is disperseed in the sorbyl alcohol of heat easily and evenly, is not lumpd.Polymkeric substance begins hydration after 1-2 minute, and carries out very rapidly after adding entry and salts solution.The gel phase that obtains is very smooth, and the toothpaste of gained is slick paste.In contrast, in Comparative Examples G, undressed carboxymethyl cellulose can not form slick dispersion.Both made the serious caking that adopts high-speed stirring also to be difficult to avoid polymkeric substance.
Embodiment 19
Present embodiment explanation contain through 20% sorbyl alcohol handle and agglomeration the preparation method of toothpaste of carrageenin.
Composition:
22 parts of glycerol
Carrageenin (through 20% sorbyl alcohol handle and by agglomeration) 0.96 part
0.50 part of Sodium Benzoate
0.2 part of soluble saccharin
0.25 part of tetrasodium pyrophosphate
0.76 part of sodium monoflurophosphate
21.28 parts of deionized waters
51.75 parts of Lin Suanergais
1.50 parts of Sodium Lauryl Sulphate BP/USPs
0.80 part of spearmint oil
Step:
The thing that do to mix of soluble saccharin, Sodium Benzoate, agglomerant carrageenin, sodium monoflurophosphate and tetrasodium pyrophosphate is mixed with glycerol and stirred 5 minutes.Add entry then, the mixture that obtains was heated 15 minutes at 66-71 ℃.Make weight return to original weight by adding distilled water.Mixture is transferred in Hobart's mixing tank (Hobart mixer), adds Lin Suanergai, the mixture that obtains was stirred 2 minutes with mixer speed 1.Close mixing tank, wipe the mixture on bowl limit and the blade off, recover to mix 10 minutes with speed 2 then.
Toothpaste is transferred in the vacuum outgas paddle-tumble.Under agitation add Sodium Lauryl Sulphate BP/USP and flavouring agent oil, under 0.98 bar pressure, mixture was outgased 5 minutes then.Then the toothpaste that obtains is packed into and store in the pipe.
In this preparation, the dispersion of agglomerant carrageenin takes place very rapidly, does not form agglomerate.
Listed examples does not limit the present invention in addition, but is used for illustrating specific embodiments more of the present invention.Below not breaking away from, under the situation of the scope of claim, can carry out many improvement and variation to the present invention.
Claims (29)
1. one kind contains through at least a polyvalent alcohol processing and at least by the composition of the granular water soluble of partial coalescence or water-swellable polysaccharide, wherein, gross weight in composition, the content of polyvalent alcohol is 10%-90% (weight), the content of polysaccharide is 10-90% (weight), and said polyvalent alcohol is selected from: sugar, sugar alcohol, glycerol, polyoxyethylene glycol, propylene glycol and their mixture.
2. the composition of claim 1, wherein said composition is compared with undressed water-soluble or water-swellable polysaccharide, can be scattered in the solvent fasterly and does not form polymer clump.
3. the composition of claim 1, wherein said processing are included in the polyvalent alcohol that sprays at least a liquid form in the fluidized-bed on water-soluble or water-swellable polyoses grain, simultaneously dry these particles.
4. the composition of claim 1, wherein said polysaccharide be selected from following at least a: ether of cellulose, guar gum, guar gum derivatives, Viscogum BE, psyllium, Sudan Gum-arabic, gum ghatti, Indian tragacanth, Tragacanth, carrageenin, agar, ammonium alginate, xanthan gum, Sclerotium gum, dextran, pectin, starch, chitin and chitosan.
5. claim 1 or 4 composition, wherein said polysaccharide is to be selected from following at least a ether of cellulose: Natvosol, hydroxypropylcellulose, water-soluble Type 3U, carboxymethyl cellulose, carboxymethyl hydroxyethyl cellulose, the hydroxypropyl Natvosol, methylcellulose gum, methylhydroxypropylcellulose, methyl hydroxyethylcellulose, carboxy methyl cellulose, the carboxymethyl cellulose of hydrophobically modified, the Natvosol of hydrophobically modified, the hydroxypropylcellulose of hydrophobically modified, the Type 3U of hydrophobically modified, the carboxymethyl hydroxyethyl cellulose of hydrophobically modified, the hydroxypropyl Natvosol of hydrophobically modified, the methylcellulose gum of hydrophobically modified, the methylhydroxypropylcellulose of hydrophobically modified, the methyl hydroxyethylcellulose of hydrophobically modified, the carboxy methyl cellulose of hydrophobically modified, the cationic hydroxyethyl cellulose of cationic hydroxyethyl cellulose and hydrophobically modified.
6. claim 1 or 4 composition, wherein said polysaccharide is to be selected from following at least a guar gum derivatives: the hydroxyethyl guar gum of the guar gum of carboxymethyl guar gum, hydroxyethyl guar gum, Rhoximat RH 148, carboxy-methyl hydroxy propyl guar gum, cationic guar gum, hydrophobically modified, the carboxymethyl guar gum of hydrophobically modified, hydrophobically modified, the Rhoximat RH 148 of hydrophobically modified, the positively charged ion Rhoximat RH 148 of hydrophobically modified, the carboxy-methyl hydroxy propyl guar gum of hydrophobically modified and the cationic guar gum of hydrophobically modified.
7. the composition of claim 1, wherein said polysaccharide is a carboxymethyl cellulose.
8. the composition of claim 1, wherein said polysaccharide is a carrageenin.
9. the composition of claim 1, wherein said polysaccharide is the mixture of carboxymethyl cellulose and carrageenin.
10. the composition of claim 1, wherein said polyvalent alcohol is selected from sorbyl alcohol, inositol, mannitol, melampyrum, arabitol, ribitol, Xylitol, sucrose, glucose, lactose, fructose, wood sugar, glycerol, polyoxyethylene glycol, propylene glycol and their mixture.
11. the composition of claim 1, wherein said polyvalent alcohol is selected from sorbyl alcohol, polyoxyethylene glycol and their mixture.
12. the composition of claim 1, wherein in the gross weight of composition, the high-content of polyvalent alcohol is 50% (weight).
13. the composition of claim 12, wherein in the gross weight of composition, the high-content of polyvalent alcohol is 30% (weight).
14. the composition of claim 1, wherein said water-soluble or water-swellable polysaccharide be selected from following at least a: carrageenin, carboxymethyl cellulose and their mixture; Wherein said polyvalent alcohol be selected from following at least a: sorbyl alcohol, polyoxyethylene glycol and their mixture, wherein in the gross weight of composition, the high-content of polyvalent alcohol is 50% (weight).
15. method for preparing dentifrice composition, comprising the polysaccharide that adopts at least a dried water-soluble or water-swellable, its improvements comprise, at least the polysaccharide that is replaced the water-soluble or water-swellable done with handling by the granular water soluble of partial coalescence or water-swellable polysaccharide composition through at least a polyvalent alcohol, wherein in the gross weight of polysaccharide composition, polysaccharide content is 10-90%, polyvalent alcohol content is 10-90%, and wherein said polyvalent alcohol is selected from: sugar, sugar alcohol, glycerol, polyoxyethylene glycol, propylene glycol and their mixture.
16. the method for claim 15 is wherein saidly compared with undressed polysaccharide water-soluble or water-swellable by agglomerant water-soluble or water-swellable polysaccharide, can the hydration of faster ground in water or water-containing solvent, and do not form polymer clump.
17. the method for claim 15, wherein said polysaccharide be selected from following at least a: ether of cellulose, guar gum, guar gum derivatives, Viscogum BE, psyllium, Sudan Gum-arabic, gum ghatti, Indian tragacanth, Tragacanth, carrageenin, agar, ammonium alginate, xanthan gum, Sclerotium gum, dextran, pectin, starch, chitin and chitosan.
18. the method for claim 17, wherein said polysaccharide are to be selected from following at least a ether of cellulose: Natvosol, hydroxypropylcellulose, water-soluble Type 3U, carboxymethyl cellulose, carboxymethyl hydroxyethyl cellulose, the hydroxypropyl Natvosol, methylcellulose gum, methylhydroxypropylcellulose, methyl hydroxyethylcellulose, carboxy methyl cellulose, the carboxymethyl cellulose of hydrophobically modified, the Natvosol of hydrophobically modified, the hydroxypropylcellulose of hydrophobically modified, the Type 3U of hydrophobically modified, the carboxymethyl hydroxyethyl cellulose of hydrophobically modified, the hydroxypropyl Natvosol of hydrophobically modified, the methylcellulose gum of hydrophobically modified, the methylhydroxypropylcellulose of hydrophobically modified, the methyl hydroxyethylcellulose of hydrophobically modified, the carboxy methyl cellulose of hydrophobically modified, the cationic hydroxyethyl cellulose of cationic hydroxyethyl cellulose and hydrophobically modified.
19. the method for claim 17, wherein said polysaccharide are to be selected from following at least a guar gum derivatives: the hydroxyethyl guar gum of the guar gum of carboxymethyl guar gum, hydroxyethyl guar gum, Rhoximat RH 148, carboxy-methyl hydroxy propyl guar gum, cationic guar gum, hydrophobically modified, the carboxymethyl guar gum of hydrophobically modified, hydrophobically modified, the Rhoximat RH 148 of hydrophobically modified, the positively charged ion Rhoximat RH 148 of hydrophobically modified, the carboxy-methyl hydroxy propyl guar gum of hydrophobically modified and the cationic guar gum of hydrophobically modified.
20. the method for claim 15, wherein said polysaccharide is selected from carboxymethyl cellulose, carrageenin, pectin and their mixture.
21. the method for claim 15, wherein said polysaccharide is a carboxymethyl cellulose.
22. the method for claim 15, wherein said polysaccharide is a carrageenin.
23. the method for claim 15, wherein said polysaccharide are the mixtures of carboxymethyl cellulose and carrageenin.
24. the method for claim 15, wherein said polyvalent alcohol is selected from sorbyl alcohol, inositol, mannitol, melampyrum, arabitol, ribitol, Xylitol, sucrose, glucose, lactose, fructose, wood sugar, glycerol, polyoxyethylene glycol, propylene glycol and their mixture.
25. the method for claim 15, wherein said polyvalent alcohol is selected from sorbyl alcohol, polyoxyethylene glycol and their mixture.
26. the method for claim 15, wherein said is by spraying the polyvalent alcohol of at least a liquid form on water-soluble or water-swellable polymer particle in fluidized-bed by the granular water soluble of partial coalescence or water-swellable polymer at least, and simultaneously dry these particles prepare.
27. the method for claim 26, wherein said polyvalent alcohol is in the aqueous solution.
28. the method for claim 15, wherein in by the gross weight of agglomerant water-soluble or water-swellable polymer, described by agglomerant water-soluble or water-swellable polymer in the content of polyvalent alcohol be 10% to 30% (weight).
29. toothpaste with the preparation of the method for claim 15 or 26.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97121750A CN1105139C (en) | 1997-12-19 | 1997-12-19 | Dispersible water-soluble or water-swellable polymers and process for making toothpastes containing them |
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| Application Number | Priority Date | Filing Date | Title |
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| CN97121750A CN1105139C (en) | 1997-12-19 | 1997-12-19 | Dispersible water-soluble or water-swellable polymers and process for making toothpastes containing them |
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| CN1220280A CN1220280A (en) | 1999-06-23 |
| CN1105139C true CN1105139C (en) | 2003-04-09 |
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| CN97121750A Expired - Lifetime CN1105139C (en) | 1997-12-19 | 1997-12-19 | Dispersible water-soluble or water-swellable polymers and process for making toothpastes containing them |
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| CN103031083B (en) * | 2012-12-28 | 2015-10-07 | 广州市白云区麒胜装饰材料厂 | A kind of pasted starch wallpaper rubber cement and preparation method thereof and application |
| CN107440078A (en) * | 2016-06-01 | 2017-12-08 | 重庆华邦制药有限公司 | A kind of method for efficiently preparing high polymer material thickening system |
| EP3484443A1 (en) * | 2016-07-15 | 2019-05-22 | The Procter and Gamble Company | Process for making oral care compositions |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4426373A (en) * | 1982-09-14 | 1984-01-17 | Colgate-Palmolive Co. | Smooth dental cream |
| EP0267788A2 (en) * | 1986-11-11 | 1988-05-18 | Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo | Complex of pullulan and polyethylene glycol |
| US5030444A (en) * | 1985-11-14 | 1991-07-09 | Chesebrough-Pond's Usa Co., Division Of Conopco, Inc. | Process for making toothpaste |
| CN1097977A (en) * | 1993-07-27 | 1995-02-01 | 青岛德普日用化学工业有限公司 | The toothpaste that contains marine biological preparation |
| US5633028A (en) * | 1993-12-14 | 1997-05-27 | Rhone-Poulenc Inc. | Fast hydrating dust-free xanthan gum |
| US5662924A (en) * | 1991-03-21 | 1997-09-02 | Smith & Nephew Plc | Wound dressing |
| US5674999A (en) * | 1995-12-18 | 1997-10-07 | The Dow Chemical Company | Process for preparing readily dispersible water-soluble cellulosic polymers |
-
1997
- 1997-12-19 CN CN97121750A patent/CN1105139C/en not_active Expired - Lifetime
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4426373A (en) * | 1982-09-14 | 1984-01-17 | Colgate-Palmolive Co. | Smooth dental cream |
| US5030444A (en) * | 1985-11-14 | 1991-07-09 | Chesebrough-Pond's Usa Co., Division Of Conopco, Inc. | Process for making toothpaste |
| EP0267788A2 (en) * | 1986-11-11 | 1988-05-18 | Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo | Complex of pullulan and polyethylene glycol |
| US5662924A (en) * | 1991-03-21 | 1997-09-02 | Smith & Nephew Plc | Wound dressing |
| CN1097977A (en) * | 1993-07-27 | 1995-02-01 | 青岛德普日用化学工业有限公司 | The toothpaste that contains marine biological preparation |
| US5633028A (en) * | 1993-12-14 | 1997-05-27 | Rhone-Poulenc Inc. | Fast hydrating dust-free xanthan gum |
| US5674999A (en) * | 1995-12-18 | 1997-10-07 | The Dow Chemical Company | Process for preparing readily dispersible water-soluble cellulosic polymers |
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| CN1220280A (en) | 1999-06-23 |
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