CN106890103B - Toothpaste suitable for pump type packing material and preparation method thereof - Google Patents

Toothpaste suitable for pump type packing material and preparation method thereof Download PDF

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CN106890103B
CN106890103B CN201710128960.XA CN201710128960A CN106890103B CN 106890103 B CN106890103 B CN 106890103B CN 201710128960 A CN201710128960 A CN 201710128960A CN 106890103 B CN106890103 B CN 106890103B
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sodium
toothpaste
paste
mixture
stirring
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CN106890103A (en
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陈敏珊
谢晓芳
肖俊芳
郑晓霞
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Guangzhou Shuke Industrial Co.,Ltd.
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Guangzhou Weimeizi Industrial Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/731Cellulose; Quaternized cellulose derivatives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/24Phosphorous; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/25Silicon; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/55Phosphorus compounds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/20Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/28Rubbing or scrubbing compositions; Peeling or abrasive compositions; Containing exfoliants
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/87Application Devices; Containers; Packaging

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Abstract

The invention discloses toothpaste suitable for a pump type packaging material and a preparation method thereof, wherein the formula of the toothpaste comprises, by weight, 15-25 parts of an abrasive, 50-60 parts of a humectant, 0.5-1 part of a thickener, 5-30 parts of deionized water, 0.01-3 parts of a surfactant, 0.01-0.5 part of a preservative, 0.01-2 parts of a stabilizer, 0.01-1.5 parts of essence, 0.01-2 parts of a taste modifier, 0.01-1 part of an appearance modifier and 0.01-10 parts of an efficacy component. The toothpaste has good shear thinning specificity and thixotropy, can be easily discharged after a pump is pressed, keeps the shape of the toothpaste on a toothbrush, can be quickly dispersed in an oral cavity during tooth brushing, can ensure that effective ingredients in the product can smoothly reach all surfaces of the oral cavity and quickly go deep into gaps of the teeth to cover the whole teeth, and cannot be dried or extruded along with the time.

Description

Toothpaste suitable for pump type packing material and preparation method thereof
Technical Field
The invention relates to a toothpaste technology, in particular to toothpaste capable of being used for a pump type packing material and a preparation method thereof.
Background
Most of the toothpaste in the current market is packaged by a flexible pipe. The toothpaste packed in the hose has the disadvantages that the toothpaste in the hose is slightly troublesome to squeeze by opening the cover, the hand-held position and the squeezing amount are not well controlled when the toothpaste is squeezed, the shape of the hose is easy to deform when the hose is squeezed, and the appearance of the deformed hose is not attractive enough. Also, the toothpaste container of this shape requires opening and closing of the cap when used, and thus is inconvenient for children to use. At present, more and more oral care brands break through the hose package, pump type bottles in various forms are used for filling toothpaste, the problem that the package appearance shape is not definite is solved, the package cannot deform like a hose, and the bottle body still keeps attractive after long-term use. And the novel pump type bottled toothpaste can quickly and conveniently provide a proper amount of toothpaste, is more beneficial to daily cleaning of teeth and oral cavities, and can conveniently and effectively control the extrusion amount and the use amount of the toothpaste.
At present, the research of pumping type toothpaste mainly aims at the research of containers, paste of the pumping type toothpaste is directly filled into a pump tube, and no new paste which meets the characteristics and requirements of a pump type packaging material is specially developed aiming at the characteristics of the pump type packaging material.
In the market, the paste used by the pump tube packaging material has two forms:
one is a viscous paste for traditional aluminum plastic tubes, which has good stiffness and can keep a good shape on a toothbrush. However, the paste is used for the pump type packing material, and the use experience of the paste is not better than that of the traditional aluminum-plastic pipe or even worse than that of the traditional aluminum-plastic pipe except that the appearance of the packing material is novel. Because the viscosity of the common toothpaste is higher and higher along with the lapse of time, even the aluminum plastic hose packing material also has the problem of difficult paste squeezing, and for the pump type packing material, the problem is more serious because of the special pump pressure structure of the pump type packing material. The paste with high viscosity is easy to cause the blockage of a piston, and particularly, the pipe orifices of a plurality of pump type packaging materials are open without sealing devices, so that the water loss of the common paste is easy to cause the phenomenon that the paste is dried and solidified to block the pipe orifices, and the paste pump cannot be discharged. Moreover, the paste has the disadvantages of high consistency and poor dispersibility, is easy to fall off during tooth brushing, and is easy to adhere to the falling part to form scale spots.
The other is a particularly thin paste like a liquid. The paste has extremely low viscosity, the pump tube is easy to pump, the paste can be discharged only by slight extrusion, but the paste cannot keep the shape on the toothbrush when being extruded on the toothbrush, and the paste is left at the bottom of the toothbrush even by the side when being extruded on the toothbrush. Not only the paste is wasted and the extruded toothpaste can not be completely used in the oral cavity, but also the medicine in the toothpaste product is difficult to be effectively transferred to the teeth. The over-diluted toothpaste is easy to be drawn and adhered to the mouth of a pipe in the use process, and is not clean and sanitary enough.
The two kinds of paste, in combination with the pump type packing material, have disadvantages, and the real commercialization of the pump type toothpaste cannot be realized.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the toothpaste which is specially suitable for a pump type packing material, is non-viscous, can be kept to be pumped out easily for a long time, can keep shape standing on a toothbrush without leakage and loss, and can be diluted and dispersed quickly during tooth brushing.
Another object of the present invention is to provide a method for preparing the above toothpaste.
The above object of the present invention is achieved by the following scheme:
the invention provides a toothpaste suitable for a pump type packaging material aiming at the characteristics and requirements of the pump type packaging material, wherein the toothpaste formula comprises the following components in parts by weight:
Figure BDA0001239385200000021
the abrasive is one or a mixture of two or more than two of calcium carbonate, silicon dioxide, calcium hydrophosphate dihydrate, aluminum hydroxide, light calcium carbonate, anhydrous calcium hydrophosphate, anhydrous calcium pyrophosphate or calcium hydroxy phosphate in any proportion; the abrasive is preferably silicon dioxide, the silicon dioxide can be prepared into transparent toothpaste, the abrasive value is relatively low, the toothpaste is mild, the teeth are not easy to be damaged, and the abrasive has various types and can be compounded; the abrasive is further preferably a mixture of abrasive silica and thickening silica, wherein the weight ratio of abrasive silica to thickening silica in the mixture is 3: 1-25: 1; the inventor discovers through research that the low cleaning power of the friction type silicon dioxide content is insufficient, the wear to enamel is caused by the high content, the thickening silicon dioxide content is too low to contribute to the viscosity of the toothpaste, the viscosity is too high to cause the difficulty in squeezing the toothpaste, the friction type silicon dioxide can not be adopted alone to adjust the viscosity of the toothpaste, the thickening silicon dioxide can not be adopted alone to satisfy the basic cleaning power of the toothpaste, and only when the weight ratio of the friction type silicon dioxide to the thickening silicon dioxide is 3: 1-25: 1, the cleaning effect of the paste can be ensured, and the viscosity of the paste can be flexibly adjusted; the friction type silicon dioxide and the thickening type silicon dioxide refer to friction type silicon dioxide and thickening type silicon dioxide described in standard silica for toothpaste (QB/T2346-2007); the friction type silicon dioxide and the thickening type silicon dioxide can be prepared by adopting products sold in the market.
The humectant is one or a mixture of two or more of sorbitol, glycerol, propylene glycol, polyethylene glycol 400, polyethylene glycol 600, polyethylene glycol 1000 and polyethylene glycol 1450 at any ratio; the humectant is preferably a mixture of sorbitol and glycerol, and the weight ratio of the sorbitol to the glycerol in the mixture is 1: 3-1: 1; the inventor finds that the humectant adopts sorbitol and glycerin according to the proportion of 1: 3-1: 1, the product can not only meet the good shear thinning characteristic and moisture retention of the pump type paste, but also solve the problem of overhigh cost of the humectant.
The thickener is one or a mixture of two or more than two of sodium carboxymethylcellulose, xanthan gum, hydroxyethyl cellulose, carbomer resin, xanthan gum, guar gum, carrageenan or magnesium aluminum silicate in any proportion; the thickening agent is preferably a mixture of sodium carboxymethyl cellulose and xanthan gum, and the weight ratio of the sodium carboxymethyl cellulose to the xanthan gum in the mixture is 1: 10-1: 2; according to the invention, researches show that the thickening agent adopts sodium carboxymethylcellulose and xanthan gum according to the weight ratio of 1: 10-1: 2, it is possible to impart better thixotropy, stringiness and consistency to the product.
The deionized water is used for toothpaste, and the using amount of the deionized water is preferably 10-20 parts.
The surfactant is sodium lauryl sulfate, sodium lauroyl ammonia, cocamidopropyl betaine or alkyl polyglucoside, preferably sodium lauryl sulfate.
The antiseptic is sodium benzoate, sorbate, methyl hydroxybenzoate, ethyl hydroxybenzoate or propyl hydroxybenzoate, preferably sodium benzoate.
The stabilizer is sodium pyrophosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium carbonate, sodium bicarbonate, citric acid, sodium citrate, succinic acid, sodium succinate, tartaric acid, sodium tartrate, vitamin C, tocopherol, stannous chloride or tea polyphenols, preferably sodium pyrophosphate.
The toothpaste body is mainly developed aiming at the characteristics of the pump type packing material, the viscosity of the toothpaste body is adjusted mainly through the material selection and the mixture ratio of the abrasive, the humectant, the thickening agent and the deionized water, so that the toothpaste can be smoothly pumped out of the pump type packing material, and even if the viscosity change of the toothpaste is extremely small along with the passage of time, the toothpaste body still keeps the level of being smoothly pumped out; in addition, the synergistic effect of the humectant and the thickener ensures that the paste body can show excellent shear thinning property and thixotropy under the condition of low viscosity, the paste body has good fluidity during extrusion and can be smoothly pumped out, when the paste body is extruded to a toothbrush, the paste body can be well erected on the toothbrush for shape keeping without leakage loss, and when tooth brushing is carried out, the toothpaste can be quickly thinned and dispersed under the action of the toothbrush, so that the toothpaste is quickly dispersed to the oral cavity, and the effective components of the toothpaste are ensured to be effectively transferred to each area of the oral cavity.
Therefore, the toothpaste formula of the invention is characterized in that the materials of the abrasive, the humectant, the thickener and the deionized water are selected and matched with a proper surfactant, a proper preservative and a proper stabilizer, in addition, the toothpaste formula of the invention also comprises essence, a taste modifier and a proper appearance modifier, and the three components are conventional components of the toothpaste formula, so that the selection of the essence, the taste modifier and the appearance modifier can be realized by adopting the conventional selection of the technicians in the field during the preparation of the toothpaste, such as: the essence adopts any one or mixture of two or more than two of mint-flavor essence, spearmint-flavor essence, wintergreen-flavor essence, fruit-flavor essence, tea-flavor essence, drug-flavor essence or essential oil in any proportion; the taste modifier is one or a mixture of two or more of saccharin, saccharin sodium, sucralose, sucrose, xylitol, sorbitol, lactose, mannitol, maltitol, erythritol, aspartame or sodium chloride in any proportion; the appearance modifier is one or the mixture of two or more than two of titanium dioxide, natural pigment, synthetic pigment and lake thereof, small-particle-size colored silicon dioxide particles or pearlescent pigment in any proportion.
In addition, the user has functional requirements on toothpaste such as whitening, tartar removal, caries prevention and the like, so the toothpaste formula of the invention further comprises effective components, and the effective components are selected according to actual needs, and are commonly used by persons skilled in the art for preparing toothpaste, such as any one or a mixture of two or more of sodium fluoride, sodium monofluorophosphate, stannous fluoride, amine fluoride, sodium phytate, potassium pyrophosphate, sodium tripolyphosphate, sodium hexametaphosphate, pearl powder, hydroxyapatite, calcium glycerophosphate, xylitol, potassium nitrate, strontium chloride, paeonol, zinc citrate, cetylpyridinium chloride, magnolol extract, tranexamic acid, eugenol, zeolite, polyvinylpyrrolidone, activated carbon, honeysuckle extract or lysozyme in any proportion.
The invention also provides a preparation method of the toothpaste suitable for the pump type packing material, which comprises the following steps:
step 1
Adding taste modifier, antiseptic, stabilizer and effective components into deionized water, stirring at 1000r/min for 15min until the raw materials are dissolved to obtain water solution;
adding a thickening agent into the humectant at a stirring speed of 500r/min, and stirring for 10 minutes until the thickening agent is uniformly dispersed to prepare a glue dispersion liquid;
putting the friction agent and the surfactant into a powder tank, stirring for 15 minutes at the speed of 20r/min, and uniformly mixing to prepare a powder mixture;
step 2
Adding the aqueous solution and the glue dispersion liquid prepared in the step 1 into a paste making machine, starting a scraper and double stirring of the paste making machine, wherein the speed of the scraper is 50r/min, the speed of the double stirring is 1000r/min, controlling the vacuum degree to be-0.04 MPa to-0.08 MPa while keeping the scraper and the double stirring of the paste making machine after running for 15 minutes, and sucking the powder mixture prepared in the step 1;
after the powder mixture is completely sucked, adjusting the vacuum degree to-0.092 MPa, adjusting the speed of a scraper to 100r/min and the double-stirring speed to 3000r/min, and then keeping the scraper and the double-stirring operation until the temperature of the paste reaches 38 ℃;
when the paste body temperature reaches 38 ℃, keeping the scraper and the double stirring operation of the paste making machine, stopping the vacuum pump, simultaneously opening the fragrance inlet valve, slowly sucking essence and appearance modifier, after the essence and the appearance modifier are mixed into the paste body, starting the vacuum pump, reducing the scraper speed to 80r/min, reducing the double stirring speed to 2200r/min, starting timing, stopping the double stirring (without stopping the vacuum pump and the scraper) after 15min, controlling the vacuum degree to be not less than-0.096 MPa, continuously vacuumizing, degassing for 15min, and preparing the toothpaste suitable for the pump type packing material.
The toothpaste suitable for the pump type packing material is non-viscous paste, the viscosity range of the toothpaste is 20e3 cP-100 e3cP, and the toothpaste extrusion pressure is controlled within 35N.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention achieves two indexes of controlling the viscosity and ensuring the cleaning power by controlling the proportion of the grinding material in the paste body; the existing liquid toothpaste is pursuing low viscosity, the dosage of the abrasive is reduced, the cleaning effect brought by the abrasive is neglected, and the prepared paste has no basic cleaning function although being easy to extrude; the friction agent is prepared by compounding friction type silicon dioxide and thickening type silicon dioxide in a proper amount, so that the cleaning force of the grinding material can be ensured, and the viscosity can be finely adjusted;
2. the phenomenon that paste at the tube opening is dried and hardened frequently occurs in the use process of the pump type toothpaste in the existing market, so that the paste can not be discharged from the pump; the invention ensures the wettability of the paste in the pump type packaging material by controlling the proportion of the humectant, and prevents the drying and caking caused by excessive water loss; in addition, the inventor finds that the ointment is easy to dry and hard when the content of the humectant in the formula is too low, the moisture retention performance is poor, and the proportion of the residual friction agent and the moisture is insufficient when the content of the humectant in the formula is too high, so that the inventor selects 50-60 parts of the humectant in the formula by experimental scheme design and data optimization;
3. in the prior art, in order to pursue low viscosity, only the extrudability is considered, but the formability of the toothpaste on the toothbrush is not considered, and the toothpaste is leaked between the toothbrushes as soon as being extruded to the toothbrushes; the thixotropy of the paste is controlled by controlling the proportion of the thickening agent, so that the paste can keep the shape on the toothbrush, and the paste is prevented from leaking between the toothbrushes; in addition, the inventor finds that the solid-liquid separation of the paste is unstable when the content of the thickener in the formula is too low, the paste is too thin and is not easy to form on a toothbrush, and the consistency of the paste is increased when the content of the thickener is too high, so that the paste is difficult to squeeze, so that the inventor selects 0.5-1 part of the thickener in the formula through experimental scheme design and data optimization;
4. according to the invention, through optimization of the formula components of the toothpaste, the toothpaste is ensured to be a non-viscous toothpaste, the viscosity range is controlled to be 20e3 cP-100 e3cP, and the toothpaste squeezing pressure is controlled to be within 35N, so that a user is ensured to have normal and good use experience when using the pump type toothpaste, and the problem of difficulty in toothpaste squeezing is avoided;
5. the toothpaste is specially developed for pump type packing materials, has good shear thinning specificity and thixotropy, can be easily discharged after a pump is pressed, can keep the shape of the toothpaste on a toothbrush, can be quickly dispersed in an oral cavity during tooth brushing, ensures that effective ingredients in a product can smoothly reach each surface of the oral cavity and quickly go deep into gaps of teeth to cover the whole teeth, and can prevent the toothpaste from drying and caking at a tube opening and prevent the toothpaste from being viscous and incapable of being extruded as time goes on;
6. the preparation method is tailored according to the toothpaste formula and the characteristics of the pump type toothpaste, the optimization of the parameters such as the speed parameter, the vacuum degree parameter and the like further ensures the property of the toothpaste body, and the preparation method is not only beneficial to pump type extrusion, but also beneficial to standing and shape keeping on a toothbrush without leakage and loss.
Detailed Description
The present invention will be further described with reference to specific examples, which are not intended to limit the present invention in any way.
Examples 1-10 are specific examples of toothpastes of the present invention, comparative examples 1-8 are comparative tests, examples 1-10 are the same as comparative examples 1-8 in formulation components, the preparation method is the same, only the dosage of some formulations is different, the specific formulations and dosages of each example are shown in tables 1, 2 and 3, and the preparation method of each example comprises the following steps:
step 1
Adding taste modifier, stabilizer, antiseptic and effective components into deionized water, stirring at 1000r/min for 15min until the raw materials are dissolved to obtain water solution; the taste modifier is saccharin sodium, the stabilizer is sodium pyrophosphate, the preservative is sodium benzoate, and the functional components are sodium monofluorophosphate and sodium phytate;
adding a thickening agent into the humectant at a stirring speed of 500r/min, and stirring for 10 minutes until the thickening agent is uniformly dispersed to prepare a glue dispersion liquid; the humectant is sorbitol and glycerin, and the thickener is sodium carboxymethylcellulose and xanthan gum;
putting the friction agent and the surfactant into a powder tank, stirring for 15 minutes at the speed of 20r/min, and uniformly mixing to prepare a powder mixture; the friction agent is friction type silicon dioxide and thickening silicon dioxide, and the surfactant is sodium lauryl sulfate;
step 2
Adding the aqueous solution and the glue dispersion liquid prepared in the step 1 into a paste making machine, starting a scraper of the paste making machine and double stirring, wherein the speed of the scraper is 50r/min, the speed of the double stirring is 1000r/min, controlling the vacuum degree to be-0.08 MPa while keeping the scraper and the double stirring of the paste making machine after running for 15 minutes, and sucking the powder mixture prepared in the step 1;
after the powder mixture is completely sucked, adjusting the vacuum degree to-0.092 MPa, adjusting the speed of a scraper to 100r/min and the double-stirring speed to 3000r/min, and then keeping the scraper and the double-stirring operation until the temperature of the paste reaches 38 ℃;
when the paste temperature reaches 38 ℃, keeping the scraper and the double stirring operation of the paste making machine, stopping the vacuum pump, simultaneously opening the fragrance inlet valve, slowly sucking in essence and titanium dioxide, after the essence and the titanium dioxide are mixed into the paste, starting the vacuum pump, reducing the speed of the scraper to 80r/min after the vacuum degree reaches-0.094 MPa, reducing the speed of the double stirring to 2200r/min, starting timing, stopping the double stirring (the vacuum pump and the scraper are not stopped) after 15min, controlling the vacuum degree to be not less than-0.096 MPa, continuously vacuumizing, degassing for 15min, and preparing the required toothpaste until the paste is compact, smooth, fine and bubble-free.
Stopping the paste making machine, breaking vacuum, sampling paste, taking the paste after the paste is detected to be qualified, and filling and inspecting the paste.
Examples 1-4 and comparative examples 1-3 were conducted to investigate the effect of humectant usage and sorbitol/glycerin ratio on toothpaste performance by comparative experiments, and the formulation components of each example and comparative example are shown in table 1.
TABLE 1 Effect of humectants on toothpaste Performance
Formulation of Example 1 Example 2 Example 3 Example 4 Comparative example 1 Comparative example 2 Comparative example 3
Sorbitol 13 16 20 30 70 50 0
Glycerol 37 34 30 30 0 10 25
Friction type silica 18 18 18 18 18 18 18
Thickening silica 2 2 2 2 2 2 2
Xanthan gum 0.5 0.5 0.5 0.5 0.5 0.5 0.5
Sodium carboxymethylcellulose 0.1 0.1 0.1 0.1 0.1 0.1 0.1
Saccharin sodium salt 0.2 0.2 0.2 0.2 0.2 0.2 0.2
Sodium benzoate 0.5 0.5 0.5 0.5 0.5 0.5 0.5
Pyrophosphoric acid sodium salt 0.5 0.5 0.5 0.5 0.5 0.5 0.5
Sodium monofluorophosphate 0.8 0.8 0.8 0.8 0.8 0.8 0.8
Sodium lauryl sulfate 2 2 2 2 2 2 2
Sodium phytate 1 1 1 1 1 1 1
Titanium dioxide 0.2 0.2 0.2 0.2 0.2 0.2 0.2
Essence 1 1 1 1 1 1 1
Deionized water 23.2 23.2 23.2 13.2 3.2 13.2 48.2
Examples 5-7 and comparative examples 4-5 were conducted to investigate the effect of the amount of abrasive and the ratio of abrasive to thickening silica on the performance of the toothpaste, and the formulation components of each example and comparative example are shown in Table 2.
TABLE 2 Effect of abrasives on toothpaste Performance
Formulation of Example 5 Example 6 Example 7 Comparative example 4 Comparative example 5 Comparative example 6
Sorbitol 20 20 20 20 20 20
Glycerol 30 30 30 30 30 30
Friction type silica 15 20 24 30 10 0
Thickening silica 5 3 1 5 20 5
Xanthan gum 0.5 0.5 0.5 0.5 0.5 0.5
Sodium carboxymethylcellulose 0.1 0.1 0.1 0.1 0.1 0.1
Saccharin sodium salt 0.2 0.2 0.2 0.2 0.2 0.2
Sodium benzoate 0.5 0.5 0.5 0.5 0.5 0.5
Pyrophosphoric acid sodium salt 0.5 0.5 0.5 0.5 0.5 0.5
Sodium monofluorophosphate 0.8 0.8 0.8 0.8 0.8 0.8
Sodium lauryl sulfate 2 2 2 2 2 2
Sodium phytate 1 1 1 1 1 1
Titanium dioxide 0.2 0.2 0.2 0.2 0.2 0.2
Essence 1 1 1 1 1 1
Deionized water 23.2 20.2 17.2 8.2 13.2 38.2
Examples 8-10 and comparative examples 7-8 are comparative experiments to study the effect of the ratio of sodium carboxymethylcellulose and collagen in the thickener on the performance of toothpaste, and the formulation components of each example and comparative example are shown in table 3.
TABLE 3 Effect of thickening Agents on toothpaste Performance
Figure BDA0001239385200000071
Figure BDA0001239385200000081
For paste examinations of all the above examples and comparative examples, differences between the examples and comparative examples were evaluated by pertinently examining the following indexes. The investigation indexes comprise initial viscosity, viscosity after 1 year, initial paste extrusion pressure, paste extrusion toothpaste after 1 year, stability condition, formability on the toothbrush, cleaning force test and shear thinning characteristic indexes.
Viscosity index measures viscosity immediately after preparation and twelve months. The viscosity was measured in cP using a Brookfield viscometer RVDV-II + P type rotor No. S95 at (20. + -.5) ° C and rotating at a rotation speed of 5 revolutions per minute.
The squeeze pressure index measured the force required to pump the toothpaste just prepared and the force required to pump the toothpaste twelve months after it had been left in place when the pump package was used. The determination adopts a tensile testing machine, the pump type toothpaste is placed on the support under the condition of (20 +/-5) DEG C, the tensile testing machine descends at a constant speed (100 +/-10) mm/min, a pressure head of the tensile testing machine vertically acts on a pump head of the pump pipe, and the force of the tensile testing machine in the time period from the time when the tensile testing machine contacts the pump head to the time when the pump head is pressed to the bottom of the pump head is determined, wherein the unit is N.
The stability inspection mainly inspects whether the paste in the pump pipe has the problems of solid-liquid separation, flavor change, dryness, hardness, flatulence, color change, granulation, pH value exceeding a standard range, thickness change, bacteria change, functional component content change and the like in the process from just preparation to twelve months. If the above situation does not occur in the paste in the course of twelve months, the stability is judged to pass the stability investigation.
The moldability index on the toothbrush is to examine the retention of the toothpaste on the toothbrush when the toothpaste is extruded from the pump tube onto the toothbrush. If the toothpaste can stay upright on the toothbrush, the toothpaste is kept for 30s without sinking, and the toothpaste cannot leak to the gap of the toothbrush, the toothpaste is judged to pass.
The cleaning power test index reflects the cleaning and whitening effect of the toothpaste on the tooth surface. And (3) measuring the whitening effect by using an SP62 colorimeter: the international commission on illumination (CIE) L a b standard color system is the most commonly used color system in dentistry, L denotes the visual brightness, the value is 0 to 100, the larger the brightness is close to white, and the smaller the color is close to black. The changes in L values of the teeth before and after brushing using the toothpastes prepared in examples and comparative examples were recorded, and if the L values after brushing were increased from the L values before brushing and the values before and after brushing were statistically significantly different, the cleaning power test was judged to be passed.
TABLE 4 evaluation of paste indexes of examples 1 to 4 and comparative examples 1 to 3
Test index Example 1 Example 2 Example 3 Example 4 Comparative example 1 Comparative example 2 Comparative example 3
Initial viscosity (× e)3cP) 20 25 27 31 90 60 6
Viscosity (. times.e) at 1 month3cP) 32 37 40 49 140 80 6.5
Viscosity (. times.e) for 1 year3cP) 70 81 85 96 210 170 8
Initial squeezing pressure (N) 26 26 27 28 33 32 20
One month squeezing pressure (N) 28 28 29 29 36 35 20
Pressure of squeezing paste after 1 year (N) 31 33 33 33 41 40 22
Stability survey By passing By passing By passing By passing Dry knot at the pipe mouth Dry knot at the pipe mouth By passing
Formability on toothbrushes By passing By passing By passing By passing By passing By passing Without forming
According to the paste viscosity test results of examples 1 to 4 and comparative examples 1 to 3, the content change of the humectant has a significant influence on the instant viscosity and the subsequent viscosity increase change of the paste.
When the content of the humectant is controlled within the range of 50-60%, indexes such as paste viscosity index, paste extrusion pressure index, stability inspection index and formability on a toothbrush reach standards, and the use performance of the paste is not affected.
When the content of the humectant is higher than 60% and the content proportion of glycerin is lower than 10%, the paste body is thick, the viscosity index and the squeezing pressure index of the paste body reach 2 times of those of the paste body with a proper proportion, and the paste body at the pipe orifice is thick and contacts with air, so that the water loss is fast, the dry and hard state occurs, and the use is influenced. But after the dry part is removed, the extruded paste has good striping property and can stand well on the toothbrush.
When the content of the humectant is lower than 30%, the paste is thin in viscosity and normal in stability, but the paste is poor in standing property and cannot be formed on a toothbrush, and the paste immediately penetrates into gaps of the toothbrush after extrusion, so that the use is influenced.
TABLE 5 evaluation of paste indexes of examples 5 to 7 and comparative examples 4 to 6
Test index Example 5 Example 6 Example 7 Comparative example 4 Comparative example 5 Comparative example 6
Initial viscosity (× e)3cP) 30 35 21 130 250 2
Viscosity (. times.e) at 1 month3cP) 53 59 44 150 Is unable to detect 3
Viscosity (. times.e) for 1 year3cP) 90 98 79 250 Is unable to detect 5
Initial squeezing pressure (N) 26 27 26 35 39 18
1 month squeezing pressure (N) 29 29 28 40 Can not be extruded out 19
Pressure of squeezing paste after 1 year (N) 33 34 35 46 Can not be extruded out 20
Cleaning force test By passing By passing By passing By passing By passing Is not communicated withFor treating
According to the paste viscosity test results of examples 5 to 7 and comparative examples 4 to 6, the viscosity of the paste and the paste squeezing pressure are also affected by the content of the friction material in the paste formula.
When the level of abrasive in the paste formulation is too high, reaching 30% as in example 5, the paste is very viscous and cannot be extruded after 1 month growth. When the content of the abrasive in the paste formula is as low as 5%, although the paste has proper viscosity, the cleaning power of the paste is insufficient, and the basic function of the toothpaste for cleaning the oral cavity cannot be met. When the content of the abrasive in the paste formula is controlled to be 15-25%, not only can the paste viscosity suitable for the pump type packaging material be achieved, but also the cleaning power of the abrasive on teeth can be ensured.
TABLE 6 evaluation of paste indexes of examples 8 to 10 and comparative examples 7 to 8
Test index Example 8 Example 9 Example 10 Comparative example 7 Comparative example 8
Initial viscosity (× e)3cP) 2.2 2 2.1 240 9
Viscosity (. times.e) at 1 month3cP) 3.3 3.9 3.5 Is unable to detect 9.5
Viscosity (. times.e) for 1 year3cP) 7.6 8.1 8.7 Is unable to detect 11
Initial squeezing pressure (N) 26 24 24 37 19
1 month squeezing pressure (N) 28 29 29 Can not be extruded out 19
Pressure of squeezing paste after 1 year (N) 30 32 31 Can not be extruded out 20
Stability survey By passing By passing By passing By passing Oil-water separation
According to the paste viscosity test results of the embodiments 8 to 10 and the comparative examples 7 to 8, it can be known that the thickener, as a key influencing factor of the paste, not only directly influences the viscosity of the paste, but also has a key influence on the stability of the product when being used as an adhesive for connecting the solid phase and the liquid phase of the paste.
When the content of the thickening agent in the paste formula is 1.5%, the paste viscosity is rapidly increased, the increase speed is faster than that of the paste caused by the humectant and the grinding material, and the paste cannot be extruded for 1 month. When the content of the thickening agent in the paste formula is as low as 0.2%, the oil-water separation phenomenon of the paste occurs.
Variations and modifications to the above-described embodiments may occur to those skilled in the art, which fall within the scope and spirit of the above description. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and some modifications and variations of the present invention should fall within the scope of the claims of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.

Claims (3)

1. The toothpaste suitable for the pump type packing material is characterized in that the formula of the toothpaste comprises the following components in parts by weight:
Figure FDA0002418053940000011
the friction agent is a mixture of friction type silicon dioxide and thickening type silicon dioxide, and the weight ratio of the friction type silicon dioxide to the thickening type silicon dioxide in the mixture is 3: 1-25: 1; the humectant is a mixture of sorbitol and glycerol, and the weight ratio of the sorbitol to the glycerol in the mixture is 1: 3-1: 1; the thickening agent is a mixture of sodium carboxymethylcellulose and xanthan gum, and the weight ratio of the sodium carboxymethylcellulose to the xanthan gum in the mixture is 1: 10-1: 2.
2. the toothpaste suitable for use in a pump pack according to claim 1, wherein the surfactant is sodium lauryl sulfate, sodium lauroyl amide, cocamidopropyl betaine or alkyl polyglucoside, the preservative is sodium benzoate, sorbate, methyl hydroxybenzoate, ethylparaben or propylhydroxybenzoate, the stabilizer is sodium pyrophosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium carbonate, sodium bicarbonate, citric acid, sodium citrate, succinic acid, sodium succinate, tartaric acid, sodium tartrate, vitamin C, tocopherol, stannous chloride or tea polyphenol, the flavor is any one or a mixture of two or more of mint-flavor, spearmint-flavor, wintergreen-flavor, fruit-flavor, tea-flavor, drug-flavor, or essential oil, and the taste modifier is saccharin, One or two or more of saccharin sodium, sucralose, sucrose, xylitol, sorbitol, lactose, mannitol, maltitol, erythritol, aspartame or sodium chloride are mixed in any proportion, the appearance modifier is any one or mixture of two or more than two of titanium dioxide, natural pigment, synthetic pigment and lake thereof, colored silicon dioxide particles or pearlescent pigment in any proportion, the functional components are any one or two or more than two of sodium fluoride, sodium monofluorophosphate, stannous fluoride, amine fluoride, sodium phytate, potassium pyrophosphate, sodium tripolyphosphate, sodium hexametaphosphate, pearl powder, hydroxyapatite, calcium glycerophosphate, xylitol, potassium nitrate, strontium chloride, paeonol, zinc citrate, cetylpyridinium chloride, magnolol extract, tranexamic acid, eugenol, zeolite, polyvinylpyrrolidone, active carbon, honeysuckle extract or lysozyme, and the mixture is in any proportion.
3. A method of preparing a toothpaste suitable for use in a pump pack according to claim 1 or 2, comprising the steps of:
step 1
Adding taste modifier, stabilizer, antiseptic and effective components into deionized water, stirring at 1000r/min for 15min until the raw materials are dissolved to obtain water solution;
adding a thickening agent into the humectant at a stirring speed of 500r/min, and stirring for 10 minutes until the thickening agent is uniformly dispersed to prepare a glue dispersion liquid;
putting the friction agent and the surfactant into a powder tank, stirring for 15 minutes at the speed of 20r/min, and uniformly mixing to prepare a powder mixture;
step 2
Adding the aqueous solution and the glue dispersion liquid prepared in the step 1 into a paste making machine, starting a scraper and double stirring of the paste making machine, wherein the speed of the scraper is 50r/min, the speed of the double stirring is 1000r/min, controlling the vacuum degree to be-0.04 MPa to-0.08 MPa while keeping the scraper and the double stirring of the paste making machine after running for 15 minutes, and sucking the powder mixture prepared in the step 1;
after the powder mixture is completely sucked, adjusting the vacuum degree to-0.092 MPa, adjusting the speed of a scraper to 100r/min and the double-stirring speed to 3000r/min, and then keeping the scraper and the double-stirring operation until the temperature of the paste reaches 38 ℃;
and when the paste body temperature reaches 38 ℃, keeping the scraper and the double stirring operation of the paste making machine, stopping the vacuum pump, simultaneously opening the fragrance inlet valve, slowly sucking essence and appearance modifier, after the essence and the appearance modifier are mixed into the paste body, starting the vacuum pump, reducing the speed of the scraper to 80r/min, reducing the double stirring speed to 2200r/min, starting timing, stopping the double stirring and non-stop vacuum pump and the scraper after 15min, controlling the vacuum degree to be not less than-0.096 MPa, continuously vacuumizing, and degassing for 15min to prepare the toothpaste suitable for the pump type packing material.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105307624A (en) * 2013-06-18 2016-02-03 株式会社Lg生活健康 Oral composition
CN105456041A (en) * 2015-12-11 2016-04-06 广州薇美姿实业有限公司 Toothpaste containing particles and transparent viscous substance

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3123091B2 (en) * 1990-01-31 2001-01-09 ライオン株式会社 Liquid dentifrice composition

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105307624A (en) * 2013-06-18 2016-02-03 株式会社Lg生活健康 Oral composition
CN105456041A (en) * 2015-12-11 2016-04-06 广州薇美姿实业有限公司 Toothpaste containing particles and transparent viscous substance

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