CN109316372A - Phytate nanoparticle cladding goes stain compound friction agent and the preparation method and application thereof - Google Patents
Phytate nanoparticle cladding goes stain compound friction agent and the preparation method and application thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/27—Zinc; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/55—Phosphorus compounds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
- A61K2800/28—Rubbing or scrubbing compositions; Peeling or abrasive compositions; Containing exfoliants
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
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Abstract
Stain compound friction agent and the preparation method and application thereof is gone the invention discloses phytate nanoparticle cladding.The compound friction agent preparation method is that toothpaste abrasive grain is immersed in plant acid solution and is stirred, its surface is made to adhere to phytate molecule；The partial size of toothpaste abrasive grain is 5~15um；After the filtering of toothpaste abrasive grain or centrifuge separation that are adsorbed with phytate molecule are removed liquid phase, it is placed in the solution of metal ion and stirs, react phytic acid in abrasive particle surface with metal ion, and deposit insoluble phytate nanoparticle on toothpaste abrasives surface；After being filtered, washed, drying, the toothpaste compound friction agent of surface cladding phytate nanoparticle is obtained.Obtained compound friction agent is both physical friction agent and chemical stain removal agent, local concentration and overall density of the phytate in toothpaste is not only increased, and will increase the contact probability of phytate and dental surface when brushing teeth, to improve its stain-removing effect.
Description
Technical field
The present invention relates to a kind of toothpaste rubbing agents, and in particular to a kind of surface cladding the compound of phytate nanoparticle is rubbed
Liniment and preparation method thereof, and the stain removing toothpaste containing the compound friction agent；Belong to daily chemical products technical field.
Background technique
Long-term smoking, have tea, drink coffee or diet in pigment such as soy sauce etc. dental surface can be made to deposit one layer of yellowish-brown
Spot or form exogenous color class, the substances such as sugar, protein, carbohydrate or lipid in saliva are also easier to be adsorbed in
Facing forms organic film, and influences beautiful teeth and health.With ordinary toothpaste brush teeth it is more difficult it is removed, and use chemical bleaching
Or peroxide dissolution inevitably injures tooth even whole oral cavity.
Phytic acid is often extensive in the form of free acid, sodium phytate etc. as a kind of natural plants compound also known as phytic acid
It is present in cereal, beans, oil crops, pollen, spore and organic soil.Phytic acid or phytate are a kind of organic phosphoric acid chemical combination
Object, has very strong sequestering power, and band can also be with albumen in addition to can be in conjunction with metal cation there are six negative phosphate groups
Matter molecule etc. is effectively cooperated.Therefore the phytates such as phytic acid or sodium phytate are proved to have with enamel surface higher affine
Power can influence spot, protein and pigment in the absorption of enamel surface, can prevent pigmentation and capable of helping remove pigment and
Calculus dentalis.
Have at present and some is disclosed about the patent of invention containing phytic acid or sodium phytate isoreactivity object stain removing toothpaste
(201710789677.1,201710073575.X, 201710941568.7,201610361649.5).However, the prior art is equal
It is that the sodium phytate of the phytic acid of these liquids or water soluble is directly appended in formulation of tooth-paste, the additive amount of phytic acid or sodium phytate is big
It is lower than 5% (mass percent) more, because the increase of liquid phase composition or solvable composition not only will affect toothpaste molding and stability,
And reduce the potential resistance to electrolyte contamination ability of the compositions such as thickener.And the phytic acid of relatively low content or solvable sodium phytate are added into
It after in toothpaste, also to be diluted by other components, in addition these phytic acid or phytate active matter can not be with (the frictions of toothpaste abrasive grain
Agent) efficiently contacts and rub with facing, its ability for removing spot can be reduced.Therefore often in addition phytic acid or sodium phytate
Meanwhile can also add it is some it is other go stain component, if patent of invention 201710789677.1 is by sodium tripolyphosphate, soluble phytic acid
Sodium, perlite and hydroxyapatite etc. are a variety of to go stain composition and powder to be compounded, and the toothpaste with polishing whitening function is made.
This not only makes toothpaste complex in compositionization, it is also possible to which strong complex reaction and adsorption capacity of the meeting because of phytic acid lead to the additives such as phytic acid
Between or additive react or adsorb with powder, to prevent the stain-removing effect of phytic acid from thoroughly playing.
Summary of the invention
For defect existing for existing stain removing toothpaste technology, what primary and foremost purpose of the present invention was to provide a kind of toothpaste goes stain to imitate
Fruit is significant, and stability is good, toothpaste compound friction agent and its preparation side of the phytate nanoparticle cladding containing beneficial element
Method；Its preparation process is extremely simple efficiently, is not necessarily to high-temperature high-voltage reaction.
What another object of the present invention was to provide the phytate nanoparticle cladding goes stain compound friction agent in toothpaste
Application.
The present invention is different from the prior art and directly the phytic acid of liquid or soluble phytate is added in toothpaste, but
Conventional toothpaste abrasive grain (rubbing agent) such as silica, calcium carbonate surface synthesize solid phase phytate nanoparticle not soluble in water,
And it is coated on these conventional toothpaste abrasive particle surfaces.During brushing teeth, these are coated with the Compostie abrasive particles of phytate nano particle
It can play the role of the chemical complexing stain-removing effect that traditional physical friction removes stain and phytate.Since toothpaste abrasives exist
Content in formulation of tooth-paste is higher, more than reachable 40% (mass percent), so if these toothpaste abrasive grain (rubbing agent) tables
Face is relatively evenly coated with insoluble phytate nanoparticle, can not only improve the local concentration of phytate (not due to dissolution
Be diluted), due also to the high additive amount of rubbing agent and considerably increase the overall density of phytate, in addition, these phytates are micro-
Grain directly can also be contacted and be rubbed with facing spot with toothpaste abrasives, this has been considerably improved containing phytate particle encapsulation
The stain-removing effect of compound friction agent toothpaste.Preparation process and technique of the present invention are extremely simple efficiently, are not necessarily to high-temperature high-voltage reaction, hold
Easily promote.
The object of the invention is achieved through the following technical solutions:
The preparation method for going stain compound friction agent of phytate nanoparticle cladding, comprising the following steps:
1) toothpaste abrasive grain is immersed in plant acid solution and is stirred 2~10 minutes, its surface is made to adhere to phytate molecule；It is described
The partial size of toothpaste abrasive grain is 5~15um, and the mass ratio of the plant acid solution and toothpaste abrasive grain is 20:1~30:1；
2) the toothpaste abrasive grain for being adsorbed with phytate molecule is filtered or is centrifugated after removing liquid phase, be placed in metal ion
It is stirred 2~10 minutes in solution, reacts phytic acid in abrasive particle surface with metal ion, and deposit insoluble phytate nanoparticle
On toothpaste abrasives surface；After being filtered, washed, drying, the toothpaste compound friction of surface cladding phytate nanoparticle is obtained
Agent.
To further realize the object of the invention, it is preferable that the concentration of the plant acid solution is 0.05~0.5mol/L.
Preferably, the toothpaste abrasive grain is at least one of silica, calcium carbonate and insoluble diedairy fiber.
Preferably, the metal ion be positive ferric ion, positive trivalent cerium ion, positive divalent zinc ion, positive monovalence silver
At least one of ion.Salt containing the metal ion is FeCl3、Ce(NO3)3·6H2O、Zn(NO3)2·6H2O or AgNO3。
Preferably, the concentration of metal ions is 0.05~1.0mol/L.
Preferably, step 1) and the revolving speed of stirring described in step 2) are 300~800rpm, and mixing time is 2~10 points
Clock.
A kind of phytate nanoparticle cladding goes stain compound friction agent, and the covering amount of insoluble phytate is 5.9%
~7.8wt%, the partial size of phytate nanoparticle are 200nm hereinafter, being uniformly coated on toothpaste abrasive grain microsphere surface.
By weight percentage, the raw material components composition of the stain removing toothpaste are as follows: phytate nanoparticle cladding goes stain
Compound friction agent 35%-45%, moisturizer 20%-30%, sodium phytate 2-5%, thickener 1%-3%, surfactant 1%-
2%, sweetener 0.1%-0.5%, flavouring agent 0.5%-1%；Surplus is water.
Preferably, the moisturizer is the mixture of any one in glycerol and sorbierite or both；
The thickener is any one in sodium carboxymethylcellulose, hydroxyethyl cellulose and antler glue；
The surfactant is lauryl sodium sulfate；
The sweetener is saccharin sodium；
The flavouring agent is food-grade essence；The essence is one of peppermint oil, spearmint oil and lemon oil.
The water is deionized water.
Preferably, it when preparation, blunges in premix kettle and dissolves sweetener and sodium phytate, then be transferred to vacuum cream kettle
In, then sequentially add moisturizer, phytate nanoparticle cladding remove the agent of stain compound friction, thickener and surfactant,
High-speed stirred homogeneous, adds flavouring agent, is stirred until homogeneous, and deaerates filling, obtains and goes stain containing phytate nanoparticle cladding
The stain removing toothpaste of compound friction agent.
Ordinary toothpaste rubbing agent mainly includes abrasive silicas, calcium carbonate rubbing agent or insoluble diedairy fiber friction
Agent etc.；The stain compound friction agent of going of phytate nanoparticle cladding of the present invention is insoluble in ordinary toothpaste rubbing agent surface cladding
Phytic acid iron, PHYTIC ACID ZINC SALT, phytic acid cerium or phytic acid silver nano-particle.
Compared with the prior art, the present invention has the following advantages and the utility model has the advantages that
1, the phytate stain removal agent of the phytic acid of liquid or water soluble is directly added to tooth different from the prior art by the present invention
In cream, but solid phase phytic acid not soluble in water is synthesized in conventional toothpaste rubbing agent (abrasive grain) such as silica, calcium carbonate surface
Salt nanoparticle, and these conventional toothpaste rubbing agent surfaces are coated on, then be added in toothpaste.During brushing teeth, these packets
The Compostie abrasive particles for being covered with phytate nanoparticle can play the role of the chemical network that traditional physical friction removes stain and phytate
Close stain-removing effect.And phytate therein can keep the contact and friction of high-efficient and lasting with toothpaste abrasive grain with facing, thus
Achieve the purpose that strength removes tooth stain.
2, the content due to toothpaste abrasives in formulation of tooth-paste is higher, up to 45% (mass percent), so if
These toothpaste abrasives surfaces are equably coated with insoluble phytate nanoparticle, just can not only improve the office of phytate
Portion's concentration (is not diluted) because of dissolution, due also to the high additive amount of rubbing agent and considerably increase the overall density of phytate,
In addition, these phytate particles directly can also be contacted and be rubbed with facing spot with toothpaste abrasives, this, which has been considerably improved, contains
There is the stain-removing effect of the compound friction agent toothpaste of phytate particle encapsulation；Simultaneously because the packet of these of a relatively loose nanoparticles
It covers, toothpaste abrasive grain is worn caused by tooth also can accordingly be reduced.
3, the present invention is not significantly changed since phytate to be coated on to (being mostly incomplete cladding) toothpaste abrasive particle surface
The original formula composition of toothpaste, i.e., both do not dramatically increase liquid phase composition, also without excessive addition powder into lotion, be not in because
Liquid phase composition excessively leads to liquid-solid phase separation, isolates the situations such as liquid in lotion, will not generate to cross because of powder and often have cream
Body knot grain, it is coarse the defects of, so that toothpaste is kept preferable stability.It does not influence to thicken additionally, due to insoluble phytate particle
The potential resistance to electrolyte contamination ability of the compositions such as agent can also make lotion of toothpaste character keep preferable stability.
4, the present invention is not only substantially increased containing the stain removing toothpaste for coating insoluble phytate nanoparticle composite mill liniment
The stain-removing effect of toothpaste also increases other functions of toothpaste because introducing the beneficial elements such as zinc, cerium, iron.For example, zinc has inhibition
Plaque produces the effect of acid and cariogenic bacteria growth and prevents the formation of calculus dentalis；Cerium is light rare earth elements, in addition to inhibiting tooth bacterium
Spot is formed, and also has anti-inflammatory effect, mitigates the inflammation such as periodontitis, gingivitis, and healing acceleration.Existing research shows external source
Property color class in dental surface calmness, the induction for being usually associated with bacterium promotes pigment deposition effect, and these antibacterials or antibacterial
The introducing of element then can further slow down the pigment deposition phenomenon induced by bacterium.
Detailed description of the invention
Fig. 1 is the scanning electricity of the silica Compostie abrasive particles of the insoluble phytate nanoparticle of cladding prepared by embodiment 1
Sub- microscope photo；
Fig. 2 is the electron scanning micrograph of uncoated toothpaste abrasive grain silica；
Fig. 3 is the energy color of the silica Compostie abrasive particles of the insoluble phytate nanoparticle of cladding prepared by embodiment 1
It dissipates X-ray energy spectrogram (Energy dispersive X-ray spectroscopy, EDS)；
Fig. 4 is the energy dispersion X-ray energy spectrum diagram (EDS) of uncoated toothpaste abrasive grain silica.
Specific embodiment
For a better understanding of the invention, the present invention is further illustrated with reference to the accompanying drawings and examples, but implements
Example does not limit in any form the present invention.Unless stated otherwise, raw material and equipment used in the present embodiment are this skill
The raw material and equipment of art field regular market purchase；Toothpaste preparation method is the art conventional method.
Stain removing toothpaste disclosed by the invention is coated Compostie abrasive particles, phytic acid or the phytic acid of insoluble phytate particle by surface
The composition such as sodium and the conventional use of moisturizer of toothpaste, thickener, surfactant, sweetener, essence and deionized water.Originally it goes
Stain toothpaste energy high-efficiency cleaning tooth spot, cleaning and resistance oral bacteria, no any substance that is harmful to the human body are provided by the invention
Toothpaste security performance is high, and cleaning effect is good.It is insoluble below in conjunction with several specific embodiments the present invention is further explained surface cladding
The compound friction agent of property phytate nanoparticle and preparation process containing the strong stain removing toothpaste of compound friction agent.Wherein
Embodiment 1-5 provides the compound friction agent that a kind of surface for being used to prepare stain removing toothpaste coats insoluble phytate nanoparticle,
Embodiment 6-12 is compared using the stain removing toothpaste of this compound friction agent and the stain-removing effect of stain removing toothpaste sample.
Embodiment 1
By 150g rubbing agent silica (SiO2) 4L concentration is immersed in stir in 0.08mol/L phytic acid (PA) solution
5min clock makes rubbing agent surface adhere to phytate molecule；Then it after the abrasive silicas filtering of phytate molecule being adsorbed with, sets
In 4L concentration be 0.1mol/L iron chloride (FeCl3) 5min clock is stirred in solution, using phytic acid to the chelation of iron ion,
The reaction of abrasive silicas surface, and insoluble phytic acid iron particle is deposited on abrasive silicas surface；It filters, wash
After washing, drying, the Silica Using for Toothpaste compound friction agent that surface coats insoluble phytic acid iron nanoparticle is obtained.Fig. 1 is to sweep
The silica for retouching the insoluble phytic acid iron nanoparticle of cladding that electron microscope (Hitachi-SU8220) observes compound rubs
Liniment surface picture, Fig. 2 are uncoated silica compound friction agent surface.It will be seen from figure 1 that silica abrasive grain table
Face generates a large amount of partial sizes in 200nm phytic acid iron nanoparticle below, these particles are equably coated on silica abrasive grain
Surface；And Fig. 2 uncoated silica abrasive grain, surface are relatively smooth, only a small amount of silica clast is attached to
Its surface.Fig. 3 is the energy dispersion X-ray energy spectrum diagram for coating the silica Compostie abrasive particles of insoluble phytic acid iron nanoparticle
(Energy dispersive X-ray spectroscopy, EDS), utilizes the energy dispersion X-ray being attached in scanning electron microscope
Power spectrum (EDS) analytical unit carries out elemental analysis to sample, and surface-element percentage composition is as shown in table 1；Fig. 4 is then uncoated
Toothpaste abrasive grain silica energy dispersion X-ray energy spectrum diagram (EDS), penetrated using the energy dispersion X being attached in scanning electron microscope
Line power spectrum (EDS) analytical unit carries out elemental analysis to sample, and surface-element percentage composition is as shown in table 2.The EDS member of table 1
Element analysis shows, after silica abrasive grain is coated phytic acid iron nanoparticle, surface-element in addition to Si and O, there is also P and Fe member
Element shows that phytic acid iron coats successfully.And uncoated silica abrasive grain surface-element then only has Si and O (table 2).To cladding
The silica abrasive grain weight comparative analysis of front and back shows that covering amount of the phytic acid iron nanoparticle on silica abrasive grain is
7.8% (mass percent).
Table 1
| Element | Wt% | Atomic percent |
| O | 51.30 | 65.16 |
| Si | 47.25 | 34.19 |
| P | 0.41 | 0.27 |
| Fe | 1.05 | 0.38 |
| Total amount | 100.00 | 100.00 |
Table 2
| Element | Wt% | Atomic percent |
| O | 56.47 | 69.49 |
| Si | 43.53 | 30.51 |
| Total amount | 100.00 | 100.00 |
Embodiment 2
By 150g rubbing agent silica (SiO2) be immersed in 4L 0.12mol/L phytic acid (PA) solution, stir 5min
Clock makes rubbing agent surface adhere to phytate molecule；Then after the abrasive silicas filtering of phytate molecule being adsorbed with, it is placed in 4L
0.15mol/L zinc nitrate (Zn (NO3)2·6H2O 5min clock) is stirred in solution, using phytic acid to the chelation of zinc ion,
The reaction of abrasive silicas surface, and insoluble PHYTIC ACID ZINC SALT particle is deposited on abrasive silicas surface；It filters, wash
After washing, drying, the Silica Using for Toothpaste compound friction agent that surface coats insoluble PHYTIC ACID ZINC SALT nanoparticle is obtained.Before cladding
Silica abrasive grain weight comparative analysis afterwards shows that covering amount of the phytic acid iron zinc rice particle on silica abrasive grain is
6.9% (mass percent).
Embodiment 3
By 150g rubbing agent silica (SiO2) be immersed in 4L 0.22mol/L phytic acid (PA) solution, stir 5min
Clock makes rubbing agent surface adhere to phytate molecule；Then after the abrasive silicas filtering of phytate molecule being adsorbed with, it is placed in 4L
0.25mol/L cerous nitrate (Ce (NO3)3·6H2O 5min clock) is stirred in solution, using phytic acid to the chelation of cerium ion,
The reaction of abrasive silicas surface, and insoluble phytic acid cerium particle is deposited on abrasive silicas surface；It filters, wash
After washing, drying, the Silica Using for Toothpaste compound friction agent that surface coats insoluble phytic acid cerium nanoparticle is obtained.Before cladding
Silica abrasive grain weight comparative analysis afterwards shows that covering amount of the phytic acid cerium nanoparticle on silica abrasive grain is
6.8% (mass percent).
Embodiment 4
In the present embodiment, by 150g rubbing agent silica (SiO2) it is immersed in 4L 0.3mol/L phytic acid (PA) solution
In, 5min clock is stirred, rubbing agent surface is made to adhere to phytate molecule；Then the abrasive silicas mistake of phytate molecule will be adsorbed with
After filter, it is placed in 4L 0.35mol/L silver nitrate (AgNO3) 5min clock is stirred in solution, made using chelating of the phytic acid to silver ion
With being reacted on abrasive silicas surface, and deposit insoluble phytic acid Argent grain on abrasive silicas surface；It crosses
After filter, washing, drying, the Silica Using for Toothpaste compound friction agent that surface coats insoluble phytic acid silver nano-particle is obtained.It is right
The silica abrasive grain weight comparative analysis of cladding front and back shows covering amount of the phytic acid silver nano-particle on silica abrasive grain
For 5.9% (mass percent).
Embodiment 5
In the present embodiment, 100g insoluble diedairy fiber is immersed in 4L 0.15mol/L phytic acid (PA) solution, is stirred
5min clock is mixed, rubbing agent surface is made to adhere to phytate molecule；Then after the dietary fiber rubbing agent filtering of phytate molecule being adsorbed with,
It is placed in 4L0.15mol/L iron chloride (FeCl3) 5min clock is stirred in solution, using phytic acid to the chelation of iron ion, in meals
The reaction of fibre frictoin agent surface is eaten, and deposits insoluble phytic acid iron particle on dietary fiber rubbing agent surface；Be filtered, washed,
After drying, the toothpaste diet fiber composite rubbing agent that surface coats insoluble phytic acid iron nanoparticle is obtained.To cladding front and back
Dietary fiber grain weight comparative analysis show covering amount of the phytic acid iron nanoparticle on silica abrasive grain be 7.1%
(mass percent).
The surface of the strong stain removing toothpaste of the present invention coats the compound friction agent of insoluble phytate nanoparticle, can be according to normal
Rule toothpaste abrasives are added in toothpaste, and additive amount is 35%-45% (by weight percentage).In addition, lotion of toothpaste matrix
Component usually also includes moisturizer (20%-30%), thickener (1%-3%), surfactant (1%-2%), sweetener
(0.1%-0.5%), flavouring agent (0.5%-1%) and deionized water etc..The surface coats insoluble phytate nanoparticle
Compound friction agent be to coat insoluble phytic acid iron, PHYTIC ACID ZINC SALT, phytic acid cerium or Phytic acid silver on ordinary toothpaste rubbing agent surface to receive
Rice particle, the ordinary toothpaste rubbing agent includes abrasive silicas, calcium carbonate rubbing agent or insoluble diedairy fiber friction
Agent etc.；The moisturizer be glycerol, in sorbierite any one or both mixture；The thickener is carboxymethyl cellulose
Plain sodium, hydroxyethyl cellulose, any one in antler glue；The surfactant is lauryl sodium sulfate；The sweet tea
Taste agent is saccharin sodium；The flavouring agent is one of food-grade essence, peppermint oil, spearmint oil or lemon oil.
The component formula and its stain-removing effect of the stain removing toothpaste are further described below with reference to embodiment 6-12.
Embodiment 6
By weight percentage, a kind of original of the stain removing toothpaste containing surface cladding phytate nanoparticle compound friction agent
Material group is grouped as are as follows: surface prepared by embodiment 1 coats the silica compound friction agent of insoluble phytic acid iron nanoparticle
40.0%, glycerol 12.0%, sorbierite 12.0%, sodium carboxymethylcellulose 1.2%, lauryl sodium sulfate 1.2%, saccharin sodium
0.3%, essence 0.8%, surplus is deionized water.When preparation, blunges in premix kettle and dissolve saccharin sodium, then be transferred to vacuum
In cream kettle processed, then sequentially adds surface prepared by glycerol, sorbierite, embodiment 1 and coat insoluble phytic acid iron nanoparticle
The agent of silica compound friction, sodium carboxymethylcellulose, lauryl sodium sulfate add after high-speed stirred homogeneous 50 minutes
Essence continues high-speed stirred to uniform, the filling stain removing toothpaste A to obtain the final product of degassing.
Embodiment 7
The present embodiment difference from Example 6 is, on the basis of the formula of embodiment 6, is added to 3.5% (quality
Percentage) sodium phytate.
By weight percentage, a kind of original of the stain removing toothpaste containing surface cladding phytate nanoparticle compound friction agent
Material group is grouped as are as follows: surface coats the silica compound friction agent 40.0% of insoluble phytic acid iron nanoparticle, sodium phytate
3.5%, glycerol 12.0%, sorbierite 12.0%, sodium carboxymethylcellulose 1.2%, lauryl sodium sulfate 1.2%, saccharin sodium
0.3%, essence 0.8%, surplus is deionized water.When preparation, blunges in premix kettle and dissolve sodium phytate, saccharin sodium, then
It is transferred in vacuum cream kettle, then sequentially adds the surface insoluble PHYTIC ACID ZINC SALT of cladding prepared by glycerol, sorbierite, embodiment 1 and receive
The silica compound friction agent of rice particle, sodium carboxymethylcellulose, lauryl sodium sulfate, high-speed stirred homogeneous 50 minutes
Afterwards, essence is added, continues high-speed stirred to uniform, the filling stain removing toothpaste B to obtain the final product of degassing.
Embodiment 8
By weight percentage, a kind of original of the stain removing toothpaste containing surface cladding phytate nanoparticle compound friction agent
Material group is grouped as are as follows: surface coats the silica compound friction agent 40.0% of insoluble PHYTIC ACID ZINC SALT nanoparticle, sodium phytate
3.5%, glycerol 12.0%, sorbierite 12.0%, sodium carboxymethylcellulose 1.2%, lauryl sodium sulfate 1.2%, saccharin sodium
0.3%, essence 0.8%, surplus is deionized water.When preparation, blunges in premix kettle and dissolve sodium phytate, sweetener, then
It is transferred in vacuum cream kettle, then sequentially adds the surface insoluble PHYTIC ACID ZINC SALT of cladding prepared by glycerol, sorbierite, embodiment 1 and receive
The silica compound friction agent of rice particle, sodium carboxymethylcellulose, lauryl sodium sulfate, high-speed stirred homogeneous 50 minutes
Afterwards, essence is added, continues high-speed stirred to uniform, the filling stain removing toothpaste C to obtain the final product of degassing.
Embodiment 9
By weight percentage, a kind of original of the stain removing toothpaste containing surface cladding phytate nanoparticle compound friction agent
Material group is grouped as are as follows: surface coats the silica compound friction agent 40.0% of insoluble phytic acid cerium nanoparticle, sodium phytate
3.5%, glycerol 12.0%, sorbierite 12.0%, sodium carboxymethylcellulose 1.2%, lauryl sodium sulfate 1.2%, saccharin sodium
0.3%, essence 0.8%, surplus is deionized water.When preparation, blunges in premix kettle and dissolve sodium phytate, sweetener, then
It is transferred in vacuum cream kettle, then sequentially adds the surface insoluble PHYTIC ACID ZINC SALT of cladding prepared by glycerol, sorbierite, embodiment 1 and receive
The silica compound friction agent of rice particle, sodium carboxymethylcellulose, lauryl sodium sulfate, high-speed stirred homogeneous 50 minutes
Afterwards, essence is added, continues high-speed stirred to uniform, the filling stain removing toothpaste D to obtain the final product of degassing.
Embodiment 10
By weight percentage, a kind of original of the stain removing toothpaste containing surface cladding phytate nanoparticle compound friction agent
Material group is grouped as are as follows: surface coats the silica compound friction agent 40.0% of insoluble phytic acid silver nano-particle, sodium phytate
3.5%, glycerol 12.0%, sorbierite 12.0%, sodium carboxymethylcellulose 1.2%, lauryl sodium sulfate 1.2%, saccharin sodium
0.3%, essence 0.8%, surplus is deionized water.When preparation, blunges in premix kettle and dissolve sodium phytate, sweetener, then
It is transferred in vacuum cream kettle, then sequentially adds the surface insoluble PHYTIC ACID ZINC SALT of cladding prepared by glycerol, sorbierite, embodiment 1 and receive
The silica compound friction agent of rice particle, sodium carboxymethylcellulose, lauryl sodium sulfate, high-speed stirred homogeneous 50 minutes
Afterwards, essence is added, continues high-speed stirred to uniform, the filling stain removing toothpaste E to obtain the final product of degassing.
Embodiment 11
The present embodiment is comparative example (having uncoated general silica rubbing agent and soluble sodium phytate), this reality
Apply weight percent shared by a stain removing toothpaste each component are as follows: uncoated abrasive silicas 40.0%, sodium phytate 3.5%,
Glycerol 12.0%, sorbierite 12.0%, sodium carboxymethylcellulose 1.2%, lauryl sodium sulfate 1.2%, saccharin sodium 0.3%,
Essence 0.8%, surplus are deionized water.It blunges in premix kettle and dissolves sodium phytate, sweetener, then be transferred to vacuum cream kettle
In, then sequentially add glycerol, sorbierite, uncoated abrasive silicas, sodium carboxymethylcellulose, dodecyl sulphate
Sodium after high-speed stirred homogeneous 50 minutes, adds essence, continues high-speed stirred to uniform, the filling comparative example to obtain the final product of degassing
Stain removing toothpaste F.
Embodiment 12
The present embodiment be another comparative example (have uncoated general silica rubbing agent, soluble sodium phytate with
And the insoluble phytate directly added), weight percent shared by the present embodiment stain removing toothpaste each component are as follows: uncoated dioxy
SiClx rubbing agent 40.0%, sodium phytate 3.5%, insoluble phytic acid iron 3.1% (in order to containing coating insoluble phytate friction
The toothpaste stain-removing effect of agent is compared, using with the comparable insoluble phytate additive amount of maximum covering amount: 7.8% ╳ 40%
=3.1%), glycerol 12.0%, sorbierite 12.0%, sodium carboxymethylcellulose 1.2%, lauryl sodium sulfate 1.2%, saccharin
Sodium 0.3%, essence 0.8%, surplus are deionized water.
Insoluble phytic acid iron is made by the following method: it is dense that phytic acid (PA) solution that 4L concentration is 0.1mol/L is added to 4L
Degree is the iron chloride (FeCl of 0.15mol/L3) stir 5 minutes in solution, both make to react, and by the sediment mistake of formation
Filter, washing are dried to get insoluble phytic acid iron granules is arrived.
When preparation, blunges in premix kettle and dissolve the soluble components such as sodium phytate, sweetener, then be transferred to vacuum cream kettle
In, it is fine then to sequentially add glycerol, sorbierite, uncoated abrasive silicas, insoluble phytic acid iron granules, carboxymethyl
Plain sodium, lauryl sodium sulfate are tieed up, after high-speed stirred homogeneous 50 minutes, adds essence, continues high-speed stirred to uniform, degassing
Filling comparative example stain removing toothpaste G to obtain the final product.
Contrast test:
It is compared using stain-removing effect of the CIE standard colorimetric system to following Table 3 toothpaste sample, this method is to comment at present
The most popular method of valence toothpaste cleaning tooth performance.L*It indicates lightness (brightness), can usually measure the lightness variation for front and back of brushing teeth
ΔL*=L* after brushing teeth‐L* before brushing teethValue come evaluate toothpaste removal dental exogenous mottle stain-removing effect.
Measuring method is as follows: healthy bovine-enamel block being polished, is cleaned, acid etching, is put into dyeing liquor and carries out
5 days (37 DEG C of constant temperature) is dyed, dyeing liquor is coffee, black tea, mucin, the FeCl of 3.5% (mass percent)3(mass ratio 1:
1:0.8:0.5) with the mixed liquor of water, sootiness 30min clock is finally used.The enamel block number that will have been dyed, is separately fixed at brush
On tooth machine, using high density soft bristle tooth brush, brushed teeth respectively with the toothpaste sample slurries simulation of (mass ratio) 35% in table 3, back and forth
It brushes teeth 2400 times, takes out tooth enamel mass and be rinsed with water, dry, the lightness difference DELTA L after measurement is brushed teeth and before brushing teeth*=L* after brushing teeth‐
L* before brushing teethCome the stain-removing effect (tooth enamel mass of the lightness near 40 is selected before brushing teeth) of valence toothpaste sample, Δ L*Value goes more greatly stain to imitate
Fruit is better.
Relatively find out from sample F (comparative example 11), G (comparative example 12) measurement result, directly adds 3.1%
Sample F of the sample G of (mass percent) insoluble phytic acid iron than being free of insoluble phytic acid iron, toothpaste stain-removing effect have centainly
The increase of degree, increment rate are as follows: (18.02-16.79)/16.79=7.3%；And surface is used to coat insoluble phytate particle
Compostie abrasive particles toothpaste, even if stain-removing effect is just when being not added with 3.5% soluble sodium phytate (the sample A of embodiment 6)
It has been substantially better than directly while having been added the toothpaste sample G (comparative example 12) of insoluble phytic acid iron and soluble sodium phytate, has been gone
Stain effect increment rate is；(21.36-18.02)/18.02=18.5% shows that the addition manner of phytate goes stain to imitate in toothpaste
Fruit influence is very big, and coating insoluble phytate nanoparticle in conventional toothpaste abrasive particle surface has to pass weight the stain-removing effect of toothpaste
The effect wanted.And under conditions of adding 3.5% soluble sodium phytate, contain the toothpaste sample for coating insoluble phytate rubbing agent
Product B (embodiment 7), tooth of the stain-removing effect than directly adding 3.1% insoluble phytic acid iron and 3.5% soluble sodium phytate simultaneously
Cream sample G (comparative example 12) improves 21.5%.Show (the sample in containing the toothpaste for coating insoluble phytate rubbing agent
Product A) soluble sodium phytate (3.5%) is further added, though stain-removing effect increases, increasing degree is simultaneously little
(21.5%-18.5%=3%).Toothpaste is gone it can be seen that coating insoluble phytate nanoparticle in conventional toothpaste abrasive particle surface
Stain effect plays a crucial role, and stain-removing effect is much higher than directly adds insoluble phytate or soluble sodium phytate in toothpaste,
Even much higher than the directly toothpaste sample of both additions simultaneously (although coating the plant in insoluble phytate abrasive toothpaste sample
Half of the phosphate content only less than the latter), make us unexpected.This is because being coated in conventional toothpaste abrasive particle surface insoluble
Phytate nanoparticle not only can make the phytate of solid phase evenly dispersed in toothpaste component, not due to the increase of solid phase composition
Influence toothpaste appearance character and stability, it is often more important that maintain higher stain removal agent concentration, increase these and go stain and tooth
The contact probability of tooth surface, to significantly improve the stain-removing effect of toothpaste.
The stain-removing effect of 3 toothpaste sample of table compares
The present invention coats the toothpaste sample of the Compostie abrasive particles of insoluble phytate nanoparticle, stain-removing effect using surface
It has been more than that existing background technique contains that sodium tripolyphosphate, perlite, hydroxyapatite and soluble sodium phytate etc. are a variety of to go stain
Toothpaste with whitening function made of composition and powder compounding.And a variety of powders of the prior art or complexity go stain composition can band
Carry out some drawbacks, for example stain removal agent solubility sodium phytate can be lost because being adsorbed to inside by various powders；Tripolyphosphate
Sodium can generate thickening power in lotion, and content can make powder or lotion phenomena such as knot grain, coarse occur when increasing.However this
Invention coats the toothpaste of the Compostie abrasive particles of insoluble phytate nanoparticle using surface, removes simple (the only phytic acid of stain composition
Salt), not only simplify toothpaste making process, but also toothpaste caused by adsorbing because of a variety of interference for removing stain composition or reaction can also be prevented
The deficiency of stability or appearance character.Simultaneously because the insoluble phytate nanoparticle of the present invention is wrapped by and is fixed on rubbing agent table
Face would not make phytate nanoparticle occur to reunite or tie grain phenomenon, and be able to maintain higher stain removal agent concentration, while also increasing
The contact probability of these stain removal agents and dental surface is added, to be remarkably improved the stain-removing effect of toothpaste.
Embodiment is only used to that the present invention is explained further, and is not intended to limit the present invention in any form, any affiliated
Has usually intellectual in technical field, if utilizing disclosed skill in the case where not departing from the technology of the present invention feature
The equivalent transformation for locally changing or modifying made by art content, still falls in the scope of the present invention.
Claims (10)
1. the preparation method for going stain compound friction agent of phytate nanoparticle cladding, it is characterised in that the following steps are included:
1) toothpaste abrasive grain is immersed in plant acid solution and is stirred 2~10 minutes, its surface is made to adhere to phytate molecule；The toothpaste
The partial size of abrasive grain is 5~15um, and the mass ratio of the plant acid solution and toothpaste abrasive grain is 20:1~30:1；
2) the toothpaste abrasive grain for being adsorbed with phytate molecule is filtered or is centrifugated after removing liquid phase, be placed in the solution of metal ion
Middle stirring 2~10 minutes, reacts phytic acid in abrasive particle surface with metal ion, and deposit insoluble phytate nanoparticle in tooth
Cream rubbing agent surface；After being filtered, washed, drying, obtain phytate nanoparticle cladding goes stain compound friction agent.
2. preparation method according to claim 1, it is characterised in that: the concentration of the plant acid solution be 0.05~
0.5mol/L。
3. preparation method according to claim 1, it is characterised in that: the toothpaste abrasive grain is silica, calcium carbonate
At least one of with insoluble diedairy fiber.
4. preparation method according to claim 1, it is characterised in that: the metal ion is positive ferric ion, just
At least one of trivalent cerium ion, positive divalent zinc ion and positive monovalence silver ion.
5. preparation method according to claim 1, it is characterised in that: the concentration of metal ions be 0.05~
1.0mol/L。
6. preparation method according to claim 1, it is characterised in that: step 1) and the revolving speed of stirring described in step 2) are
300~800rpm, mixing time are 2~10 minutes.
7. a kind of phytate nanoparticle cladding goes stain compound friction agent, which is characterized in that go insoluble in stain compound friction agent
Property phytate covering amount be 5.9%~7.8wt%, the partial size of phytate nanoparticle is 200nm hereinafter, phytate nanometer is micro-
Grain is uniformly coated on toothpaste abrasive grain microsphere surface.
8. it is a kind of containing the phytate nanoparticle as claimed in claim 7 cladding go stain compound friction agent remove stain tooth
Cream, it is characterised in that: by weight percentage, the raw material components of the stain removing toothpaste form are as follows: phytate nanoparticle cladding
Remove stain compound friction agent 35%-45%, moisturizer 20%-30%, sodium phytate 2-5%, thickener 1%-3%, surface-active
Agent 1%-2%, sweetener 0.1%-0.5%, flavouring agent 0.5%-1%；Surplus is water.
9. stain removing toothpaste according to claim 8, it is characterised in that: the moisturizer is appointing in glycerol and sorbierite
The mixture for one or both of anticipating；
The thickener is any one in sodium carboxymethylcellulose, hydroxyethyl cellulose and antler glue；
The surfactant is lauryl sodium sulfate；
The sweetener is saccharin sodium；
The flavouring agent is food-grade essence；The essence is one of peppermint oil, spearmint oil and lemon oil；
The water is deionized water.
10. stain removing toothpaste according to claim 8, it is characterised in that: when preparation, blunge in premix kettle and dissolve sweet tea
Then taste agent and sodium phytate, then be transferred in vacuum cream kettle sequentially add moisturizer, phytate nanoparticle cladding goes the stain multiple
It closes rubbing agent, thickener and surfactant, high-speed stirred homogeneous to add flavouring agent, be stirred until homogeneous, deaerates filling, obtain
The stain removing toothpaste for going stain compound friction agent containing phytate nanoparticle cladding.
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| CN201811248074.1A CN109316372A (en) | 2018-10-25 | 2018-10-25 | Phytate nanoparticle cladding goes stain compound friction agent and the preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112877152A (en) * | 2021-02-06 | 2021-06-01 | 濮阳宏业环保技术研究院有限公司 | Coated sodium percarbonate material and preparation method and application thereof |
| CN114225101A (en) * | 2021-12-23 | 2022-03-25 | 西安交通大学 | Nano-composite hydrogel dressing and preparation method and application thereof |
-
2018
- 2018-10-25 CN CN201811248074.1A patent/CN109316372A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112877152A (en) * | 2021-02-06 | 2021-06-01 | 濮阳宏业环保技术研究院有限公司 | Coated sodium percarbonate material and preparation method and application thereof |
| CN114225101A (en) * | 2021-12-23 | 2022-03-25 | 西安交通大学 | Nano-composite hydrogel dressing and preparation method and application thereof |
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