CN108714122A - A kind of permanent tooth emulsifiable paste and preparation method thereof containing rhizoma nardostachyos - Google Patents
A kind of permanent tooth emulsifiable paste and preparation method thereof containing rhizoma nardostachyos Download PDFInfo
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- A61K9/006—Oral mucosa, e.g. mucoadhesive forms, sublingual droplets; Buccal patches or films; Buccal sprays
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Abstract
The present invention provides a kind of permanent tooth emulsifiable paste containing rhizoma nardostachyos, contain the drug ingedient being made of Radix Notoginseng, Radix Et Rhizoma Nardostachyos extract, borneol and basil oil in the emulsifiable paste, the percentage that wherein Radix Notoginseng accounts for emulsifiable paste lotion weight in terms of notoginseng total saponin is 0.05~0.1%%, the percentage that Radix Et Rhizoma Nardostachyos extract accounts for emulsifiable paste lotion weight is 0.5~1%, Radix Et Rhizoma Nardostachyos extract is petroleum ether extract of the rhizoma nardostachyos after alcohol reflux extracts, the percentage that borneol accounts for emulsifiable paste lotion weight is 0.5~1%, and the percentage that basil oil accounts for emulsifiable paste lotion weight in terms of eugenol is 0.5~1%;Also contain rubbing agent in the lotion of emulsifiable paste, the rubbing agent is MULTILAYER COMPOSITE silica dioxide granule, and the percentage for accounting for emulsifiable paste lotion weight is 30~45%.The present invention also provides the preparation method of above-mentioned emulsifiable paste simultaneously.The present invention solves the problems, such as that rhizoma nardostachyos component and effect plays difference and traditional Chinese medicinal components type is complicated, while having permanent tooth shield gum, deodorization and sterilization effect.
Description
Technical field
The present invention relates to a kind of permanent tooth emulsifiable paste, especially a kind of permanent tooth emulsifiable paste and preparation method thereof containing rhizoma nardostachyos.
Background technology
Emulsifiable paste is common cleaning supplies in daily life, there is very long history.With the continuous hair of science and technology
Exhibition, technological equipment continuously improve and it is perfect, various types of emulsifiable pastes are come out one after another, and the quality and grade of product is continuously improved,
Present emulsifiable paste kind develops into great variety of goods, vdiverse in function by single clean type emulsifiable paste, a brands up to a hundred it is multi-functional
Type emulsifiable paste meets the needs of the different levels level of consumption.
There are many type in China market, and wherein Chinese herbal medicine emulsifiable paste is become with advantages such as its green nature, safety, effect uniquenesses
The bright spot of emulsifiable paste industry also appeared in market in recent years wherein containing the one kind of the emulsifiable paste of rhizoma nardostachyos as Chinese herbal medicine emulsifiable paste.Example
As the patent document of Publication No. CN103405365A, CN105769726A, CN105250193A, CN1633970A disclose
A kind of Chinese medicine preparation emulsifiable paste also all contains rhizoma nardostachyos in ingredient, but the traditional Chinese medicine ingredients contained in above-mentioned patented product exist
Ten kinds or more, some is even more than 20 kinds, and rhizoma nardostachyos therein is not used as main ingredient and plays its effect.It is understood that
When brushing teeth, emulsifiable paste can only stop two minutes in the oral cavity, and the emulsifiable paste weight used every time is about 1.5g, since existing emulsifiable paste produces
Traditional Chinese medicinal components type is excessive in product and rhizoma nardostachyos is not key component, therefore the rhizoma nardostachyos ingredient in existing emulsifiable paste is when actually brushing teeth
The pharmacologic action that can be generated is extremely limited.To sum up, how on the decrease in the case of medicine constituent species ensure rhizoma nardostachyos at
Point the effect of playing stably property become current the art will the problem that there is an urgent need for capture.
Invention content
For overcome the deficiencies in the prior art, the present invention provides a kind of permanent tooth emulsifiable paste containing rhizoma nardostachyos and its preparation side
Method solves the problems, such as that rhizoma nardostachyos component and effect plays difference in the prior art and traditional Chinese medicinal components type is complicated, while there is sterilization to remove
Smelly effect.
The technical solution adopted by the present invention to solve the technical problems is:
Present invention firstly provides the permanent tooth emulsifiable paste that a kind of emulsifiable paste contains rhizoma nardostachyos, contain drug ingedient in the emulsifiable paste, it is described
Drug ingedient is made of Radix Notoginseng, Radix Et Rhizoma Nardostachyos extract, borneol and basil oil, wherein the Radix Notoginseng accounts for institute in terms of arasaponin
The percentage for stating emulsifiable paste lotion weight is 0.05~0.1%, and the Radix Et Rhizoma Nardostachyos extract accounts for the percentage of the emulsifiable paste lotion weight
It is 0.5~1%, the Radix Et Rhizoma Nardostachyos extract is petroleum ether extract of the rhizoma nardostachyos after alcohol reflux extracts, and the borneol accounts for described
The percentage of emulsifiable paste lotion weight is 0.5~1%, and the basil oil accounts for the hundred of the emulsifiable paste lotion weight in terms of eugenol
Divide than being 0.5~1%;Also containing rubbing agent in the lotion of the emulsifiable paste, the rubbing agent is MULTILAYER COMPOSITE silica dioxide granule,
The percentage for accounting for the emulsifiable paste lotion weight is 30~45%.
Preferably, wetting agent, adhesive and foaming agent are also contained in the lotion of the emulsifiable paste.
Preferably, the wetting agent is one or both of glycerine, sorbierite, propylene glycol, accounts for the emulsifiable paste lotion weight
The percentage of amount is 20~30%;Described adhesive is hydroxyethyl cellulose, and the percentage for accounting for the emulsifiable paste lotion weight is 0.6
~2.5%;The foaming agent is lauryl sodium sulfate, and the percentage for accounting for the emulsifiable paste lotion weight is 1.6~2.5%.
The present invention also provides the preparation methods that a kind of emulsifiable paste contains the permanent tooth emulsifiable paste of rhizoma nardostachyos, include the following steps:
S1 weighs 3~8g Silica microparticles, adds it in the absolute ethyl alcohol of 120~150ml, is added simultaneously
1.2~1.8g cetyl trimethylammonium bromides, ultrasonic disperse 30~45 minutes, resulting dispersion system;
The urea of 0.9~1.6g is added in S2 under stirring into above-mentioned dispersion, while being added 20~30ml's
Deionized water is placed in 40~50 DEG C of water bath with thermostatic control and keeps the temperature;
S3 addition 0.7~1.1g tannic acids in the case where speed is 600~800 revs/min of stirring condition, stirring 5~10 minutes, so
It is 9~9.5 that ammonium hydroxide is added afterwards and adjusts pH value of solution, obtains mixing suspension;
The polyvinylpyrrolidone of 2.5~6g is uniformly mixed by S4 with the ethyl orthosilicate of 20~30ml, must mix dropwise addition
This is mixed dropping liquid and is slowly dropped in the mixing suspension, continues to be stirred to react 4~6 hours by liquid, separating, washing,
Dry SiO2Core@SiO2Shell micron particles;
S5 is by SiO obtained2Core@SiO2Shell micron particles are added to the hydrofluoric acid solution that volumetric concentration is 0.1~0.2%
In, wherein SiO2Core@SiO2The weight ratio of shell micron particles and the hydrofluoric acid solution is 2~3:10, etch 10-15 minutes with
To SiO2Shell carries out pitting, and separating, washing, drying obtains SiO2The porous SiO of core@2Shell micron particles;
S6 takes the SiO2The porous SiO of core@2Shell 8~10g of micron particles, is added in the absolute ethyl alcohol of 20~35ml, so
0.1~0.2g azones and the Radix Et Rhizoma Nardostachyos extract of 8~12g are added afterwards, is protected under the conditions of 40~50 DEG C of waters bath with thermostatic control after stirring evenly
It holds 1~2 hour;
Cetyl trimethylammonium bromide 5~8ml of aqueous solution that mass concentration is 5%, ultrasound are added under S7 stirrings
Dispersion 10 minutes, is then slowly added dropwise the ethyl orthosilicate of 25~35ml, while it is 9~10 that ammonium hydroxide, which is added, to adjust pH value of solution, drop
Add finish after the reaction was continued 3~4 hours, separating, washing, drying obtains the MULTILAYER COMPOSITE that internal penetration is coated with Radix Et Rhizoma Nardostachyos extract
Silica dioxide granule, the mass ratio of Radix Et Rhizoma Nardostachyos extract and silica is 1 in this MULTILAYER COMPOSITE silica dioxide granule:20~30;
S8 takes wetting agent and adhesive to be placed in container, and stirring makes it be uniformly mixed, and a certain amount of Radix Et Rhizoma Nardostachyos extract is being stirred
It mixes and is added slowly under state in the mixture of wetting agent and adhesive, stirring obtains transparent colloid in 3~5 minutes;
S9 takes the MULTILAYER COMPOSITE silica dioxide granule and Radix Notoginseng, borneol and basil oil to be uniformly mixed, and is then added
Into the transparent colloid, stirring adds foaming agent, stirs evenly to uniform paste is become;
It is filling after S10 vacuum outgas.
The positive effect of the present invention:The core-shell silica particle with rough surface has been made in the present invention first, with
Convenient for carrying out surface borrosion hole to this nucleocapsid particles and then obtaining the porous micron particles of shell, to its borrosion hole internal penetration rhizoma nardostachyos
After extract, recycles silicon dioxide layer to be coated, obtain three layers that unique internal penetration is coated with Radix Et Rhizoma Nardostachyos extract
Silica dioxide granule, this multi-layer silica dioxide type rubbing agent has stronger dirt-removing power, while can effectively reduce to tooth
Caused by wear, and using the method for the invention prepare emulsifiable paste when, stratiform silica is easy by the friction with tooth
Breakage occurs to fall off, internal Radix Et Rhizoma Nardostachyos extract plays a role jointly with the active ingredient being added directly into emulsifiable paste lotion,
It is remarkably improved the practical pharmacologic action of traditional Chinese medicine ingredients especially rhizoma nardostachyos, it is at the same time, most of sweet before rubbing agent friction is damaged
Loose extract is implied in inside rubbing agent particle, can effectively avoid the loss of Active Components of Nardostachys chinensis when brushing teeth, preferably to send out
Wave its effect.The present invention is aided with borneol, basil oil only using rhizoma nardostachyos, Radix Notoginseng as main ingredient, and traditional Chinese medicinal components type is extremely simple,
Wherein rhizoma nardostachyos has the work(of regulating qi-flowing for relieving pain, calm maincenter, work(of the Radix Notoginseng with dissipate stasis of blood hemostasis, detumescence ding-tong to be divided into this two kinds of groups
The effect of main ingredient, then the effect of be aided with the clearing heat and detoxicating of borneol, erosion prevention and muscle growing, the dispelling wind and eliminating pain of basil oil, antisepsis and sterilization,
It is subject to the special existence of Radix Et Rhizoma Nardostachyos extract, good synergistic effect can be generated between each component, product of the present invention has strong
Root permanent tooth, clearing away heat to stop bleeding, the effect of cleaning gum, strong tooth shield gum, deodorization and sterilization and fresh breath, go out tooth mobility, gum
Blood, gum swelling etc. have remarkable result.
Specific implementation mode
Below to a preferred embodiment of the present invention will be described in detail.
Embodiment 1
The preferred embodiment of the present invention 1 provides a kind of permanent tooth emulsifiable paste containing rhizoma nardostachyos, contains drug ingedient in the emulsifiable paste, institute
It states drug ingedient to be made of Radix Notoginseng, Radix Et Rhizoma Nardostachyos extract, borneol and basil oil, wherein the Radix Notoginseng is accounted in terms of arasaponin
The percentage of the emulsifiable paste lotion weight is 0.05%, and the percentage that the Radix Et Rhizoma Nardostachyos extract accounts for the emulsifiable paste lotion weight is
1%, the Radix Et Rhizoma Nardostachyos extract is petroleum ether extract of the rhizoma nardostachyos after alcohol reflux extracts, and the borneol accounts for the emulsifiable paste lotion
The percentage of weight is 1.0%, and the percentage that the basil oil accounts for the emulsifiable paste lotion weight in terms of eugenol is
0.5%;Also contain rubbing agent in the lotion of the emulsifiable paste, the rubbing agent is MULTILAYER COMPOSITE silica dioxide granule, accounts for the breast
The percentage of cream lotion weight is 35%.
Also contain wetting agent, adhesive and foaming agent in the lotion of the emulsifiable paste.
The wetting agent is glycerine, and the percentage for accounting for the emulsifiable paste lotion weight is 21%;Described adhesive is ethoxy
Cellulose, the percentage for accounting for the emulsifiable paste lotion weight are 0.9%;The foaming agent is lauryl sodium sulfate, accounts for the breast
The percentage of cream lotion weight is 1.7%.
Embodiment 2
The preferred embodiment of the present invention 2 provides a kind of permanent tooth emulsifiable paste containing rhizoma nardostachyos, contains drug ingedient in the emulsifiable paste, institute
It states drug ingedient to be made of Radix Notoginseng, Radix Et Rhizoma Nardostachyos extract, borneol and basil oil, wherein the Radix Notoginseng is accounted in terms of notoginseng total saponin
The percentage of the emulsifiable paste lotion weight is 0.75%, and the percentage that the Radix Et Rhizoma Nardostachyos extract accounts for the emulsifiable paste lotion weight is
0.65%, the Radix Et Rhizoma Nardostachyos extract is petroleum ether extract of the rhizoma nardostachyos after alcohol reflux extracts, and the borneol accounts for the emulsifiable paste
The percentage of lotion weight is 0.8%, and the percentage that the basil oil accounts for the emulsifiable paste lotion weight in terms of eugenol is
0.8%;Also contain rubbing agent in the lotion of the emulsifiable paste, the rubbing agent is MULTILAYER COMPOSITE silica dioxide granule, accounts for the breast
The percentage of cream lotion weight is 38%.
Also contain wetting agent, adhesive and foaming agent in the lotion of the emulsifiable paste.
The wetting agent is sorbierite and propylene glycol mixture, and the percentage for accounting for the emulsifiable paste lotion weight is 26%;Institute
It is hydroxyethyl cellulose to state adhesive, and the percentage for accounting for the emulsifiable paste lotion weight is 1.3%;The foaming agent is dodecyl
Sodium sulphate, the percentage for accounting for the emulsifiable paste lotion weight are 2.0%.
Embodiment 3
The preferred embodiment of the present invention 3 provides a kind of permanent tooth emulsifiable paste containing rhizoma nardostachyos, contains drug ingedient in the emulsifiable paste, institute
It states drug ingedient to be made of Radix Notoginseng, Radix Et Rhizoma Nardostachyos extract, borneol and basil oil, wherein the Radix Notoginseng is accounted in terms of notoginseng total saponin
The percentage of the emulsifiable paste lotion weight is 0.09%, and the percentage that the Radix Et Rhizoma Nardostachyos extract accounts for the emulsifiable paste lotion weight is
0.85%, the Radix Et Rhizoma Nardostachyos extract is petroleum ether extract of the rhizoma nardostachyos after alcohol reflux extracts, and the borneol accounts for the emulsifiable paste
The percentage of lotion weight is 0.75%, and the percentage that the basil oil accounts for the emulsifiable paste lotion weight in terms of eugenol is
0.85%;Also contain rubbing agent in the lotion of the emulsifiable paste, the rubbing agent is MULTILAYER COMPOSITE silica dioxide granule, accounts for the breast
The percentage of cream lotion weight is 42%.
Also contain wetting agent, adhesive and foaming agent in the lotion of the emulsifiable paste.
The wetting agent is propylene glycol, and the percentage for accounting for the emulsifiable paste lotion weight is 28%;Described adhesive is hydroxyl second
Base cellulose, the percentage for accounting for the emulsifiable paste lotion weight are 2.1%;The foaming agent is lauryl sodium sulfate, is accounted for described
The percentage of emulsifiable paste lotion weight is 2.1%.
Embodiment 4
The preferred embodiment of the present invention 4 provides a kind of permanent tooth emulsifiable paste containing rhizoma nardostachyos, contains drug ingedient in the emulsifiable paste, institute
It states drug ingedient to be made of Radix Notoginseng, Radix Et Rhizoma Nardostachyos extract, borneol and basil oil, wherein the Radix Notoginseng is accounted in terms of notoginseng total saponin
The percentage of the emulsifiable paste lotion weight is 0.1%, and the percentage that the Radix Et Rhizoma Nardostachyos extract accounts for the emulsifiable paste lotion weight is
1%, the Radix Et Rhizoma Nardostachyos extract is petroleum ether extract of the rhizoma nardostachyos after alcohol reflux extracts, and the borneol accounts for the emulsifiable paste lotion
The percentage of weight is 1%, and the percentage that the basil oil accounts for the emulsifiable paste lotion weight in terms of eugenol is 1%;Institute
It states and also contains rubbing agent in the lotion of emulsifiable paste, the rubbing agent is MULTILAYER COMPOSITE silica dioxide granule, accounts for the emulsifiable paste lotion weight
The percentage of amount is 44%.
Also contain wetting agent, adhesive and foaming agent in the lotion of the emulsifiable paste.
The wetting agent is sorbierite, and the percentage for accounting for the emulsifiable paste lotion weight is 29%;Described adhesive is hydroxyl second
Base cellulose, the percentage for accounting for the emulsifiable paste lotion weight are 1.6%;The foaming agent is lauryl sodium sulfate, is accounted for described
The percentage of emulsifiable paste lotion weight is 2.1%.
Embodiment 5
The preferred embodiment of the present invention 5 provides a kind of preparation method of the above-mentioned permanent tooth emulsifiable paste containing rhizoma nardostachyos, including walks as follows
Suddenly:
S1 weighs 4g Silica microparticles, adds it in the absolute ethyl alcohol of 120ml, while 1.3g 16 is added
Alkyl trimethyl ammonium bromide, ultrasonic disperse 30 minutes, resulting dispersion system;
The urea of 1.0g is added in S2 under stirring into above-mentioned dispersion, while the deionized water of 21ml is added,
It is placed in 40 DEG C of water bath with thermostatic control and keeps the temperature;
0.8g tannic acids are added in the case where speed is 600 revs/min of stirring condition in S3, stir 6 minutes, and ammonium hydroxide is then added and adjusts
PH value of solution is 9, obtains mixing suspension;
The polyvinylpyrrolidone of 2.6g is uniformly mixed by S4 with the ethyl orthosilicate of 22ml, obtains mixing dropping liquid, by this
Mixing dropping liquid is slowly dropped in the mixing suspension, continues to be stirred to react 4 hours, separating, washing, drying obtains SiO2
Core@SiO2Shell micron particles;
S5 is by SiO obtained2Core@SiO2Shell micron particles are added in the hydrofluoric acid solution that volumetric concentration is 0.1%,
Middle SiO2Core@SiO2The weight ratio of shell micron particles and the hydrofluoric acid solution is 2:10, etch 10 minutes is with to SiO2Shell carries out
Pitting, separating, washing, drying obtain SiO2The porous SiO of core@2Shell micron particles;
S6 weighs the SiO2The porous SiO of core@2Shell micron particles 8.1g, is added in the absolute ethyl alcohol of 23ml, then adds
Enter 0.12g azones and the Radix Et Rhizoma Nardostachyos extract of 10g, is kept for 1.2 hours under the conditions of 40 DEG C of waters bath with thermostatic control after stirring evenly;
The cetyl trimethylammonium bromide aqueous solution 5ml that mass concentration is 5%, ultrasonic disperse are added under S7 stirrings
10 minutes, the ethyl orthosilicate of 26ml is then slowly added dropwise, while it is 9.2 that ammonium hydroxide, which is added, to adjust pH value of solution, is added dropwise subsequent
Continuous reaction 3 hours, separating, washing, drying obtains the MULTILAYER COMPOSITE silica dioxide granule that internal penetration is coated with Radix Et Rhizoma Nardostachyos extract,
The mass ratio of Radix Et Rhizoma Nardostachyos extract and silica is 1 in this MULTILAYER COMPOSITE silica dioxide granule:28;Storage, it is spare;
S8 takes wetting agent and adhesive to be placed in container, and stirring makes it be uniformly mixed, and a certain amount of Radix Et Rhizoma Nardostachyos extract is being stirred
It mixes and is slowly added under state in the mixture of wetting agent and adhesive, stirring obtains transparent colloid in 3 minutes;
S9 weighs the i.e. described MULTILAYER COMPOSITE silica dioxide granule of rubbing agent and Radix Notoginseng, borneol, basil oil are uniformly mixed,
It is then added in the transparent colloid, stirring adds foaming agent, stir evenly to uniform paste is become;
It is filling after S10 vacuum outgas.
Stability of cream:
According to the national standard of GB8372-2008, embodiment 1-4 products are put into -8 DEG C of refrigerator, are taken after 8 hours
Go out, be subsequently placed into 45 ± 1 DEG C of constant incubators and taken out after 8h, place 4h at room temperature, checks that lotion hardens whether there is or not dry and hard
Situation, the results are shown in table below:
Color and luster, pH value, consistency of emulsifiable paste of the embodiment that makes discovery from observation 1-4 etc. are normal.
Clinical application evaluation
Select the patient 100 for having gingivitis, patient 100, the halitosis patient 100 of canker sore respectively by existing plan
Example, the permanent tooth emulsifiable paste one week containing rhizoma nardostachyos obtained using embodiment 2 do not find adverse reaction and toxic side effect, and for tooth
The healing effective percentage of oulitis patient is 98%, and the healing effective percentage for canker sore patient is 89%, for halitosis patient's
It is 92% to cure efficient.
Clinical application is also carried out for the emulsifiable paste that other embodiments are obtained, as a result with embodiment 2 without bigger difference.
In short, product invention prepared by the present invention is aided with borneol, clore basil only using Radix Et Rhizoma Nardostachyos extract, Radix Notoginseng as main ingredient
Oil, traditional Chinese medicinal components type is extremely simple and each component additive amount does not also dramatically increase compared with prior art, is subject to rhizoma nardostachyos extraction
The special existence of object, good synergistic effect can be generated between each component, and there is product of the present invention strong root permanent tooth, heat-clearing to stop
Blood, the effect for cleaning gum, deodorization and sterilization and fresh breath, especially have prophylaxis of teeth loosening, bleeding gums, gum swelling etc.
Remarkable result.
It is above-described to be merely a preferred embodiment of the present invention, it should be understood that the explanation of above example is only used
In facilitating the understanding of the method and its core concept of the invention, it is not intended to limit the scope of protection of the present invention, it is all the present invention's
Any modification for being made within thought and principle, equivalent replacement etc., should all be included in the protection scope of the present invention.
Claims (4)
1. a kind of emulsifiable paste contains the permanent tooth emulsifiable paste of rhizoma nardostachyos, contain drug ingedient in the emulsifiable paste, it is characterised in that:The drug at
Divide and be made of Radix Notoginseng, Radix Et Rhizoma Nardostachyos extract, borneol and basil oil, wherein the Radix Notoginseng accounts for the emulsifiable paste in terms of notoginseng total saponin
The percentage of lotion weight be 0.05~0.1%, the Radix Et Rhizoma Nardostachyos extract account for the emulsifiable paste lotion weight percentage be 0.5~
1%, the Radix Et Rhizoma Nardostachyos extract is petroleum ether extract of the rhizoma nardostachyos after alcohol reflux extracts, and the borneol accounts for the emulsifiable paste lotion
The percentage of weight is 0.5~1%, and the percentage that the basil oil accounts for the emulsifiable paste lotion weight in terms of eugenol is
0.5~1%;Also contain rubbing agent in the lotion of the emulsifiable paste, the rubbing agent is MULTILAYER COMPOSITE silica dioxide granule, is accounted for described
The percentage of emulsifiable paste lotion weight is 30~45%.
2. a kind of emulsifiable paste according to claim 1 contains the permanent tooth emulsifiable paste of rhizoma nardostachyos, it is characterised in that:The lotion of the emulsifiable paste
In also contain wetting agent, adhesive and foaming agent.
3. a kind of emulsifiable paste according to claim 2 contains the permanent tooth emulsifiable paste of rhizoma nardostachyos, it is characterised in that:The wetting agent is sweet
One or both of oil, sorbierite, propylene glycol, the percentage for accounting for the emulsifiable paste lotion weight are 20~30%;The bonding
Agent is hydroxyethyl cellulose, and the percentage for accounting for the emulsifiable paste lotion weight is 0.6~2.5%;The foaming agent is dodecyl
Sodium sulphate, the percentage for accounting for the emulsifiable paste lotion weight are 1.6~2.5%.
4. a kind of emulsifiable paste described in claim 1 contains the preparation method of the permanent tooth emulsifiable paste of rhizoma nardostachyos, which is characterized in that including as follows
Step:
S1 weighs 3~8g Silica microparticles, adds it in the absolute ethyl alcohol of 120~150ml, while being added 1.2
~1.8g cetyl trimethylammonium bromides, ultrasonic disperse 30~45 minutes, resulting dispersion system;
S2 under stirring into above-mentioned dispersion be added 0.9~1.6g urea, while be added 20~30ml go from
Sub- water is placed in 40~50 DEG C of water bath with thermostatic control and keeps the temperature;
0.7~1.1g tannic acids are added in the case where speed is 600~800 revs/min of stirring condition in S3, stir 5~10 minutes, then add
It is 9~9.5 to enter ammonium hydroxide to adjust pH value of solution, obtains mixing suspension;
The polyvinylpyrrolidone of 2.5~6g is uniformly mixed by S4 with the ethyl orthosilicate of 20~30ml, obtains mixing dropping liquid, will
This mixing dropping liquid is slowly dropped in the mixing suspension, continues to be stirred to react 4~6 hours, separating, washing, drying
Obtain SiO2Core@SiO2Shell micron particles;
S5 is by SiO obtained2Core@SiO2Shell micron particles are added in the hydrofluoric acid solution that volumetric concentration is 0.1~0.2%,
Middle SiO2Core@SiO2The weight ratio of shell micron particles and the hydrofluoric acid solution is 2~3:10, etch 10-15 minutes is with to SiO2
Shell carries out pitting, and separating, washing, drying obtains SiO2The porous SiO of core@2Shell micron particles;
S6 takes the SiO2The porous SiO of core@2Shell 8~10g of micron particles, is added in the absolute ethyl alcohol of 20~35ml, then adds
Enter 0.1~0.2g azones and the Radix Et Rhizoma Nardostachyos extract of 8~12g, after stirring evenly under the conditions of 40~50 DEG C of waters bath with thermostatic control keep 1~
2 hours;
Cetyl trimethylammonium bromide 5~8ml of aqueous solution that mass concentration is 5%, ultrasonic disperse are added under S7 stirrings
10 minutes, the ethyl orthosilicate of 25~35ml is then slowly added dropwise, while it is 9~10 that ammonium hydroxide, which is added, to adjust pH value of solution, is dripped
The reaction was continued 3~4 hours after finishing, and separating, washing, drying obtains the MULTILAYER COMPOSITE dioxy that internal penetration is coated with Radix Et Rhizoma Nardostachyos extract
Silicon carbide particle, the mass ratio of Radix Et Rhizoma Nardostachyos extract and silica is 1 in this MULTILAYER COMPOSITE silica dioxide granule:20~30;
S8 takes wetting agent and adhesive to be placed in container, and stirring makes it be uniformly mixed, by a certain amount of Radix Et Rhizoma Nardostachyos extract in stirring shape
It is added slowly under state in the mixture of wetting agent and adhesive, stirring obtains transparent colloid in 3~5 minutes;
S9 takes the MULTILAYER COMPOSITE silica dioxide granule and Radix Notoginseng, borneol and basil oil to be uniformly mixed, and is then added to institute
It states in transparent colloid, stirring adds foaming agent, stir evenly to uniform paste is become;
It is filling after S10 vacuum outgas.
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