CN111874918A - Silica for toothpaste with anti-allergy and antibacterial effects and preparation method thereof - Google Patents
Silica for toothpaste with anti-allergy and antibacterial effects and preparation method thereof Download PDFInfo
- Publication number
- CN111874918A CN111874918A CN202010753367.6A CN202010753367A CN111874918A CN 111874918 A CN111874918 A CN 111874918A CN 202010753367 A CN202010753367 A CN 202010753367A CN 111874918 A CN111874918 A CN 111874918A
- Authority
- CN
- China
- Prior art keywords
- sodium silicate
- toothpaste
- solution
- silicate solution
- sulfuric acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 235
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 113
- 229940034610 toothpaste Drugs 0.000 title claims abstract description 100
- 239000000606 toothpaste Substances 0.000 title claims abstract description 100
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 53
- 230000003266 anti-allergic effect Effects 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 54
- 239000008118 PEG 6000 Substances 0.000 claims abstract description 35
- 229920002584 Polyethylene Glycol 6000 Polymers 0.000 claims abstract description 35
- BIVBRWYINDPWKA-VLQRKCJKSA-L Glycyrrhizinate dipotassium Chemical compound [K+].[K+].O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@H]1CC[C@]2(C)[C@H]3C(=O)C=C4[C@@H]5C[C@](C)(CC[C@@]5(CC[C@@]4(C)[C@]3(C)CC[C@H]2C1(C)C)C)C(O)=O)C([O-])=O)[C@@H]1O[C@H](C([O-])=O)[C@@H](O)[C@H](O)[C@H]1O BIVBRWYINDPWKA-VLQRKCJKSA-L 0.000 claims abstract description 15
- 229940101029 dipotassium glycyrrhizinate Drugs 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 208
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 152
- 239000004115 Sodium Silicate Substances 0.000 claims description 118
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 118
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 112
- 238000003756 stirring Methods 0.000 claims description 35
- 238000006243 chemical reaction Methods 0.000 claims description 34
- 239000011259 mixed solution Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 9
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 8
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 8
- 235000011152 sodium sulphate Nutrition 0.000 claims description 8
- 239000008236 heating water Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 2
- 238000011085 pressure filtration Methods 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 239000011593 sulfur Substances 0.000 claims 1
- 229910052717 sulfur Inorganic materials 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 16
- 239000007771 core particle Substances 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 27
- 238000012360 testing method Methods 0.000 description 21
- 238000003825 pressing Methods 0.000 description 11
- 230000000694 effects Effects 0.000 description 9
- 230000008569 process Effects 0.000 description 8
- 201000002170 dentin sensitivity Diseases 0.000 description 5
- 230000036347 tooth sensitivity Effects 0.000 description 5
- 208000025157 Oral disease Diseases 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 208000030194 mouth disease Diseases 0.000 description 4
- 238000005755 formation reaction Methods 0.000 description 3
- 208000007565 gingivitis Diseases 0.000 description 3
- 210000000214 mouth Anatomy 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 206010006326 Breath odour Diseases 0.000 description 2
- 208000032139 Halitosis Diseases 0.000 description 2
- 206010061218 Inflammation Diseases 0.000 description 2
- 208000007117 Oral Ulcer Diseases 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 241000589517 Pseudomonas aeruginosa Species 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 208000002399 aphthous stomatitis Diseases 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000012258 culturing Methods 0.000 description 2
- 239000001963 growth medium Substances 0.000 description 2
- 230000004054 inflammatory process Effects 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000002085 persistent effect Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 230000003405 preventing effect Effects 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000000638 stimulation Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 238000009631 Broth culture Methods 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 208000034619 Gingival inflammation Diseases 0.000 description 1
- 206010028034 Mouth ulceration Diseases 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003467 diminishing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000003906 humectant Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 239000002324 mouth wash Substances 0.000 description 1
- 229940051866 mouthwash Drugs 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 201000001245 periodontitis Diseases 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000035755 proliferation Effects 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 230000035807 sensation Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 159000000008 strontium salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
- C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
-
- 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
- A61K8/25—Silicon; Compounds thereof
-
- 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
- A61K8/63—Steroids; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
- A61P1/02—Stomatological preparations, e.g. drugs for caries, aphtae, periodontitis
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/02—Local antiseptics
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P37/00—Drugs for immunological or allergic disorders
- A61P37/08—Antiallergic agents
-
- 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
-
- 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
- A61Q17/005—Antimicrobial preparations
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Pharmacology & Pharmacy (AREA)
- Medicinal Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Communicable Diseases (AREA)
- Oncology (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Immunology (AREA)
- Dermatology (AREA)
- Pulmonology (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Cosmetics (AREA)
Abstract
The invention belongs to the technical field of silicon dioxide, and particularly relates to silicon dioxide with anti-allergy and antibacterial effects for toothpaste and a preparation method thereof. The preparation process provided by the invention prepares the silicon dioxide core particles with micropores under the conditions of low temperature, low concentration and acidity, adds dipotassium glycyrrhizinate at high temperature to enable the dipotassium glycyrrhizinate to be adsorbed in the micropores of the silicon dioxide core particles, finally generates a silicon dioxide shell on the surface of the core particles at high temperature, and adds PEG-6000 to control the particle size of the silicon dioxide, thus preparing the silicon dioxide for the toothpaste with anti-allergy and antibacterial effects. The silicon dioxide generated by the preparation process provided by the invention has small particle size, does not need to be crushed, is applied to toothpaste without adding other anti-sensitive antibacterial components, reduces the production cost of the silicon dioxide and the toothpaste, reduces the energy consumption and has good anti-sensitive antibacterial effect.
Description
Technical Field
The invention belongs to the technical field of silicon dioxide, and particularly relates to silicon dioxide with anti-allergy and antibacterial effects for toothpaste and a preparation method thereof.
Background
The most oral diseases such as halitosis, oral ulcer and gingival inflammation are caused by bacterial proliferation and infection in oral cavity, and halitosis is caused by inflammation in oral cavity, such as periodontitis and gingivitis. Dentinal sensitivity is a common condition of the oral cavity, with symptoms of sudden sensations of soreness and irritation when teeth are stimulated by cold, heat, acid, sweetness and mechanical action. The toothpaste has the effects of refreshing breath and cleaning teeth, and is helpful for oral diseases and tooth sensitivity of people.
Toothpaste with tooth sensitivity preventing and relieving effects and antibacterial effects is common in the market, wherein some of the toothpaste achieve sensitivity preventing effects by adding chemical substances of strontium salt, potassium salt, fluoride and the like, and achieve antibacterial effects by adding some trichloro sand or salts with silver and zinc ions, but the anti-sensitivity or antibacterial toothpaste needs to be added with anti-sensitivity antibacterial ingredients in a common toothpaste formula, and the more anti-sensitivity antibacterial ingredients are added into the toothpaste, the higher the cost is, the more the stability of the toothpaste is easily affected, and the toothpaste is not beneficial to long-term storage. The other method realizes the anti-sensitivity and anti-bacterial effects by improving the silicon dioxide in the toothpaste, but the initial particle size of the silicon dioxide for the toothpaste synthesized by reaction is generally larger, and the silicon dioxide for the toothpaste needs to be crushed to meet the application index of the toothpaste, and the smaller the crushed particle size is, the higher the energy consumption is, the higher the cost is, and the greater the pollution to the environment is.
Patent publication No. CN106821775B discloses an anti-allergy toothpaste and a preparation method thereof, and the formula components of the anti-allergy toothpaste comprise a sylvite anti-allergy component, a surfactant, a humectant, an abrasive and a thickening agent. The anti-allergy sylvite component accounts for 5-10% of the toothpaste by mass, and the surfactant is a mixture of at least one of an amino acid surfactant and an amphoteric surfactant and sodium dodecyl sulfate. Although the anti-allergy toothpaste has certain antibacterial performance, the stability of the toothpaste body is reduced due to the addition of the anti-allergy potassium salt component, and the long-term storage is not facilitated.
Patent publication No. CN111232995A discloses a preparation method and application of a silica for toothpaste for relieving tooth sensitivity, wherein the preparation process comprises the steps of synthesizing silica, filter pressing, drying, crushing, grinding and the like. The preparation method of the silicon dioxide has the advantages of large energy consumption and high production cost.
In conclusion, the technical problems of poor stability, high energy consumption, high production cost and the like generally exist in the prior art.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide silica for toothpaste with anti-allergy and antibacterial effects and a preparation method thereof. The silicon dioxide prepared by the preparation method provided by the invention has an anti-allergic and antibacterial effect, and the preparation process has no crushing process, so that the energy consumption is reduced, the cost is saved, and the environmental pollution is avoided.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of silica for toothpaste with anti-allergy and antibacterial effects comprises the following steps:
s1, respectively preparing a sodium silicate solution with the molar concentration of 1.0-1.2mol/L and a sulfuric acid solution with the molar concentration of 2.0-2.5 mol/L;
s2, respectively preparing a sodium silicate solution with the molar concentration of 2.0-2.2mol/L and a sulfuric acid solution with the molar concentration of 7.8-8.0 mol/L;
s3, adding 6-7m of solution into the reaction tank3Heating water to 60 deg.C, stirring at 25-35Hz, adding dropwise sodium silicate solution and sulfuric acid solution prepared in step S1, maintaining pH at 4-5, and adding sodium silicate solution dropwise at 2m3Stopping dripping the sodium silicate solution and the sulfuric acid solution, heating to 80 ℃, adding 6-8kg of dipotassium glycyrrhizinate into the reaction tank, and continuously stirring for 10min to obtain a mixed solution A;
s4, adding 1m to the mixed solution A prepared in the step S33Sodium silicate solution prepared in step S2 and 2m3Heating sodium sulfate solution with mass percent concentration of 5.5 percent to 80 ℃, stirring at the rotation speed of 25-35Hz, dropwise adding the sodium silicate solution and the sulfuric acid solution prepared in the step S2, keeping the pH value of the solution at 8-9 in the reaction process, and when the addition amount of the sodium silicate solution reaches 2m3Stopping dripping the sodium silicate solution and the sulfuric acid solution to prepare a mixed solution B;
s5, adding PEG-6000 into the residual sodium silicate solution prepared in the step S2, stirring uniformly, continuing to stir at the rotating speed of 25-35Hz, and dropwise adding the sulfuric acid solution prepared in the step S2 and the sodium silicate solution after the PEG-6000 is added until the total using amount of the sodium silicate solution is 4m3Stopping dripping the sodium silicate solution, continuously dripping the sulfuric acid solution until the pH value in the system is 3.5-4.5, and filtering to obtain silicon dioxide;
s6, press-filtering and washing the silicon dioxide prepared in the step S5, and drying the prepared silicon dioxide wet material to obtain the silicon dioxide wet material.
Further, the dropping speed of the sodium silicate solution in the step S3 of the preparation method of the silicon dioxide for toothpaste with anti-allergic and antibacterial effects is 9-10m3The dropping speed of the sulfuric acid solution is 3-3.5m3/h。
Further, the dropping speed of the sodium silicate solution in the step S4 of the preparation method of the silicon dioxide for toothpaste with anti-allergic and antibacterial effects is 13-14m3The dropping speed of the sulfuric acid solution is 3-3.5m3/h。
Further, the adding weight of PEG-6000 in the step S5 of the preparation method of the silica for the toothpaste with the anti-allergic and antibacterial effects is 4-8% of the mass of the residual sodium silicate solution.
Further, the dropping speed of the sulfuric acid solution in the step S5 of the preparation method of the silica for toothpaste with anti-allergic and antibacterial effects is 3-3.5m3The dropping speed of the sodium silicate solution added with PEG-6000 is 13-14m3/h。
Further, the preparation method of the silica for toothpaste with the anti-allergy and anti-bacterial effects has the pressure filtration pressure of 0.5-1.5Mpa and the drying temperature of 90-110 ℃ in the step S6.
The invention also provides silicon dioxide prepared by the preparation method of the toothpaste silicon dioxide with the anti-allergy and antibacterial effects and application of the silicon dioxide in toothpaste.
The preparation method of the silica for the toothpaste with the anti-allergy and anti-bacterial effects comprises the steps of firstly adopting the reaction under the acidic conditions of low temperature of 60 ℃, low acid-base concentration and pH value of 4-5 to generate silica initial particles with a plurality of microporous structures, finally raising the temperature to 80 ℃, and adding dipotassium glycyrrhizinate, wherein the molecular motion in a reaction solution is accelerated due to the temperature rise in a system, so that the large amount of adsorption of the microporous structures of the silica is facilitated, and the added dipotassium glycyrrhizinate is adsorbed in the micropores of the silica.
And the fourth step is to add high concentration water glass and sodium sulfate solution at 80 deg.c for acid-base dropping reaction to form one compact silica shell on the basis of the initial silica particle and to block the dipotassium glycyrrhizinate inside the pores inside the silica core. PEG-6000 is a non-ionic surfactant, and can be adsorbed on the surface of silicon dioxide particles when added into a reaction system, so that the silicon dioxide particles can be prevented from growing, the linking effect among colloidal particles can be achieved, and the long chains are intertwined to promote the agglomeration of the colloidal particles, so that the particle size in the system tends to be uniform.
Compared with the prior art, the silica for toothpaste with anti-allergy and antibacterial effects and the preparation method thereof provided by the invention have the following advantages:
(1) the silicon dioxide generated by the preparation method provided by the invention has small initial particle size, does not need to be crushed, and reduces the production cost and energy consumption;
(2) the preparation method provided by the invention cannot damage the internal structure of the silicon dioxide, and the micropores of the inner core of the silicon dioxide contain a large amount of dipotassium glycyrrhizinate, so that when the preparation method is applied to toothpaste, the stability of the toothpaste is not influenced, other tooth-sensitive and antibacterial components are not required to be additionally added, and the production cost of the toothpaste is reduced;
(3) the dipotassium glycyrrhizinate contained in the silicon dioxide provided by the invention has the functions of diminishing inflammation and resisting bacteria, and has certain efficacy on treating oral diseases such as oral ulcer, gingivitis, tooth sensitivity and the like;
(4) the preparation method provided by the invention has the advantages of simple process and controllable operation, and is favorable for realizing industrial production.
Detailed Description
The present invention will be further described below by way of specific embodiments, but the present invention is not limited to only the following examples. Various modifications can be made by those skilled in the art based on the basic idea of the invention, but it is within the scope of the invention as long as it does not depart from the basic idea of the invention.
Example 1 silica for toothpaste having anti-allergic and antibacterial effects
A preparation method of silica for toothpaste with anti-allergy and antibacterial effects comprises the following steps:
s1, respectively preparing a sodium silicate solution with the molar concentration of 1.0mol/L and a sulfuric acid solution with the molar concentration of 2.0 mol/L;
s2, respectively preparing a sodium silicate solution with the molar concentration of 2.0mol/L and a sulfuric acid solution with the molar concentration of 7.8 mol/L;
s3, adding 6m into the reaction tank3Heating water to 60 deg.C, stirring at 25Hz, and simultaneously dripping sodium silicate solution and sulfuric acid solution prepared in step S1 at a speed of 9m3The dropping speed of the sulfuric acid solution is 3m3H, keeping the pH value of the reaction process to be 4, and when the dropping amount of the sodium silicate solution is 2m3When the dropping is stopped, the sodium silicate solution and the sulfuric acid solution are droppedHeating to 80 deg.C, adding 6kg dipotassium glycyrrhizinate into the reaction tank, and stirring for 10min to obtain mixed solution A;
s4, adding 1m to the mixed solution A prepared in the step S33Sodium silicate solution prepared in step S2 and 2m3Heating sodium sulfate solution with mass percent concentration of 5.5 percent to 80 ℃, stirring at the rotation speed of 25Hz, and dropwise adding the sodium silicate solution and the sulfuric acid solution prepared in the step S2, wherein the dropwise adding speed of the sodium silicate solution is 13m3The dropping speed of the sulfuric acid solution is 3m3H, keeping the pH value of the reaction process to be 8, and when the addition amount of the sodium silicate solution reaches 2m3Stopping dripping the sodium silicate solution and the sulfuric acid solution to prepare a mixed solution B;
s5, adding PEG-6000 into the residual sodium silicate solution prepared in the step S2, wherein the adding weight of the PEG-6000 is 4% of the mass of the residual sodium silicate solution, stirring uniformly, continuing to stir at the rotating speed of 25Hz, and dropwise adding the sulfuric acid solution prepared in the step S2 and the sodium silicate solution after the PEG-6000 is added until the total using amount of the sodium silicate solution is 4m3When the process is carried out, the dropwise addition of the sodium silicate solution is stopped, the sulfuric acid solution is continuously added until the pH value in the system is 3.5, and the dropwise addition speed of the sulfuric acid solution is 3m3The dropping speed of the sodium silicate solution after adding PEG-6000 is 13m3H, filtering to prepare silicon dioxide;
s6, performing filter pressing and washing on the silicon dioxide prepared in the step S5, wherein the pressure of the filter pressing is 0.5Mpa, and drying the prepared silicon dioxide wet material at 90 ℃ to obtain the silicon dioxide wet material.
Example 2 silica for toothpaste having anti-allergic and antibacterial effects
A preparation method of silica for toothpaste with anti-allergy and antibacterial effects comprises the following steps:
s1, respectively preparing a sodium silicate solution with the molar concentration of 1.1mol/L and a sulfuric acid solution with the molar concentration of 2.1 mol/L;
s2, respectively preparing a sodium silicate solution with the molar concentration of 2.1mol/L and a sulfuric acid solution with the molar concentration of 7.9 mol/L;
s3, adding 6.2m into the reaction tank3Heating water to 60 deg.c,stirring at 28Hz, and simultaneously dripping the sodium silicate solution prepared in step S1 and the sulfuric acid solution at a sodium silicate solution dripping speed of 9.2m3The dropping speed of the sulfuric acid solution is 3.1m3H, keeping the pH value of the reaction process to be 4.2, and when the dropping amount of the sodium silicate solution is 2m3Stopping dripping the sodium silicate solution and the sulfuric acid solution, heating to 80 ℃, adding 8kg of dipotassium glycyrrhizinate into the reaction tank, and continuing stirring for 10min to obtain a mixed solution A;
s4, adding 1m to the mixed solution A prepared in the step S33Sodium silicate solution prepared in step S2 and 2m3Heating sodium sulfate solution with mass percent concentration of 5.5 percent to 80 ℃, stirring at the rotation speed of 28Hz, and dropwise adding the sodium silicate solution and the sulfuric acid solution prepared in the step S2, wherein the dropwise adding speed of the sodium silicate solution is 13.2m3The dropping speed of the sulfuric acid solution is 3.1m3H, keeping the pH value in the reaction process to be 8.2, and when the addition amount of the sodium silicate solution reaches 2m3Stopping dripping the sodium silicate solution and the sulfuric acid solution to prepare a mixed solution B;
s5, adding PEG-6000 into the residual sodium silicate solution prepared in the step S2, wherein the adding weight of the PEG-6000 is 5% of the mass of the residual sodium silicate solution, stirring uniformly, continuing stirring at the rotating speed of 28Hz, and dropwise adding the sulfuric acid solution prepared in the step S2 and the sodium silicate solution after the PEG-6000 is added until the total using amount of the sodium silicate solution is 4m3When the process is finished, the dropwise addition of the sodium silicate solution is stopped, the sulfuric acid solution is continuously added until the pH value in the system is 3.7, and the dropwise addition speed of the sulfuric acid solution is 3.1m3The dropping speed of the sodium silicate solution added with PEG-6000 is 13.2m3H, filtering to prepare silicon dioxide;
s6, performing filter pressing and washing on the silicon dioxide prepared in the step S5, wherein the pressure of the filter pressing is 0.7Mpa, and drying the prepared silicon dioxide wet material at 95 ℃ to obtain the silicon dioxide wet material.
Example 3 silica for toothpaste having anti-allergic and antibacterial effects
A preparation method of silica for toothpaste with anti-allergy and antibacterial effects comprises the following steps:
s1, respectively preparing a sodium silicate solution with the molar concentration of 1.2mol/L and a sulfuric acid solution with the molar concentration of 2.4 mol/L;
s2, respectively preparing a sodium silicate solution with the molar concentration of 2.0mol/L and a sulfuric acid solution with the molar concentration of 7.9 mol/L;
s3, adding 6.3m into the reaction tank3Heating water to 60 deg.C, stirring at 30Hz, and simultaneously dripping sodium silicate solution and sulfuric acid solution prepared in step S1 at a speed of 9.6m3The dropping speed of the sulfuric acid solution is 3.3m3H, keeping the pH value of the reaction process to be 4.8, and when the dropping amount of the sodium silicate solution is 2m3Stopping dripping the sodium silicate solution and the sulfuric acid solution, heating to 80 ℃, adding 6.4kg of dipotassium glycyrrhizinate into the reaction tank, and continuously stirring for 10min to obtain a mixed solution A;
s4, adding 1m to the mixed solution A prepared in the step S33Sodium silicate solution prepared in step S2 and 2m3Heating sodium sulfate solution with mass percent concentration of 5.5 percent to 80 ℃, stirring at the rotation speed of 30Hz, and dropwise adding the sodium silicate solution and the sulfuric acid solution prepared in the step S2, wherein the dropwise adding speed of the sodium silicate solution is 13.4m3The dropping speed of the sulfuric acid solution is 3.3m3H, keeping the pH value in the reaction process to be 8.5, and when the addition amount of the sodium silicate solution reaches 2m3Stopping dripping the sodium silicate solution and the sulfuric acid solution to prepare a mixed solution B;
s5, adding PEG-6000 into the residual sodium silicate solution prepared in the step S2, wherein the adding weight of the PEG-6000 is 7% of the mass of the residual sodium silicate solution, stirring uniformly, continuing to stir at the rotating speed of 30Hz, and dropwise adding the sulfuric acid solution prepared in the step S2 and the sodium silicate solution after the PEG-6000 is added until the total using amount of the sodium silicate solution is 4m3When the process is finished, the dropwise addition of the sodium silicate solution is stopped, the sulfuric acid solution is continuously added until the pH value in the system is 4.1, and the dropwise addition speed of the sulfuric acid solution is 3.2m3The dropping speed of the sodium silicate solution added with PEG-6000 is 13.6m3H, filtering to prepare silicon dioxide;
s6, performing filter pressing and washing on the silicon dioxide prepared in the step S5, wherein the pressure of the filter pressing is 0.9Mpa, and drying the prepared silicon dioxide wet material at 100 ℃ to obtain the silicon dioxide wet material.
Example 4 silica for toothpaste having anti-allergic and antibacterial effects
A preparation method of silica for toothpaste with anti-allergy and antibacterial effects comprises the following steps:
s1, respectively preparing a sodium silicate solution with the molar concentration of 1.15mol/L and a sulfuric acid solution with the molar concentration of 2.3 mol/L;
s2, respectively preparing a sodium silicate solution with the molar concentration of 2.2mol/L and a sulfuric acid solution with the molar concentration of 8.0 mol/L;
s3, adding 6.6m into the reaction tank3Heating water to 60 deg.C, stirring at 33Hz, and simultaneously dripping sodium silicate solution and sulfuric acid solution prepared in step S1 at a speed of 9.4m3The dropping speed of the sulfuric acid solution is 3.4m3H, keeping the pH value of the reaction process to be 4.5, and when the dropping amount of the sodium silicate solution is 2m3Stopping dripping the sodium silicate solution and the sulfuric acid solution, heating to 80 ℃, adding 6.2kg of dipotassium glycyrrhizinate into the reaction tank, and continuously stirring for 10min to obtain a mixed solution A;
s4, adding 1m to the mixed solution A prepared in the step S33Sodium silicate solution prepared in step S2 and 2m3Heating sodium sulfate solution with mass percent concentration of 5.5 percent to 80 ℃, stirring at the rotating speed of 33Hz, and dropwise adding the sodium silicate solution and the sulfuric acid solution prepared in the step S2, wherein the dropwise adding speed of the sodium silicate solution is 14m3The dropping speed of the sulfuric acid solution is 3.5m3H, keeping the pH value of the reaction process to be 9, and when the addition amount of the sodium silicate solution reaches 2m3Stopping dripping the sodium silicate solution and the sulfuric acid solution to prepare a mixed solution B;
s5, adding PEG-6000 into the residual sodium silicate solution prepared in the step S2, wherein the adding weight of the PEG-6000 is 8% of the mass of the residual sodium silicate solution, stirring uniformly, continuing to stir at the rotating speed of 33Hz, and dropwise adding the sulfuric acid solution prepared in the step S2 and the sodium silicate solution after the PEG-6000 is added until the total using amount of the sodium silicate solution is 4m3When the process is finished, the dropwise addition of the sodium silicate solution is stopped, the sulfuric acid solution is continuously added until the pH value in the system is 4.3, and the dropwise addition speed of the sulfuric acid solution is 3.4m3The dropping speed of the sodium silicate solution added with PEG-6000 is 13.4m3H, filtering to prepare silicon dioxide;
s6, performing filter pressing and washing on the silicon dioxide prepared in the step S5, wherein the pressure of the filter pressing is 1.5Mpa, and drying the prepared silicon dioxide wet material at 105 ℃ to obtain the silicon dioxide wet material.
Example 5 silica for toothpaste having anti-allergic and antibacterial effects
A preparation method of silica for toothpaste with anti-allergy and antibacterial effects comprises the following steps:
s1, respectively preparing a sodium silicate solution with the molar concentration of 1.1mol/L and a sulfuric acid solution with the molar concentration of 2.5 mol/L;
s2, respectively preparing a sodium silicate solution with the molar concentration of 2.1mol/L and a sulfuric acid solution with the molar concentration of 7.8 mol/L;
s3, adding 7m into the reaction tank3Heating water to 60 deg.C, stirring at 35Hz, and simultaneously dripping sodium silicate solution and sulfuric acid solution prepared in step S1 at a speed of 10m3The dropping speed of the sulfuric acid solution is 3.5m3H, keeping the pH value of the reaction process to be 5, and when the dropping amount of the sodium silicate solution is 2m3Stopping dripping the sodium silicate solution and the sulfuric acid solution, heating to 80 ℃, adding 6.8kg of dipotassium glycyrrhizinate into the reaction tank, and continuously stirring for 10min to obtain a mixed solution A;
s4, adding 1m to the mixed solution A prepared in the step S33Sodium silicate solution prepared in step S2 and 2m3Heating sodium sulfate solution with mass percent concentration of 5.5 percent to 80 ℃, stirring at the rotating speed of 35Hz, and dropwise adding the sodium silicate solution and the sulfuric acid solution prepared in the step S2, wherein the dropwise adding speed of the sodium silicate solution is 13.8m3The dropping speed of the sulfuric acid solution is 3.4m3H, keeping the pH value of the reaction process to be 8.7, and when the addition amount of the sodium silicate solution reaches 2m3Stopping dripping the sodium silicate solution and the sulfuric acid solution to prepare a mixed solution B;
s5, adding PEG-6000 into the residual sodium silicate solution prepared in the step S2, wherein the adding weight of the PEG-6000 is 6% of the mass of the residual sodium silicate solution, stirring uniformly, continuing to stir at the rotating speed of 35Hz, and dropwise adding the sulfuric acid solution prepared in the step S2 and the sodium silicate solution after the PEG-6000 is added until the total using amount of the sodium silicate solution is 4m3When the process is finished, the dropwise addition of the sodium silicate solution is stopped, the sulfuric acid solution is continuously added until the pH value in the system is 4.5, and the dropwise addition speed of the sulfuric acid solution is 3.5m3The dropping speed of the sodium silicate solution after adding PEG-6000 is 14m3H, filtering to prepare silicon dioxide;
s6, performing filter pressing and washing on the silicon dioxide prepared in the step S5, wherein the pressure of the filter pressing is 1.2Mpa, and drying the prepared silicon dioxide wet material at 110 ℃ to obtain the silicon dioxide wet material.
Comparative example 1 silica for toothpaste
The silica for toothpaste in this comparative example was prepared in a similar manner to example 2.
The comparative example differs from example 2 in that: the reaction temperature in step S3 of this comparative example was maintained at 80 ℃.
Comparative example 2 silica for toothpaste
The silica for toothpaste in this comparative example was prepared in a similar manner to example 2.
The comparative example differs from example 2 in that: the pH during the reaction was maintained at 7 in step S3 of this comparative example.
Comparative example 3 silica for toothpaste
The silica for toothpaste in this comparative example was prepared in a similar manner to example 2.
The comparative example differs from example 2 in that: the amount of PEG-6000 added in step S5 of this comparative example was 2% by mass of the remaining sodium silicate solution.
Comparative example 4 silica for toothpaste
The silica for toothpaste in this comparative example was prepared in a similar manner to example 2.
The comparative example differs from example 2 in that: this comparative example, step S5, PEG-6000 was addedThe dropping speed of the sodium silicate solution is 10m3/h。
Test example I, silica Performance test
Test samples: silicas obtained in examples 1 to 5, comparative example 1 and comparative examples 3 to 4;
the test method comprises the following steps: detecting the apparent density, the specific surface area and the median particle size of a test sample by referring to GB/T32661-2016 spherical silica powder; determining the RDA value of the silicon dioxide by adopting a radioactive tracing method;
and (3) test results: the test results are shown in Table 1.
Table 1 silica performance test results
| Group of | Apparent density g/cm3 | Specific surface area m2/g | Median particle diameter μm | RDA value |
| Example 1 | 0.51 | 60 | 11 | 204 |
| Example 2 | 0.59 | 69 | 9 | 219 |
| Example 3 | 0.54 | 62 | 10 | 213 |
| Example 4 | 0.57 | 67 | 13 | 207 |
| Example 5 | 0.52 | 64 | 10 | 215 |
| Comparative example 1 | 0.37 | 43 | 25 | 106 |
| Comparative example 2 | 0.41 | 38 | 19 | 134 |
| Comparative example 3 | 0.35 | 47 | 28 | 127 |
| Comparative example 4 | 0.44 | 45 | 31 | 109 |
As can be seen from Table 1, the apparent density of the silica for toothpaste having an anti-sensitivity antibacterial effect provided by the present invention is 0.51 to 0.59g/cm3The specific surface area is 60-69m2The silica for toothpaste has the advantages of small particle size and good abrasive property, does not need to be additionally crushed when being applied to toothpaste, and can bring good cleaning effect to toothpaste. Among them, the silica for toothpaste having an anti-sensitivity antibacterial effect obtained in example 2 is the best example in all aspects of performance.
Comparative example 1 changed the temperature during the silica core particle formation reaction compared to example 2, but the properties of the produced silica were degraded to various degrees, which indicates that low temperature is a necessary condition for the formation of silica core particles. Comparative examples 3 and 4 change the amount of PEG-6000 used in the formation of the silica shell and the dropping rate of the sodium silicate solution to which PEG-6000 was added, respectively, but the properties of the prepared silica were decreased in various aspects, which shows that PEG-6000 has excellent control ability in the reaction process for the density, particle size, etc. of the formed silica.
Test example two evaluation of silica application
Test samples: toothpaste prepared using the silicas obtained in examples 1-5 and comparative example 2;
the specific toothpaste formulations are shown in table 2.
TABLE 2 toothpaste formula with antibacterial and antiallergic effects
The test method comprises the following steps: testing the stability of the toothpaste: respectively placing the test samples in a 25 ℃ room temperature shelf, a-8 ℃ refrigerator and a 45 ℃ oven for 7 days, 1 month and 3 months respectively, and observing whether the toothpaste body is deteriorated;
and (3) sensitivity resistance test: 120 patients suffering from tooth sensitivity are selected, male and female are unlimited, the groups are averagely divided into 5 groups, 20 patients in each group use toothpaste A, toothpaste B, toothpaste C, toothpaste D, toothpaste E and toothpaste F respectively, the use period is 3 months, and the test samples are used for brushing teeth normally in the morning and at night every day in the use period. After 3 months, evaluating by using three methods of mechanical stimulation, temperature test and subjective evaluation respectively, detecting at least 3 teeth by each person, and counting the number of effective persons, the number of ineffective persons and the effective rate of each group;
mechanical stimulation: lightly stroking the sensitive part of the tooth by using a probe to judge;
temperature test: mouth wash test with purified water at 15 deg.C;
evaluation criteria: and (3) mechanical testing: 0-no discomfort; 1 ═ mild discomfort or pain; 2-moderate pain; 3 ═ severe pain and persistent; and (3) temperature testing: 0-no discomfort; 1 ═ mild discomfort or pain; 2-moderate pain; 3 ═ severe pain and persistent; subjective evaluation: 0-no change; 1, improvement; -1 ═ weighting.
And (3) antibacterial property test: weighing 1g of toothpaste body and an aseptic triangular flask respectively, sucking quantitative aseptic normal saline by using an aseptic straw to dissolve the toothpaste body to prepare toothpaste liquid with the mass percentage concentration of 30%, separating by using a centrifugal machine, taking supernatant, and removing filter residue; culturing staphylococcus aureus and pseudomonas aeruginosa by using a broth culture medium; picking colony with sterile inoculating loop, uniformly coating on suitable plate culture medium, drying, punching hole on the plate with sterile punch, adding 1mL of toothpaste liquid with sterile pipette, culturing at 37 deg.C for 8-12h, and measuring the diameter of the zone.
And (3) test results: the test results are shown in tables 3, 4 and 5.
Table 3 toothpaste stability test results
As can be seen from Table 3, the silica having anti-sensitivity antibacterial effect provided by the present invention does not affect the high and low temperature stability of the toothpaste when applied to the toothpaste.
TABLE 4 toothpaste anti-allergy Effect test results
| Toothpaste tube | Number of valid persons (human) | Invalid number of people (human) | Total number (human) | Effective rate (%) |
| A | 16 | 4 | 20 | 80 |
| B | 18 | 2 | 20 | 90 |
| C | 15 | 5 | 20 | 75 |
| D | 16 | 4 | 20 | 80 |
| E | 14 | 6 | 20 | 70 |
| F | 5 | 11 | 20 | 25 |
As can be seen from table 4, the silica for toothpaste with anti-allergy and antibacterial effects provided by the present invention has good anti-allergy effects when applied to toothpaste, wherein the toothpaste prepared by applying the silica for toothpaste with anti-allergy and antibacterial effects in example 2 has the best anti-allergy effects, and the anti-allergy effective rate reaches 90% within three months, which is the best embodiment of the present invention.
Compared with toothpaste B, toothpaste F uses the silica prepared in comparative example 2, and comparative example 2 changes the pH value in the process of generating the silica core particles compared with example 2, but the anti-sensitivity effect is greatly reduced, because the increase of the pH value changes the structure of the silica core particles and reduces the number of pore structures on the surface of the silica core particles, so that the adsorption amount of dipotassium glycyrrhizinate is reduced, and the anti-sensitivity effect is poor.
TABLE 5 toothpaste antibacterial Effect test results
As can be seen from table 5, the silica for toothpaste having an anti-sensitivity antibacterial effect provided by the present invention has a good inhibitory effect on staphylococcus aureus and pseudomonas aeruginosa when applied to toothpaste, and oral diseases such as oral ulcer and gingivitis can be effectively improved after 8 to 12 hours of toothpaste using the silica for toothpaste having an anti-sensitivity antibacterial effect provided by the present invention.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Those skilled in the art will recognize that changes may be made to the embodiments described above without departing from the spirit and scope of the invention. Therefore, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the technical spirit of the present invention are covered by the claims of the present invention.
Claims (7)
1. A preparation method of silica for toothpaste with anti-allergy and antibacterial effects is characterized by comprising the following steps:
s1, respectively preparing a sodium silicate solution with the molar concentration of 1.0-1.2mol/L and a sulfuric acid solution with the molar concentration of 2.0-2.5 mol/L;
s2, respectively preparing a sodium silicate solution with the molar concentration of 2.0-2.2mol/L and a sulfuric acid solution with the molar concentration of 7.8-8.0 mol/L;
s3, adding 6-7m of solution into the reaction tank3Heating water to 60 deg.C, stirring at 25-35Hz, adding dropwise sodium silicate solution and sulfuric acid solution prepared in step S1, maintaining pH at 4-5, and adding sodium silicate solution dropwise at 2m3When the addition of the sodium silicate solution and sulfur is stoppedHeating the acid solution to 80 deg.C, adding 6-8kg dipotassium glycyrrhizinate into the reaction tank, and stirring for 10min to obtain mixed solution A;
s4, adding 1m to the mixed solution A prepared in the step S33Sodium silicate solution prepared in step S2 and 2m3Heating sodium sulfate solution with mass percent concentration of 5.5 percent to 80 ℃, stirring at the rotation speed of 25-35Hz, dropwise adding the sodium silicate solution and the sulfuric acid solution prepared in the step S2, keeping the pH value of the solution at 8-9 in the reaction process, and when the addition amount of the sodium silicate solution reaches 2m3Stopping dripping the sodium silicate solution and the sulfuric acid solution to prepare a mixed solution B;
s5, adding PEG-6000 into the residual sodium silicate solution prepared in the step S2, stirring uniformly, continuing to stir at the rotating speed of 25-35Hz, and dropwise adding the sulfuric acid solution prepared in the step S2 and the sodium silicate solution after the PEG-6000 is added until the total using amount of the sodium silicate solution is 4m3Stopping dripping the sodium silicate solution, continuously dripping the sulfuric acid solution until the pH value in the system is 3.5-4.5, and filtering to obtain silicon dioxide;
s6, press-filtering and washing the silicon dioxide prepared in the step S5, and drying the prepared silicon dioxide wet material to obtain the silicon dioxide wet material.
2. The method for preparing silica for toothpaste having anti-sensitivity antibacterial effect according to claim 1, wherein the dropping speed of the sodium silicate solution in the step S3 is 9-10m3The dropping speed of the sulfuric acid solution is 3-3.5m3/h。
3. The method for preparing silica for toothpaste having anti-sensitivity antibacterial effect according to claim 1, wherein the dropping speed of the sodium silicate solution in the step S4 is 13 to 14m3The dropping speed of the sulfuric acid solution is 3-3.5m3/h。
4. The method for preparing silica for toothpaste having anti-sensitivity antibacterial effect according to claim 1, wherein the weight of PEG-6000 added in step S5 is 4-8% of the mass of the remaining sodium silicate solution.
5. The method for preparing silica for toothpaste having anti-sensitivity antibacterial effect according to claim 1, wherein the dropping speed of sulfuric acid solution in step S5 is 3-3.5m3The dropping speed of the sodium silicate solution added with PEG-6000 is 13-14m3/h。
6. The method for preparing silica for toothpaste having anti-sensitivity antibacterial effect according to claim 1, wherein the pressure filtration in the step S6 is 0.5 to 1.5Mpa and the drying temperature is 90 to 110 ℃.
7. A silica obtained by the method for producing a silica for toothpaste having an anti-sensitivity antibacterial effect according to any one of claims 1 to 6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010753367.6A CN111874918B (en) | 2020-07-30 | 2020-07-30 | Silica for toothpaste with anti-allergy and antibacterial effects and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010753367.6A CN111874918B (en) | 2020-07-30 | 2020-07-30 | Silica for toothpaste with anti-allergy and antibacterial effects and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111874918A true CN111874918A (en) | 2020-11-03 |
| CN111874918B CN111874918B (en) | 2021-02-19 |
Family
ID=73204663
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010753367.6A Active CN111874918B (en) | 2020-07-30 | 2020-07-30 | Silica for toothpaste with anti-allergy and antibacterial effects and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111874918B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112870093A (en) * | 2021-01-19 | 2021-06-01 | 金三江(肇庆)硅材料股份有限公司 | Silica-coated medicinal powder particle and preparation method thereof |
| CN117224446A (en) * | 2023-10-27 | 2023-12-15 | 广东时尚女孩生物科技有限公司 | A kind of mint ointment with moisturizing and soothing function and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070003465A1 (en) * | 2005-06-29 | 2007-01-04 | Yung-Hui Huang | Method for making precipitated silica compositions and products thereof |
| CN103435053A (en) * | 2013-09-04 | 2013-12-11 | 沈阳化工大学 | Method for preparing high-dispersion nano white black carbon from sodium silicate |
| CN105236415A (en) * | 2015-09-02 | 2016-01-13 | 广州市飞雪材料科技有限公司 | Core-shell-type precipitated silicon dioxide and preparation method thereof |
| US20160206523A1 (en) * | 2015-01-21 | 2016-07-21 | Chattem Inc. | Oral composition for xerostomia |
| CN106672986A (en) * | 2010-07-23 | 2017-05-17 | 罗地亚管理公司 | Precipitated silica production process |
| CN110755337A (en) * | 2019-12-11 | 2020-02-07 | 苏州清馨健康科技有限公司 | Anti-allergy repairing toothpaste |
-
2020
- 2020-07-30 CN CN202010753367.6A patent/CN111874918B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070003465A1 (en) * | 2005-06-29 | 2007-01-04 | Yung-Hui Huang | Method for making precipitated silica compositions and products thereof |
| CN106672986A (en) * | 2010-07-23 | 2017-05-17 | 罗地亚管理公司 | Precipitated silica production process |
| CN103435053A (en) * | 2013-09-04 | 2013-12-11 | 沈阳化工大学 | Method for preparing high-dispersion nano white black carbon from sodium silicate |
| US20160206523A1 (en) * | 2015-01-21 | 2016-07-21 | Chattem Inc. | Oral composition for xerostomia |
| CN105236415A (en) * | 2015-09-02 | 2016-01-13 | 广州市飞雪材料科技有限公司 | Core-shell-type precipitated silicon dioxide and preparation method thereof |
| CN110755337A (en) * | 2019-12-11 | 2020-02-07 | 苏州清馨健康科技有限公司 | Anti-allergy repairing toothpaste |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112870093A (en) * | 2021-01-19 | 2021-06-01 | 金三江(肇庆)硅材料股份有限公司 | Silica-coated medicinal powder particle and preparation method thereof |
| CN117224446A (en) * | 2023-10-27 | 2023-12-15 | 广东时尚女孩生物科技有限公司 | A kind of mint ointment with moisturizing and soothing function and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111874918B (en) | 2021-02-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111874918B (en) | Silica for toothpaste with anti-allergy and antibacterial effects and preparation method thereof | |
| CN115444795B (en) | A kind of peony antibacterial shower lotion | |
| CN107251906B (en) | Nano silver complex solution and preparation method thereof | |
| CN108837159A (en) | A kind of nano antibacterial agent and preparation method thereof | |
| CN103891775A (en) | Zinc-carrying nano organic montmorillonite antimicrobial agent and preparation method thereof | |
| EP0296441A2 (en) | Use of insoluble, polyfunctional quaternary ammonium compounds for the adsorptive binding of microorganisms | |
| WO2020019903A1 (en) | Silicon dioxide for toothpaste having antibacterial properties and preparation method therefor | |
| CN111232995B (en) | Preparation method and application of toothpaste silicon dioxide for relieving tooth sensitivity | |
| CN115137669A (en) | Preparation method of silicon dioxide loaded nano-silver composite material | |
| CN106120313A (en) | The preparation method of a kind of antimildew and antibacterial agent and the application in weaving face fabric thereof | |
| CN107981441B (en) | A kind of Medical efficient bactericidal mask | |
| CN108403455A (en) | A method of it doing inorganic antibacterial filler with diatomite and makes toothpaste | |
| CN106432534B (en) | A kind of liquid curdlan and its production method | |
| CN105885063B (en) | A kind of preparation method of the medical temperature-sensitive hydrogel containing nano silver | |
| CN104724922B (en) | A kind of bioglass particles material and its preparation technology | |
| CN119499107B (en) | Antibacterial hand sanitizer and preparation method thereof | |
| CN105287244A (en) | Montmorillonite-containing functional toothpaste and preparation method thereof | |
| CN118370807B (en) | Composition for inhibiting Porphyromonas gingivalis and preparation method and application thereof | |
| CN119280082B (en) | Tooth polishing agent with antibacterial effect and preparation method thereof | |
| CN111700813A (en) | Moisturizing cosmetic, moisturizing mask and modified attapulgite | |
| CN117898971A (en) | Sodium hyaluronate chlorhexidine antibacterial composition and preparation method and application thereof | |
| CN110840788A (en) | Toothpaste formula | |
| CN117224437A (en) | Composite anti-dandruff shampoo | |
| CN109893269B (en) | Bite block pad capable of reducing bacteria attachment rate | |
| Angelova et al. | ANTIFUNGAL ACTIVITY OF SILVER DOPED HYBRIDS BASED ON SILICA AND CELLULOSE DERIVATES AGAINST ASPERGILLUS NIGER. |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |