CN115321549B - Preparation method of precipitated silica for toothpaste thickener - Google Patents
Preparation method of precipitated silica for toothpaste thickener Download PDFInfo
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- CN115321549B CN115321549B CN202211061096.3A CN202211061096A CN115321549B CN 115321549 B CN115321549 B CN 115321549B CN 202211061096 A CN202211061096 A CN 202211061096A CN 115321549 B CN115321549 B CN 115321549B
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- toothpaste
- water glass
- thickener
- sulfuric acid
- precipitated silica
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 216
- 229940034610 toothpaste Drugs 0.000 title claims abstract description 108
- 239000000606 toothpaste Substances 0.000 title claims abstract description 108
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 104
- 239000002562 thickening agent Substances 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 102
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 76
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 68
- 238000006243 chemical reaction Methods 0.000 claims abstract description 67
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims abstract description 22
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 20
- 230000001105 regulatory effect Effects 0.000 claims abstract description 19
- 238000010521 absorption reaction Methods 0.000 claims abstract description 10
- 230000001276 controlling effect Effects 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 33
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 9
- 239000004115 Sodium Silicate Substances 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- 238000004537 pulping Methods 0.000 claims description 8
- 238000005086 pumping Methods 0.000 claims description 8
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 8
- 238000001694 spray drying Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 208000002064 Dental Plaque Diseases 0.000 abstract description 3
- 206010044029 Tooth deposit Diseases 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 100
- 230000000052 comparative effect Effects 0.000 description 11
- OVBPIULPVIDEAO-LBPRGKRZSA-N folic acid Chemical compound C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-LBPRGKRZSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 8
- 238000004140 cleaning Methods 0.000 description 6
- OVBPIULPVIDEAO-UHFFFAOYSA-N N-Pteroyl-L-glutaminsaeure Natural products C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)NC(CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-UHFFFAOYSA-N 0.000 description 5
- 229960000304 folic acid Drugs 0.000 description 5
- 235000019152 folic acid Nutrition 0.000 description 5
- 239000011724 folic acid Substances 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000001680 brushing effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 210000000214 mouth Anatomy 0.000 description 2
- 230000035935 pregnancy Effects 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 239000000341 volatile oil Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 206010006326 Breath odour Diseases 0.000 description 1
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 1
- 206010018276 Gingival bleeding Diseases 0.000 description 1
- 208000032139 Halitosis Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 235000004347 Perilla Nutrition 0.000 description 1
- 244000124853 Perilla frutescens Species 0.000 description 1
- 241001085205 Prenanthella exigua Species 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 241000234314 Zingiber Species 0.000 description 1
- 235000006886 Zingiber officinale Nutrition 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000000551 dentifrice Substances 0.000 description 1
- 230000003467 diminishing effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 210000000887 face Anatomy 0.000 description 1
- 235000008397 ginger Nutrition 0.000 description 1
- 208000007565 gingivitis Diseases 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000010517 secondary reaction Methods 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229940095688 toothpaste product Drugs 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
- 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
-
- 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
- C01P2006/12—Surface area
-
- 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
- C01P2006/14—Pore volume
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- 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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- 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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/65—Chroma (C*)
-
- 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
- C01P2006/80—Compositional purity
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Cosmetics (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to the technical field of toothpaste thickeners, and discloses a preparation method of precipitated silica for a toothpaste thickener, which comprises the following steps: (1) Firstly, preparing a water glass solution and a sulfuric acid solution; (2) Adding sulfuric acid solution into a reaction kettle, regulating the temperature of the reaction kettle, firstly adding tetrasodium pyrophosphate, then dropwise adding water glass solution, controlling the reaction pH after the water glass solution is dropwise added, then continuously adding sulfuric acid solution until the reaction pH is 4.0-5.0, regulating the temperature, and preserving heat; (3) obtaining silica particles; (4) Crushing the obtained silicon dioxide particles to obtain precipitated silicon dioxide for the toothpaste thickener; the precipitated silica for the toothpaste thickener prepared by the invention has the product friction value RDA in the range of 100-150, the RDA on the toothpaste refers to the friction value of the toothpaste, the higher the value is, the higher the representative friction force is, the stronger the capability of removing dental plaque and tartar is, the water absorption is higher than 50ml/20g, and the specific surface area is 70-110m 2 In the range of/g.
Description
Technical Field
The invention relates to the technical field of toothpaste thickeners, in particular to a preparation method of precipitated silica for a toothpaste thickener.
Background
The toothpaste is a cleaning product commonly used in daily life, is a dentifrice, is generally gel, can be smeared on a toothbrush generally, is used for cleaning teeth, keeps the teeth beautiful and bright white, has a long history, is a health care product for cleaning the teeth, is an auxiliary product for brushing teeth, has the functions of friction and plaque removal, cleaning and polishing the tooth surface, and enables the oral cavity to be fresh
The toothpaste mainly comprises two parts, wherein one part is for removing halitosis and peculiar smell, inhibiting bacteria and diminishing inflammation, and refreshing breath and oral cavity; and secondly, the tooth care and moth prevention function is realized, so that the teeth are protected.
For example, the prior art publication number is CN 105267080B, and the invention discloses a folic acid toothpaste and a preparation method thereof. The folic acid toothpaste contains folic acid 0.005-0.1 wt%, ginger volatile oil or extract 0.01-10 wt% and perilla leaf volatile oil or extract 0.01-10 wt%, and is prepared with common supplementary material and through certain toothpaste preparing process. The invention also provides a preparation method of the folic acid toothpaste. The folic acid toothpaste provided by the invention has the effects of relieving gingivitis and gingival bleeding during pregnancy and postpartum, and is a compound toothpaste especially suitable for preventing nausea and vomiting caused by tooth brushing during pregnancy.
China is a large country for producing and consuming toothpaste, but the consumption of the silicon dioxide serving as a constituent component of the toothpaste is not large at present, the toothpaste product faces more vigorous market competition, the importance of the market on the quality of the toothpaste is also increased, and the silicon dioxide serving as a thickener of the toothpaste with excellent performance is expected to be applied in a wider range.
Based on the above, we propose a preparation method of precipitated silica for toothpaste thickener, which is hopeful to solve the defects in the prior art.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a preparation method of precipitated silica for a toothpaste thickener.
(II) technical scheme
In order to achieve the above purpose, the present invention provides the following technical solutions:
a method for preparing precipitated silica for a toothpaste thickener comprising:
(1) Firstly, preparing a water glass solution, adding sodium silicate into deionized water, and stirring for 40min at a rotating speed of 200-250r/min to obtain a water glass solution with 13-18 wt%;
preparing sulfuric acid solution, slowly adding sulfuric acid into deionized water, and stirring while adding until the solution is uniformly mixed to obtain sulfuric acid solution with the mass fraction of 40-50%;
(2) Adding sulfuric acid solution into a reaction kettle, regulating the temperature of the reaction kettle to 80 ℃, then under the condition of stirring, firstly adding tetrasodium pyrophosphate, then dropwise adding water glass solution, controlling the reaction pH to 8.0-9.0 after the water glass solution is dropwise added, reacting for 50-60min, then continuously adding sulfuric acid solution until the reaction pH is 4.0-5.0, then regulating the temperature to 85-95 ℃, and preserving heat;
(3) Pumping the reaction kettle to vacuum under the condition that the pH value is kept in the range of 4.5-5.0, then carrying out secondary feeding, dropwise adding water glass solution with the same amount as that in the step (2) into the reaction kettle, continuously adding sulfuric acid solution after the dropwise adding of the water glass solution is finished until the reaction pH value is controlled in the range of 4.0-4.2, stirring and aging for 30min, and then carrying out filter pressing, washing, pulping and spray drying to obtain silicon dioxide particles;
(4) The obtained silica particles are crushed to an average particle size of 8-10 microns to obtain precipitated silica for toothpaste thickener.
As a further technical scheme, the modulus of the water glass solution is 3.3-3.5, and the transparency is more than 210mm.
As a further technical scheme, the conductivity of the deionized water is 15 mu s/cm.
As a further technical scheme: the adding amount of the tetrasodium pyrophosphate is 0.8-1.2% of the mass of the water glass solution.
As a further technical scheme, the vacuum degree of the vacuumized air is 0.02-0.05Pa.
As a further embodiment, the RDA rub value of the precipitated silica for the toothpaste thickener is between 100 and 150.
As a further technical scheme: the pH of the precipitated silica for the toothpaste thickener is between 5.5 and 8.5.
As a further technical scheme: the purity of the silicon dioxide in the precipitated silicon dioxide for the toothpaste thickener is more than or equal to 96 percent.
As a further technical scheme: the toothpaste thickener has a water absorption of < 50ml/20g with precipitated silica.
As a further technical scheme: the precipitated silica for the toothpaste thickener has a refractive index of 1.43-1.46N.
The invention can improve the supersaturation degree of the silicon dioxide generated by the reaction in the reaction mother liquor, the reaction rate and the reaction progress, ensure that the primary particles with small silicon dioxide are rapidly dissolved and grown into large regular spherical particles, reduce the specific surface area of the silicon dioxide, and increase the light transmittance and the fluidity of the prepared precipitated silicon dioxide, thereby improving the friction coefficient and the particle strength of the precipitated silicon dioxide, improving the friction value RDA, being introduced into toothpaste as a thickening agent, improving the capability of removing dental plaque and tartar of the toothpaste, and meeting various technical indexes of the silicon dioxide abrasive for the toothpaste.
According to the invention, through carrying out secondary reaction by vacuumizing in the reaction process, the structure of the silicon dioxide synthesis reaction can be controlled to form a three-dimensional space network structure, so that the friction coefficient and the particle strength of the product are improved, meanwhile, moderate abrasion can be ensured, obvious damage to gums can not be caused, active ingredients in the toothpaste can be effectively absorbed and released, and the toothpaste has excellent compatibility with various active ingredients in the toothpaste.
The precipitated silica for the toothpaste thickener has lower refractive index, when the liquid phase of the toothpaste is similar to the refractive index of the precipitated silica for the toothpaste thickener, transparent toothpaste can be prepared, the liquid phase refractive index of the toothpaste can be adjusted according to actual requirements, and the toothpaste with different transparency degrees can be obtained.
(III) beneficial effects
Compared with the prior art, the invention provides a preparation method of precipitated silica for toothpaste thickener, which has the following beneficial effects:
the precipitated silica for the toothpaste thickener prepared by the invention has the product friction value RDA in the range of 100-150, the RDA on the toothpaste refers to the friction value of the toothpaste, the higher the value is, the higher the representative friction force is, the stronger the capability of removing dental plaque and tartar is, the water absorption is higher than 50ml/20g, and the specific surface area is 70-110m 2 In the range of/g.
By adding tetrasodium pyrophosphate as a regulator, the aggregation degree of the polymer matrix is regulated, and meanwhile, the friction value RDA of precipitated silica for the toothpaste thickener is improved.
The precipitated silica for the toothpaste thickener can improve the cleaning performance of the toothpaste and has excellent thickening effect.
Drawings
FIG. 1 is a graph comparing the effect of varying reaction vacuum on the refractive index of precipitated silica for toothpaste thickener;
FIG. 2 is a graph comparing the effect of different tetrasodium pyrophosphate additions on RDA rub values.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The following are specific examples:
example 1
A method for preparing precipitated silica for a toothpaste thickener comprising:
(1) Firstly, preparing a water glass solution, adding sodium silicate into deionized water, and stirring for 40min at a rotating speed of 200r/min to obtain a water glass solution with the concentration of 13 wt%;
preparing sulfuric acid solution, slowly adding sulfuric acid into deionized water, and stirring while adding until the solution is uniformly mixed to obtain sulfuric acid solution with the mass fraction of 40%;
(2) Adding sulfuric acid solution into a reaction kettle, regulating the temperature of the reaction kettle to 80 ℃, then under the condition of stirring, firstly adding tetrasodium pyrophosphate, then dropwise adding water glass solution, controlling the reaction pH to 8.0-9.0 after the water glass solution is dropwise added, reacting for 50min, then continuing adding sulfuric acid solution until the reaction pH is 4.0-5.0, then regulating the temperature to 85 ℃, and preserving heat;
(3) Pumping the reaction kettle to vacuum under the condition that the pH value is kept in the range of 4.5-5.0, then carrying out secondary feeding, dropwise adding water glass solution with the same amount as that in the step (2) into the reaction kettle, continuously adding sulfuric acid solution after the dropwise adding of the water glass solution is finished until the reaction pH value is controlled in the range of 4.0-4.2, stirring and aging for 30min, and then carrying out filter pressing, washing, pulping and spray drying to obtain silicon dioxide particles;
(4) The obtained silica particles were pulverized to an average particle size of 8 μm to obtain precipitated silica for a toothpaste thickener.
The modulus of the water glass solution is 3.3, and the transparency is more than 210mm.
The conductivity of deionized water was 15. Mu.s/cm.
The adding amount of tetrasodium pyrophosphate is 0.8% of the mass of the water glass solution.
The degree of vacuum of the vacuum was 0.02Pa.
The RDA rub value for the precipitated silica for the toothpaste thickener is between 100.
The pH of the precipitated silica for toothpaste thickener is between 5.5.
The purity of the silicon dioxide in the precipitated silicon dioxide for the toothpaste thickener is more than or equal to 96 percent.
The water absorption of the precipitated silica used for the toothpaste thickener is less than 50ml/20g.
The refractive index of the precipitated silica for the toothpaste thickener was 1.43N.
Example 2
A method for preparing precipitated silica for a toothpaste thickener comprising:
(1) Firstly, preparing a water glass solution, adding sodium silicate into deionized water, and stirring for 40min at a rotating speed of 220r/min to obtain a water glass solution with the concentration of 14 wt%;
preparing sulfuric acid solution, slowly adding sulfuric acid into deionized water, and stirring while adding until the solution is uniformly mixed to obtain sulfuric acid solution with the mass fraction of 42%;
(2) Adding sulfuric acid solution into a reaction kettle, regulating the temperature of the reaction kettle to 80 ℃, then under the condition of stirring, firstly adding tetrasodium pyrophosphate, then dropwise adding water glass solution, controlling the reaction pH to 8.0-9.0 after the water glass solution is dropwise added, reacting for 55min, then continuing adding sulfuric acid solution until the reaction pH is 4.0-5.0, then regulating the temperature to 88 ℃, and preserving heat;
(3) Pumping the reaction kettle to vacuum under the condition that the pH value is kept in the range of 4.5-5.0, then carrying out secondary feeding, dropwise adding water glass solution with the same amount as that in the step (2) into the reaction kettle, continuously adding sulfuric acid solution after the dropwise adding of the water glass solution is finished until the reaction pH value is controlled in the range of 4.0-4.2, stirring and aging for 30min, and then carrying out filter pressing, washing, pulping and spray drying to obtain silicon dioxide particles;
(4) The obtained silica particles were pulverized to an average particle size of 8.5 μm to obtain precipitated silica for a toothpaste thickener.
The modulus of the water glass solution is 3.4, and the transparency is more than 210mm.
The conductivity of deionized water was 15. Mu.s/cm.
The adding amount of tetrasodium pyrophosphate is 0.9% of the mass of the water glass solution.
The degree of vacuum of the evacuated is 0.03Pa.
The RDA rub value for the precipitated silica for the toothpaste thickener was at 110.
The pH of the precipitated silica for toothpaste thickener was 6.5.
The purity of the silicon dioxide in the precipitated silicon dioxide for the toothpaste thickener is more than or equal to 96 percent.
The water absorption of the precipitated silica used for the toothpaste thickener is less than 50ml/20g.
The precipitated silica used in the toothpaste thickener had a refractive index of 1.44N.
Example 3
A method for preparing precipitated silica for a toothpaste thickener comprising:
(1) Firstly, preparing a water glass solution, adding sodium silicate into deionized water, and stirring for 40min at a rotating speed of 250r/min to obtain a water glass solution with 13-18 wt%;
preparing sulfuric acid solution, slowly adding sulfuric acid into deionized water, and stirring while adding until the solution is uniformly mixed to obtain sulfuric acid solution with the mass fraction of 50%;
(2) Adding sulfuric acid solution into a reaction kettle, regulating the temperature of the reaction kettle to 80 ℃, then under the condition of stirring, firstly adding tetrasodium pyrophosphate, then dropwise adding water glass solution, controlling the reaction pH to 8.0-9.0 after the water glass solution is dropwise added, reacting for 60min, then continuing adding sulfuric acid solution until the reaction pH is 4.0-5.0, then regulating the temperature to 95 ℃, and preserving heat;
(3) Pumping the reaction kettle to vacuum under the condition that the pH value is kept in the range of 4.5-5.0, then carrying out secondary feeding, dropwise adding water glass solution with the same amount as that in the step (2) into the reaction kettle, continuously adding sulfuric acid solution after the dropwise adding of the water glass solution is finished until the reaction pH value is controlled in the range of 4.0-4.2, stirring and aging for 30min, and then carrying out filter pressing, washing, pulping and spray drying to obtain silicon dioxide particles;
(4) The obtained silica particles are crushed to an average particle size of 8-10 microns to obtain precipitated silica for toothpaste thickener.
The water glass solution has a modulus of 3.5 and a transparency of more than 210mm.
The conductivity of deionized water was 15. Mu.s/cm.
The adding amount of tetrasodium pyrophosphate is 1.0% of the mass of the water glass solution.
The degree of vacuum of the evacuated is 0.05Pa.
The RDA rub value for the precipitated silica for the toothpaste thickener was at 150.
The pH of the precipitated silica for toothpaste thickener was 8.5.
The purity of the silicon dioxide in the precipitated silicon dioxide for the toothpaste thickener is more than or equal to 96 percent.
The water absorption of the precipitated silica used for the toothpaste thickener is less than 50ml/20g.
The refractive index of the precipitated silica for the toothpaste thickener was 1.43N.
Example 4
A method for preparing precipitated silica for a toothpaste thickener comprising:
(1) Firstly, preparing a water glass solution, adding sodium silicate into deionized water, and stirring for 40min at a rotating speed of 230r/min to obtain a 15wt% water glass solution;
preparing sulfuric acid solution, slowly adding sulfuric acid into deionized water, and stirring while adding until the solution is uniformly mixed to obtain a sulfuric acid solution with the mass fraction of 45%;
(2) Adding sulfuric acid solution into a reaction kettle, regulating the temperature of the reaction kettle to 80 ℃, then under the condition of stirring, firstly adding tetrasodium pyrophosphate, then dropwise adding water glass solution, controlling the reaction pH to 8.0-9.0 after the water glass solution is dropwise added, reacting for 55min, then continuing adding sulfuric acid solution until the reaction pH is 4.0-5.0, then regulating the temperature to 89 ℃, and preserving heat;
(3) Pumping the reaction kettle to vacuum under the condition that the pH value is kept in the range of 4.5-5.0, then carrying out secondary feeding, dropwise adding water glass solution with the same amount as that in the step (2) into the reaction kettle, continuously adding sulfuric acid solution after the dropwise adding of the water glass solution is finished until the reaction pH value is controlled in the range of 4.0-4.2, stirring and aging for 30min, and then carrying out filter pressing, washing, pulping and spray drying to obtain silicon dioxide particles;
(4) The obtained silica particles were pulverized to an average particle size of 9 μm to obtain precipitated silica for a toothpaste thickener.
The modulus of the water glass solution is 3.4, and the transparency is more than 210mm.
The conductivity of deionized water was 15. Mu.s/cm.
The adding amount of tetrasodium pyrophosphate is 1.1% of the mass of the water glass solution.
The degree of vacuum of the evacuated is 0.04Pa.
The RDA rub value for the precipitated silica for the toothpaste thickener was at 130.
The pH of the precipitated silica for toothpaste thickener was 7.5.
The purity of the silicon dioxide in the precipitated silicon dioxide for the toothpaste thickener is more than or equal to 96 percent.
The water absorption of the precipitated silica used for the toothpaste thickener is less than 50ml/20g.
The refractive index of the precipitated silica used for the toothpaste thickener was 1.46N.
Example 5
A method for preparing precipitated silica for a toothpaste thickener comprising:
(1) Firstly, preparing a water glass solution, adding sodium silicate into deionized water, and stirring for 40min at a rotating speed of 250r/min to obtain a water glass solution with 13-18 wt%;
preparing sulfuric acid solution, slowly adding sulfuric acid into deionized water, and stirring while adding until the solution is uniformly mixed to obtain sulfuric acid solution with the mass fraction of 50%;
(2) Adding sulfuric acid solution into a reaction kettle, regulating the temperature of the reaction kettle to 80 ℃, then under the condition of stirring, firstly adding tetrasodium pyrophosphate, then dropwise adding water glass solution, controlling the reaction pH to 8.0-9.0 after the water glass solution is dropwise added, reacting for 55min, then continuing adding sulfuric acid solution until the reaction pH is 4.0-5.0, then regulating the temperature to 90 ℃, and preserving heat;
(3) Pumping the reaction kettle to vacuum under the condition that the pH value is kept in the range of 4.5-5.0, then carrying out secondary feeding, dropwise adding water glass solution with the same amount as that in the step (2) into the reaction kettle, continuously adding sulfuric acid solution after the dropwise adding of the water glass solution is finished until the reaction pH value is controlled in the range of 4.0-4.2, stirring and aging for 30min, and then carrying out filter pressing, washing, pulping and spray drying to obtain silicon dioxide particles;
(4) The obtained silica particles were pulverized to an average particle size of 9 μm to obtain precipitated silica for a toothpaste thickener.
The modulus of the water glass solution is 3.4, and the transparency is more than 210mm.
The conductivity of deionized water was 15. Mu.s/cm.
The adding amount of tetrasodium pyrophosphate is 1.2% of the mass of the water glass solution.
The degree of vacuum of the evacuated is 0.04Pa.
The RDA rub value for the precipitated silica for the toothpaste thickener was at 130.
The pH of the precipitated silica for toothpaste thickener is between 6.0.
The purity of the silicon dioxide in the precipitated silicon dioxide for the toothpaste thickener is more than or equal to 96 percent.
The water absorption of the precipitated silica used for the toothpaste thickener is less than 50ml/20g.
The precipitated silica used in the toothpaste thickener had a refractive index of 1.44N.
Example 6
A method for preparing precipitated silica for a toothpaste thickener comprising:
(1) Firstly, preparing a water glass solution, adding sodium silicate into deionized water, and stirring for 40min at a rotating speed of 200r/min to obtain a 17wt% water glass solution;
preparing sulfuric acid solution, slowly adding sulfuric acid into deionized water, and stirring while adding until the solution is uniformly mixed to obtain a sulfuric acid solution with the mass fraction of 48%;
(2) Adding sulfuric acid solution into a reaction kettle, regulating the temperature of the reaction kettle to 80 ℃, then under the condition of stirring, firstly adding tetrasodium pyrophosphate, then dropwise adding water glass solution, controlling the reaction pH to 8.0-9.0 after the water glass solution is dropwise added, reacting for 58min, then continuing adding sulfuric acid solution until the reaction pH is 4.0-5.0, then regulating the temperature to 92 ℃, and preserving heat;
(3) Pumping the reaction kettle to vacuum under the condition that the pH value is kept in the range of 4.5-5.0, then carrying out secondary feeding, dropwise adding water glass solution with the same amount as that in the step (2) into the reaction kettle, continuously adding sulfuric acid solution after the dropwise adding of the water glass solution is finished until the reaction pH value is controlled in the range of 4.0-4.2, stirring and aging for 30min, and then carrying out filter pressing, washing, pulping and spray drying to obtain silicon dioxide particles;
(4) The obtained silica particles were pulverized to an average particle size of 10 μm to obtain precipitated silica for a toothpaste thickener.
The water glass solution has a modulus of 3.5 and a transparency of more than 210mm.
The conductivity of deionized water was 15. Mu.s/cm.
The adding amount of tetrasodium pyrophosphate is 1.2% of the mass of the water glass solution.
The degree of vacuum of the evacuated is 0.03Pa.
The RDA rub value for the toothpaste thickener with precipitated silica was at 120.
The pH of the precipitated silica for toothpaste thickener was between 7.2.
The purity of the silicon dioxide in the precipitated silicon dioxide for the toothpaste thickener is more than or equal to 96 percent.
The water absorption of the precipitated silica used for the toothpaste thickener is less than 50ml/20g.
The refractive index of the precipitated silica used for the toothpaste thickener was 1.45N.
Comparative example 1: the difference from example 1 is that tetrasodium pyrophosphate will not be added;
comparative example 2: except that no secondary addition was performed as in example 1;
and (3) testing:
SiO determination of examples and comparative examples Using Tristar3000 type specific surface profiler, america microphone company 2 Specific surface area of powder:
TABLE 1
| Specific surface area/m 2 /g | |
| Example 1 | 92.5 |
| Example 2 | 90.2 |
| Example 3 | 91.8 |
| Example 4 | 90.5 |
| Example 5 | 91.7 |
| Example 6 | 92.1 |
As can be seen from Table 1, the precipitated silica for toothpaste thickener prepared according to the present invention has a relatively suitable specific surface area.
The internationally recognized nitrogen physical adsorption principle is adopted to measure the pore volume of the samples of the examples and the comparative examples, and the pore volume is compared;
TABLE 2
| Pore volume cm 3 /g | |
| Example 1 | 0.856 |
| Example 2 | 0.850 |
| Example 3 | 0.853 |
| Example 4 | 0.847 |
| Example 5 | 0.851 |
| Example 6 | 0.855 |
| Comparative example 1 | 0.715 |
| Comparative example 2 | 0.604 |
As can be seen from Table 2, the precipitated silica for toothpaste thickener prepared by the present invention has a higher pore volume, and can adsorb more toothpaste active substances by increasing the pore volume, thereby not only improving the thickening effect of toothpaste, but also improving the cleaning effect of toothpaste.
Refractive index measurements were performed on samples of examples and comparative examples:
taking 0.5g of samples of examples and comparative examples, adding the samples to 15g of sorbitol/water mixed solution, stirring uniformly, vacuumizing, maintaining vacuum for 30min, testing the refractive index of the dispersion liquid at the wavelength of 589nm, and drawing a transmittance-refractive index curve, wherein the transmittance at the maximum peak of the curve is the refractive index of silicon dioxide:
TABLE 3 Table 3
As can be seen from Table 3, the precipitated silica for toothpaste thickener prepared in accordance with the present invention has a relatively low refractive index.
Whiteness measurement with ColorTouchPC whiteness meter the whiteness of the samples of the examples and comparative examples was measured:
TABLE 4 Table 4
| Whiteness degree | |
| Example 1 | 98 |
| Example 2 | 98 |
| Example 3 | 98 |
| Example 4 | 98 |
| Example 5 | 98 |
| Example 6 | 98 |
| Comparative example 1 | 95 |
| Comparative example 2 | 96 |
As can be seen from Table 4, the precipitated silica for toothpaste thickener prepared in accordance with the present invention has a higher whiteness.
Based on example 1, the effect of varying reaction vacuum on the refractive index of precipitated silica for toothpaste thickener was compared as shown in FIG. 1.
Based on the sample of example 1, the effect of different amounts of tetrasodium pyrophosphate on RDA friction values was compared and counted as the mass ratio (%) of tetrasodium pyrophosphate to water glass, as shown in FIG. 2. Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (1)
1. A method for preparing precipitated silica for a toothpaste thickener, comprising:
(1) Firstly, preparing a water glass solution, adding sodium silicate into deionized water, and stirring for 40min at a rotating speed of 200-250r/min to obtain a water glass solution with 13-18 wt%;
preparing sulfuric acid solution, slowly adding sulfuric acid into deionized water, and stirring while adding until the solution is uniformly mixed to obtain sulfuric acid solution with the mass fraction of 40-50%;
(2) Adding sulfuric acid solution into a reaction kettle, regulating the temperature of the reaction kettle to 80 ℃, then under the condition of stirring, firstly adding tetrasodium pyrophosphate, then dropwise adding water glass solution, controlling the reaction pH to 8.0-9.0 after the water glass solution is dropwise added, reacting for 50-60min, then continuously adding sulfuric acid solution until the reaction pH is 4.0-5.0, then regulating the temperature to 85-95 ℃, and preserving heat;
(3) Pumping the reaction kettle to vacuum under the condition that the pH value is kept in the range of 4.5-5.0, then carrying out secondary feeding, dropwise adding water glass solution with the same amount as that in the step (2) into the reaction kettle, continuously adding sulfuric acid solution after the dropwise adding of the water glass solution is finished until the reaction pH value is controlled in the range of 4.0-4.2, stirring and aging for 30min, and then carrying out filter pressing, washing, pulping and spray drying to obtain silicon dioxide particles;
(4) Crushing the obtained silicon dioxide particles to an average particle size of 8-10 microns to obtain precipitated silicon dioxide for the toothpaste thickener; the modulus of the water glass solution is 3.3-3.5, and the transparency is more than 210mm; the conductivity of the deionized water is 15 mu s/cm; the adding amount of the tetrasodium pyrophosphate is 0.8-1.2% of the mass of the water glass solution; the vacuum degree of the vacuumizing is 0.02-0.05Pa; the RDA friction value of the precipitated silica for the toothpaste thickener is between 100 and 150; the pH of the precipitated silica for the toothpaste thickener is between 5.5 and 8.5; the purity of silicon dioxide in the precipitated silicon dioxide for the toothpaste thickener is more than or equal to 96 percent; the water absorption capacity of the precipitated silica used for the toothpaste thickener is less than 50ml/20g; the precipitated silica for the toothpaste thickener has a refractive index of 1.43-1.46N.
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| CN1878527A (en) * | 2003-10-28 | 2006-12-13 | J·M·休伯有限公司 | Precipitated silicas suitable for transparent dentifrices |
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