CN115385346A - Friction type silicon dioxide and preparation method and application thereof - Google Patents
Friction type silicon dioxide and preparation method and application thereof Download PDFInfo
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- CN115385346A CN115385346A CN202210996943.9A CN202210996943A CN115385346A CN 115385346 A CN115385346 A CN 115385346A CN 202210996943 A CN202210996943 A CN 202210996943A CN 115385346 A CN115385346 A CN 115385346A
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- silicon dioxide
- reaction
- sodium silicate
- sulfuric acid
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 198
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 89
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 152
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 148
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 77
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 76
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 76
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 54
- 239000007788 liquid Substances 0.000 claims abstract description 48
- 239000006185 dispersion Substances 0.000 claims abstract description 27
- 238000005406 washing Methods 0.000 claims abstract description 18
- 239000000606 toothpaste Substances 0.000 claims abstract description 17
- 229940034610 toothpaste Drugs 0.000 claims abstract description 17
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 16
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 16
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 16
- 230000032683 aging Effects 0.000 claims abstract description 11
- 238000003825 pressing Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 238000010438 heat treatment Methods 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 24
- 230000008569 process Effects 0.000 claims description 17
- 239000012295 chemical reaction liquid Substances 0.000 claims description 2
- 230000002431 foraging effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 16
- 229910052731 fluorine Inorganic materials 0.000 abstract description 16
- 239000011737 fluorine Substances 0.000 abstract description 16
- 238000004140 cleaning Methods 0.000 abstract description 6
- 239000003082 abrasive agent Substances 0.000 abstract description 3
- 230000002378 acidificating effect Effects 0.000 abstract description 3
- 230000007935 neutral effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 179
- 239000002585 base Substances 0.000 description 30
- 239000000047 product Substances 0.000 description 25
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 12
- 239000004033 plastic Substances 0.000 description 8
- 229920003023 plastic Polymers 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000000523 sample Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000011775 sodium fluoride Substances 0.000 description 6
- 235000013024 sodium fluoride Nutrition 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000011550 stock solution Substances 0.000 description 6
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 5
- -1 etc.) Substances 0.000 description 5
- 238000010998 test method Methods 0.000 description 5
- 239000007853 buffer solution Substances 0.000 description 4
- 238000004043 dyeing Methods 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 239000004743 Polypropylene Substances 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 3
- 210000003298 dental enamel Anatomy 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 230000002285 radioactive effect Effects 0.000 description 3
- ANOBYBYXJXCGBS-UHFFFAOYSA-L stannous fluoride Chemical compound F[Sn]F ANOBYBYXJXCGBS-UHFFFAOYSA-L 0.000 description 3
- 229960002799 stannous fluoride Drugs 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000551 dentifrice Substances 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000007863 gel particle Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 description 1
- 241000283690 Bos taurus Species 0.000 description 1
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 1
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 description 1
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- JUNWLZAGQLJVLR-UHFFFAOYSA-J calcium diphosphate Chemical compound [Ca+2].[Ca+2].[O-]P([O-])(=O)OP([O-])([O-])=O JUNWLZAGQLJVLR-UHFFFAOYSA-J 0.000 description 1
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 description 1
- 229940043256 calcium pyrophosphate Drugs 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 210000004268 dentin Anatomy 0.000 description 1
- 235000019821 dicalcium diphosphate Nutrition 0.000 description 1
- 235000019700 dicalcium phosphate Nutrition 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000011086 high cleaning Methods 0.000 description 1
- 239000003906 humectant Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 210000004283 incisor Anatomy 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 1
- 235000019799 monosodium phosphate Nutrition 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000000467 phytic acid Substances 0.000 description 1
- 229940068041 phytic acid Drugs 0.000 description 1
- 235000002949 phytic acid Nutrition 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 239000000176 sodium gluconate Substances 0.000 description 1
- 235000012207 sodium gluconate Nutrition 0.000 description 1
- 229940005574 sodium gluconate Drugs 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 1
- 239000002562 thickening agent Substances 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
- 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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/65—Chroma (C*)
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/80—Technologies aiming to reduce greenhouse gasses emissions common to all road transportation technologies
- Y02T10/86—Optimisation of rolling resistance, e.g. weight reduction
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Animal Behavior & Ethology (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses friction type silicon dioxide and a preparation method and application thereof. The preparation method of the friction type silicon dioxide comprises the following steps: 1) Uniformly mixing a sodium sulfate solution, a sodium hydroxide solution and a sodium silicate solution to obtain a reaction base solution; 2) Continuously adding a sodium silicate solution and a sulfuric acid solution into a reaction base solution, and carrying out a first acid-base parallel flow reaction under an acidic condition to obtain a silicon dioxide primary product dispersion liquid; 3) Continuously adding a sodium silicate solution and a sulfuric acid solution into the primary silicon dioxide product dispersion liquid, and carrying out secondary acid-base parallel flow reaction under a neutral condition to obtain a silicon dioxide dispersion liquid; 4) And (3) aging, filter pressing, washing, drying and crushing the silicon dioxide dispersion liquid to obtain the friction type silicon dioxide. The friction type silicon dioxide has the advantages of high apparent density, moderate friction performance, strong cleaning power, good fluorine compatibility, high transparency and the like, and is suitable for being used as an abrasive material for preparing transparent toothpaste.
Description
Technical Field
The invention relates to the technical field of toothpaste abrasives, in particular to friction type silicon dioxide and a preparation method and application thereof.
Background
Toothpaste is a widely used dentifrice product, and mainly comprises abrasive (such as silica, calcium hydrogen phosphate, calcium carbonate, etc.), humectant, thickener, surfactant, flavoring agent, etc. The silicon dioxide has the advantages of stable physical and chemical properties, acid and alkali resistance, high temperature resistance, good cleaning performance and the like, and is widely applied to toothpaste in recent years.
The high-friction silica needs to keep the transparency more than 70 percent (the refractive index is about 1.435-1.460) to meet the requirement of the transparent toothpaste on the transparency of the grinding materials, but the silica meeting the transparency requirement prepared by the prior art generally has the apparent density lower than 0.60g/mL, and the lower apparent density of the silica can bring certain adverse effects to the preparation, transportation and application processes of the silica (for example, the lower apparent density of the silica can cause the low bag receiving rate of a packaging procedure, the bag receiving process is easy to generate bag expansion and bag explosion, the low apparent density of the silica can easily cause dust pollution to air in the using process, and the absorption of human bodies can bring certain influence to the health of the human bodies). The greater the apparent density of the high friction silica, the higher the RDA (radioactive enamel abrasion) value, and greater than 250 RDA will cause damage to the tooth (the american dental association ADA specifies an upper limit for RDA of 250), and the greater the apparent density of the high friction silica, the better.
Therefore, it is very important to develop a silica having advantages of high apparent density, moderate friction performance, strong cleaning power, good fluorine compatibility, high transparency, etc.
Disclosure of Invention
The invention aims to provide friction type silicon dioxide and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
a method for preparing friction type silicon dioxide comprises the following steps:
1) Uniformly mixing a sodium sulfate solution, a sodium hydroxide solution and a sodium silicate solution, heating to 50-65 ℃, and adding a sulfuric acid solution until the pH value of the system is 2.0-5.0 to obtain a reaction base solution;
2) Continuously adding a sodium silicate solution and a sulfuric acid solution into a reaction base solution to carry out a first acid-base parallel flow reaction, and keeping the pH value of the reaction solution at 2.0-5.0 and the reaction temperature at 50-65 ℃ in the reaction process to obtain a silicon dioxide primary product dispersion solution;
3) Heating the primary product dispersion liquid of the silicon dioxide to 65-70 ℃, adjusting the pH value to 6.5-7.5, continuously adding a sodium silicate solution and a sulfuric acid solution to perform a second acid-base concurrent flow reaction, and keeping the pH value of the reaction liquid to 6.5-7.5 and the reaction temperature to 65-70 ℃ in the reaction process to obtain the silicon dioxide dispersion liquid;
4) Adding 65-70 ℃ water into the silicon dioxide dispersion liquid for aging, keeping the temperature of the silicon dioxide dispersion liquid at 65-70 ℃ in the aging process, adjusting the pH value of the silicon dioxide dispersion liquid to 3.0-4.0, performing filter pressing, washing with water at the temperature of more than or equal to 40 ℃ until the conductivity of washing water is less than or equal to 1000 mus/cm, and drying and crushing to obtain the friction type silicon dioxide.
Preferably, the volume ratio of the sodium sulfate solution, the sodium hydroxide solution and the sodium silicate solution in the step 1) is 20-30.
Preferably, the mass fraction of the sodium sulfate solution in the step 1) is 4.0-6.0%.
Preferably, the mass fraction of the sodium hydroxide solution in the step 1) is 0.5-1.0%.
Preferably, the mass fraction of the sodium silicate solution in the step 1) is 18-23%.
Preferably, the mass fraction of the sulfuric acid solution in the step 1) is 28.5-32%.
Preferably, the volume ratio of the sodium silicate solution, the sulfuric acid solution and the reaction base solution in the step 2) is 0.49-1.30.
Preferably, the mass fraction of the sodium silicate solution in the step 2) is 18-23%.
Preferably, the mass fraction of the sulfuric acid solution in the step 2) is 28.5-32%.
Preferably, the feeding speed ratio of the sodium silicate solution to the sulfuric acid solution in the step 2) is 2-7.5.
Preferably, the volume ratio of the sodium silicate solution, the sulfuric acid solution and the silica primary product dispersion liquid in the step 3) is 0.09-0.34.
Preferably, the mass fraction of the sodium silicate solution in the step 3) is 18-23%.
Preferably, the mass fraction of the sulfuric acid solution in the step 3) is 28.5-32%.
Preferably, the feeding speed ratio of the sodium silicate solution to the sulfuric acid solution in the step 3) is 1.6-10.
Preferably, sodium silicate solution with the mass fraction of 18-23% is adopted in the step 3) to adjust the pH value of the silicon dioxide primary product dispersion liquid to 6.5-7.5.
Preferably, the volume ratio of the water at 65 ℃ to 70 ℃ and the silica dispersion liquid in the step 4) is 0.18 to 0.40.
Preferably, the aging time in the step 4) is 20 min-40 min.
Preferably, the pH value of the silicon dioxide dispersion liquid is adjusted to 3.0-4.0 by using 28.5-32% of sulfuric acid solution in the step 4).
A friction type silica produced by the above method.
A toothpaste which comprises the above abrasive silica.
The invention has the beneficial effects that: the friction type silicon dioxide has the advantages of high apparent density, moderate friction performance, strong cleaning power, good fluorine compatibility, high transparency and the like, and is suitable for being used as an abrasive material for preparing transparent toothpaste.
Specifically, the method comprises the following steps:
1) The mixed solution of sodium sulfate and sodium hydroxide is used as a reaction base solution, a step-by-step heating two-stage acid-base parallel flow reaction mode is adopted, the first stage is an acid-base parallel flow reaction under an acidic condition, the second stage is an acid-base parallel flow reaction under a neutral condition, sodium silicate solution and sulfuric acid solution are added into the reaction base solution to react, sodium hydroxide and sulfuric acid react to generate sodium sulfate, the content of sodium sulfate in a reaction system is higher and higher before sodium silicate and sulfuric acid react, the density of silicon dioxide can be improved, the transparency and the fluorine stability of the silicon dioxide can be controlled by adopting a step-by-step heating and low-temperature reaction mode (low reaction rate at low temperature), and the finally obtained silicon dioxide has high apparent density, high fluorine stability and high transparency, and has unique sand feeling when being applied to a toothpaste gravel formula and has high cleaning capability;
2) According to the invention, the product is washed by water with the temperature of more than or equal to 40 ℃ in the filter pressing washing link, so that the problem of product transparency reduction caused by large temperature difference can be avoided;
3) According to the invention, acid-base parallel flow reaction is firstly carried out under an acidic condition, more hydrogen ions are dissociated from sulfuric acid in a reaction system than alkaline ions are dissociated from water glass and sodium hydroxide, so that gel particles can be promoted to be generated in the reaction process, and the gel particles have special gravel feeling after being dried;
4) The invention adopts two-section acid-base parallel flow reaction, which can improve the dispersibility and uniformity of the obtained silicon dioxide;
5) The fluorine compatibility of the friction type silicon dioxide in a stannous fluoride system can reach more than 90 percent, and the fluorine compatibility can still reach 80 percent after 72 hours in the stannous fluoride system;
6) The friction type silicon dioxide has the RDA value (radioactive enamel abrasion value) of 180-200, the PCR value (film cleaning rate) of more than or equal to 90, the apparent density of more than or equal to 0.6g/mL, and the transparency of more than or equal to 75% (the refractive index is 1.435-1.460).
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
Example 1:
a friction type silica is prepared by the following steps:
1) Is to be 10m 3 Sodium sulfate solution with mass fraction of 5.0% and 5m 3 Adding 1.0 wt% sodium hydroxide solution into reactor 1#, and adding 0.5m 3 Starting steam to heat sodium silicate solution with mass fraction of 18%, heating the solution in the reaction tank 1# to 65 ℃, starting a stirrer, and then heating to 2.0m 3 Feed rate of/hAdding 28.5 mass percent sulfuric acid solution until the pH value of the system is 3.5, and stopping adding acid to obtain reaction base solution;
2) Continuously adding 18 mass percent of sodium silicate solution and 28.5 mass percent of sulfuric acid solution into a reaction tank 1# for carrying out a first acid-base parallel flow reaction, wherein the adding amount of the sodium silicate solution is 10m 3 The feed rate was 10m 3 H, feed rate of sulfuric acid solution was 2.5m 3 Keeping the pH value of the reaction solution at 3.5 and the reaction temperature at 65 ℃ in the reaction process, and immediately stopping adding the sulfuric acid solution when the sodium silicate solution is completely added to obtain a silicon dioxide primary product dispersion liquid;
3) Communicating a reaction tank 1# with a reaction tank 2# to ensure that the primary silicon dioxide product dispersion liquid flows back and is balanced in the reaction tank 1# and the reaction tank 2# until the material liquid heights in the two reaction tanks are consistent, then starting steam heating to ensure that the primary silicon dioxide product dispersion liquid in the two reaction tanks is heated to 65 ℃, starting a stirrer, adding a sodium silicate solution with the mass fraction of 18 percent to adjust the pH value of a system to 7.0, continuously adding a sodium silicate solution with the mass fraction of 18 percent and a sulfuric acid solution with the mass fraction of 28.5 percent into the two reaction tanks to perform a second acid-base co-current flow reaction, wherein the adding amount of the sodium silicate solution is 10m 3 The feed rate was 10m 3 H, the feed rate of the sulfuric acid solution was 2.5m 3 Keeping the pH value of the reaction solution at 7.0 and the reaction temperature at 65 ℃ in the reaction process, and stopping adding the sulfuric acid solution immediately after the sodium silicate solution is added to obtain a silicon dioxide dispersion solution;
4) Will be 10m 3 Adding process water with the temperature of 65 ℃ into two reaction tanks, stirring and aging for 30min at the temperature of 65 ℃, adding 28.5 mass percent sulfuric acid solution to adjust the pH value of the system to 4.0, performing filter pressing, washing with the process water with the temperature of 45 ℃ until the conductivity of the washing water is less than or equal to 1000 mus/cm, and drying and crushing to obtain the friction type silicon dioxide.
The abrasive silica of this example was tested to have an RDA of 188.54, a pcr of 196.55, a whiteness of 98.87%, an apparent density of 0.64g/mL, a clarity of 90.9% (refractive index of 1.4390), and a fluorine compatibility of 95.5% for a toothpaste having a particular gritty feel.
Note:
RDA values (radioactive enamel abrasion values): the Hefferren grinding test recommended by ADA and ISO was used to determine the abrasiveness of dentifrices in dentin (samples were sent to the university of Indiana, USA for testing).
PCR value (film cleaning rate): embedding a tooth standard sample (bovine incisor) on methyl methacrylate resin, polishing the surface of the tooth standard sample by using a grinding polisher under constant water flow, sequentially treating the tooth standard sample by using hydrochloric acid, sodium carbonate and phytic acid, putting the tooth standard sample in a dyeing device, alternately immersing the tooth standard sample in dyeing liquid and dry air at the rotating speed of 1r/min, wherein the dyeing period is 7 days, changing the dyeing liquid every two days, evaluating the color change of the standard sample by using a color difference instrument, wherein the L value is in the range of 30-45, is a qualified standard sample, and evaluating the L value by using a calcium pyrophosphate suspension and a tested grinding powder brush 800 on a tooth brushing machine respectively, and calculating the PCR value.
Apparent density: the test was carried out with reference to "silica for QB/T2346-2007 toothpaste".
Transparency: the test was performed with reference to "silica for QB/T2346-2007 toothpaste".
Fluorine compatibility:
reagent: sodium fluoride, disodium ethylenediaminetetraacetate, trimethylaminomethane, tris (hydroxymethyl) aminomethane, sodium hydroxide, sodium dihydrogen phosphate (1 part of crystal water) and disodium hydrogen phosphate (anhydrous or 2 parts of crystal water).
The instrument comprises the following steps: a reference electrode, a PH/mV meter, a fluoride ion selective electrode, a glass electrode, a high-speed centrifuge, a test tube rotator, a plastic wide-mouth bottle, a sealed plastic bottle, a plastic centrifugal test tube and a magnetic stirrer.
Measurement procedure: adding 7g of friction type silicon dioxide into a plastic beaker, slowly adding 30g of NaF 1624ppm stock solution, sealing (prohibiting the liquid from volatilizing), placing on a rotating frame, rotating and heating at 60 ℃ for 1h, centrifuging at 15000rpm for 15min, taking 2g of supernatant, adding into a plastic bottle, adding 9 times of EDTA/THAM buffer solution, placing on a stirrer, inserting a fluorine ion selection electrode, reading after 1min/72h, and calculating fluorine compatibility according to the following formula:
fluorine compatibility (%) = (F in sample solution) - concentration/F in standard solution - Concentration) × 100%.
Preparation of NaF 1624ppm stock solution: 0.6697g of stannous fluoride and 0.9618g of sodium gluconate were dissolved in 98.37g of water and stirred until clear.
Preparation of EDTA/THAM buffer: 74.4g of EDTA-2Na +24.2g of THAM +800mL of H 2 O, adjusting the pH to 8.0 with a 5N NaOH solution (50 g of NaOH dissolved in water, transferred into a volumetric flask, diluted to 250mL and shaken up), transferring into a 1000mL volumetric flask, diluting to the mark, and transferring into a 1000mL white reagent bottle.
Preparation of standard sample solution:
a) High standard solution (162.4 ppm): adding 90g of EDTA/THAM buffer solution into 10g of NaF 1624ppm stock solution, and filling into a polypropylene plastic bottle;
b) Low standard (16.24 ppm): adding 1g of NaF 1624ppm stock solution into 9g of water, adding 90g of EDTA/THAM buffer solution, and filling into a polypropylene plastic bottle;
c) 90% high-standard liquid: 9g of NaF 1624ppm stock solution was added to 1g of water, and 90g of EDTA/THAM buffer solution was added to the stock solution, and the mixture was filled in a polypropylene plastic bottle.
Example 2:
a friction type silicon dioxide is prepared by the following steps:
1) Will be 15m 3 Sodium sulfate solution with mass fraction of 6.0% and 5m 3 Adding 1.0 wt% sodium hydroxide solution into reaction tank 1#, and adding 0.5m 3 Starting steam heating to heat the sodium silicate solution with the mass fraction of 23% in the reaction tank 1#, heating the solution to 65 ℃, starting a stirrer, and then heating the solution at the temperature of 2.0m 3 Adding 32 mass percent sulfuric acid solution at a feeding speed of/h until the pH value of the system is 5.0, and stopping adding acid to obtain reaction base solution;
2) Continuously adding a sodium silicate solution with the mass fraction of 23% and a sulfuric acid solution with the mass fraction of 32% into a reaction tank 1# for carrying out a first acid-base concurrent flow reaction, wherein the adding amount of the sodium silicate solution is 15m 3 The feed rate was 15m 3 H, feed rate of sulfuric acid solution was 5.0m 3 Keeping the pH value of the reaction solution at 5.0 and the reaction temperature at 65 ℃ in the reaction process, and stopping adding the sulfuric acid solution immediately after the sodium silicate solution is added to obtain a silicon dioxide primary product dispersion liquid;
3) Communicating a reaction tank 1# with a reaction tank 2# to enable the silica primary product dispersion liquid to flow back and balance in the reaction tank 1# and the reaction tank 2# until the material liquid height in the two reaction tanks is consistent, starting steam heating to enable the silica primary product dispersion liquid in the two reaction tanks to be heated to 70 ℃, starting a stirrer, adding 23% by mass of sodium silicate solution to adjust the pH value of the system to 7.5, continuously adding 23% by mass of sodium silicate solution and 32% by mass of sulfuric acid solution into the two reaction tanks to perform a second acid-base parallel flow reaction, wherein the adding amount of the sodium silicate solution is 10m 3 The feed rate was 15m 3 H, the feed rate of the sulfuric acid solution was 5.0m 3 Keeping the pH value of the reaction solution at 7.5 and the reaction temperature at 70 ℃ in the reaction process, and stopping adding the sulfuric acid solution immediately after the sodium silicate solution is added to obtain a silicon dioxide dispersion solution;
4) Will be 10m 3 Adding process water with the temperature of 70 ℃ into two reaction tanks, stirring and aging for 30min at the temperature of 70 ℃, adding 32 mass percent sulfuric acid solution to adjust the pH value of the system to 3.0, performing filter pressing, washing with the process water with the temperature of 50 ℃ until the conductivity of the washing water is less than or equal to 1000 mus/cm, and drying and crushing to obtain the friction type silicon dioxide.
Upon examination (test method same as example 1), the abraded silica of this example had an RDA value of 197.73, a pcr value of 104.23, a whiteness of 97.87%, an apparent density of 0.72g/mL, a transparency of 88.9% (refractive index of 1.4390), a fluorine compatibility of 97.3%, and a special grit feel for use in toothpaste.
Example 3:
a friction type silica is prepared by the following steps:
1) Will be 12m 3 Sodium sulfate solution with mass fraction of 4.0% and 1m 3 Adding 0.5 wt% sodium hydroxide solution into reactor 1#,then add 0.5m 3 Starting steam to heat sodium silicate solution with the mass fraction of 20%, heating the solution in the reaction tank 1# to 60 ℃, starting a stirrer, and then heating the solution at 2.0m 3 Adding 30 mass percent sulfuric acid solution at a feeding speed of/h until the pH value of the system is 4.0, and stopping adding acid to obtain reaction base solution;
2) Continuously adding a sodium silicate solution with the mass fraction of 20% and a sulfuric acid solution with the mass fraction of 30% into a reaction tank 1# for carrying out a first acid-base parallel flow reaction, wherein the adding amount of the sodium silicate solution is 12m 3 The feed rate was 12m 3 H, the feed rate of the sulfuric acid solution was 3.0m 3 Keeping the pH value of the reaction solution at 4.0 and the reaction temperature at 60 ℃ in the reaction process, and stopping adding the sulfuric acid solution immediately after the sodium silicate solution is added to obtain a silicon dioxide primary product dispersion liquid;
3) Communicating a reaction tank 1# with a reaction tank 2# to ensure that the primary silicon dioxide product dispersion liquid flows back and is balanced in the reaction tank 1# and the reaction tank 2# until the material liquid heights in the two reaction tanks are consistent, then starting steam heating to ensure that the primary silicon dioxide product dispersion liquid in the two reaction tanks is heated to 65 ℃, starting a stirrer, adding a sodium silicate solution with the mass fraction of 20 percent to adjust the pH value of the system to 6.5, continuously adding a sodium silicate solution with the mass fraction of 20 percent and a sulfuric acid solution with the mass fraction of 30 percent into the two reaction tanks to perform a second acid-base co-current flow reaction, wherein the adding amount of the sodium silicate solution is 12m 3 The feed rate was 12m 3 H, feed rate of sulfuric acid solution was 3.0m 3 Keeping the pH value of the reaction solution at 6.5 and the reaction temperature at 65 ℃ in the reaction process, and immediately stopping adding the sulfuric acid solution when the sodium silicate solution is completely added to obtain a silicon dioxide dispersion solution;
4) Will be 10m 3 Adding process water with the temperature of 65 ℃ into two reaction tanks, stirring and aging for 30min at the temperature of 65 ℃, adding 30 mass percent sulfuric acid solution to adjust the pH value of the system to 3.0, performing filter pressing, washing with process water with the temperature of 45 ℃ until the conductivity of washing water is less than or equal to 1000 mus/cm, and drying and crushing to obtain the friction-type silicon dioxide.
The abraded silica of this example was tested (same test method as example 1) to have an RDA of 192.73, a pcr of 99.23, a whiteness of 99.87%, an apparent density of 0.68g/mL, a transparency of 91.4% (refractive index of 1.4390), a fluorine compatibility of 98.8%, and a special gritty feel for toothpaste.
Comparative example 1:
a silica, the preparation method of which comprises the following steps:
1) Will be 10m 3 Adding 5.0 wt% sodium sulfate solution into reactor 1#, heating with steam to raise the temperature of the solution in reactor 1#, starting stirrer, and adding 2.0m 3 Adding 32 mass percent sulfuric acid solution at a feeding speed of/h until the pH value of the system is 3.5, and stopping adding acid to obtain reaction base solution;
2) Continuously adding a sodium silicate solution with the mass fraction of 23% and a sulfuric acid solution with the mass fraction of 32% into a reaction tank 1# for carrying out a first acid-base concurrent flow reaction, wherein the adding amount of the sodium silicate solution is 10m 3 The feed rate was 10m 3 H, the feed rate of the sulfuric acid solution was 2.5m 3 Keeping the pH value of the reaction solution at 3.5 and the reaction temperature at 65 ℃ in the reaction process, and immediately stopping adding the sulfuric acid solution when the sodium silicate solution is completely added to obtain a silicon dioxide primary product dispersion liquid;
3) Communicating a reaction tank 1# with a reaction tank 2# to ensure that the primary silicon dioxide product dispersion liquid flows back and is balanced in the reaction tank 1# and the reaction tank 2# until the heights of the material liquids in the two reaction tanks are consistent, then starting steam heating to ensure that the primary silicon dioxide product dispersion liquid in the two reaction tanks is heated to 65 ℃, starting a stirrer, adding a sodium silicate solution with the mass fraction of 23 percent to adjust the pH value of the system to 7.0, continuously adding a sodium silicate solution with the mass fraction of 23 percent and a sulfuric acid solution with the mass fraction of 32 percent into the two reaction tanks to perform a second acid-base co-current flow reaction, wherein the addition amount of the sodium silicate solution is 10m 3 The feed rate was 10m 3 H, the feed rate of the sulfuric acid solution was 2.5m 3 Keeping the pH value of the reaction solution at 7.0 and the reaction temperature at 65 ℃ in the reaction process, and stopping adding the sulfuric acid solution immediately after the sodium silicate solution is added to obtain a silicon dioxide dispersion solution;
4) Will be 10m 3 Adding process water with the temperature of 65 ℃ into two reaction tanks, stirring and aging for 30min at the temperature of 65 ℃, adding 32 mass percent sulfuric acid solution to adjust the pH value of the system to 4.0, performing filter pressing, washing with process water with the temperature of 45 ℃ until the conductivity of washing water is less than or equal to 1000 mus/cm, and drying and crushing to obtain the silicon dioxide.
When tested (same test method as example 1), the silica of this comparative example had an RDA value of 178.66, a pcr value of 96.25, a whiteness of 98.42%, an apparent density of 0.53g/mL, a transparency of 76.7% (refractive index of 1.4395), a fluorine compatibility of 92.1%, and a special gritty feel for toothpaste.
Comparative example 2:
a silica, the preparation method of which comprises the following steps:
1) Is to be 10m 3 Sodium sulfate solution with mass fraction of 5.0% and 5m 3 Adding 1.0 wt% sodium hydroxide solution into the reaction tank 1#, and adding 5m 3 Starting steam heating to heat the sodium silicate solution with the mass fraction of 23% in the reaction tank 1#, heating the solution to 80 ℃, starting a stirrer, and then heating the solution at the temperature of 2.0m 3 Adding 32 mass percent sulfuric acid solution at a feeding speed of/h until the pH value of the system is 3.5, and stopping adding acid to obtain reaction base solution;
2) Continuously adding a sodium silicate solution with the mass fraction of 23% and a sulfuric acid solution with the mass fraction of 32% into a reaction tank 1# for carrying out a first acid-base concurrent flow reaction, wherein the adding amount of the sodium silicate solution is 10m 3 The feed rate was 10m 3 H, the feed rate of the sulfuric acid solution was 2.5m 3 Keeping the pH value of the reaction solution at 3.5 and the reaction temperature at 80 ℃ in the reaction process, and stopping adding the sulfuric acid solution immediately after the sodium silicate solution is added to obtain a silicon dioxide primary product dispersion liquid;
3) Communicating a reaction tank 1# with a reaction tank 2# to ensure that the primary silicon dioxide product dispersion liquid flows back and is balanced in the reaction tank 1# and the reaction tank 2# until the material liquid height in the two reaction tanks is consistent, starting steam heating to ensure that the primary silicon dioxide product dispersion liquid in the two reaction tanks is heated to 80 ℃, starting a stirrer, and adding mass componentsAdjusting the pH value of a 23% sodium silicate solution adjusting system to 7.0, continuously adding the 23% sodium silicate solution and 32% sulfuric acid solution into two reaction tanks for a second acid-base parallel flow reaction, wherein the adding amount of the sodium silicate solution is 10m 3 The feed rate was 10m 3 H, the feed rate of the sulfuric acid solution was 2.5m 3 Keeping the pH value of the reaction solution at 7.0 and the reaction temperature at 80 ℃ in the reaction process, and immediately stopping adding the sulfuric acid solution when the sodium silicate solution is completely added to obtain a silicon dioxide dispersion solution;
4) Will be 10m 3 Adding process water with the temperature of 80 ℃ into two reaction tanks, stirring and aging for 30min at the temperature of 75 ℃, adding 32 mass percent sulfuric acid solution to adjust the pH value of the system to 4.0, performing filter pressing, washing with process water at normal temperature until the conductivity of the washing water is less than or equal to 1000 mus/cm, and drying and crushing to obtain the silicon dioxide.
Upon testing (test method same as example 1), the silica of this comparative example had an RDA value of 231.44, a pcr value of 101.80, a whiteness of 98.56%, an apparent density of 0.62g/mL, a transparency of 67.4% (refractive index of 1.4430), a fluorine compatibility of 96.5%, and a special gritty feel for toothpaste.
Comparative example 3:
a silica, the preparation method of which comprises the following steps:
1) Will be 10m 3 Sodium sulfate solution with mass fraction of 3.0% and 1m 3 Adding 0.5% sodium hydroxide solution into the reaction tank 1#, and adding 0.5m 3 Starting steam to heat sodium silicate solution with mass fraction of 18%, heating the solution in the reaction tank 1# to 65 ℃, starting a stirrer, and then heating to 2.0m 3 Adding 28.5 mass percent sulfuric acid solution at a feeding speed of per hour until the pH value of the system is 3.5, and stopping adding acid to obtain reaction base solution;
2) Continuously adding 18 mass percent of sodium silicate solution and 28.5 mass percent of sulfuric acid solution into a reaction tank 1# for carrying out a first acid-base parallel flow reaction, wherein the adding amount of the sodium silicate solution is 10m 3 The feed rate was 10m 3 Feed rate of sulfuric acid solution of 2.5m 3 Keeping the pH value of the reaction solution at 3.5 and the reaction temperature at 65 ℃ in the reaction process, and stopping adding the sulfuric acid solution immediately after the sodium silicate solution is added to obtain a silicon dioxide primary product dispersion liquid;
3) Communicating a reaction tank 1# with a reaction tank 2# to ensure that the primary silicon dioxide product dispersion liquid flows back and is balanced in the reaction tank 1# and the reaction tank 2# until the heights of the material liquids in the two reaction tanks are consistent, then starting steam heating to ensure that the primary silicon dioxide product dispersion liquid in the two reaction tanks is heated to 65 ℃, starting a stirrer, then adding a sodium silicate solution with the mass fraction of 18 percent to adjust the pH value of the system to 7.5, and then adding 10m sodium silicate solution to adjust the pH value of the system to 7.5 3 Sodium silicate solution with the mass fraction of 18% and sulfuric acid solution with the mass fraction of 28.5% are continuously added into two reaction tanks for secondary acid-base parallel flow reaction, and the adding amount of the sodium silicate solution is 10m 3 The feed rate was 10m 3 H, feed rate of sulfuric acid solution was 2.5m 3 Keeping the pH value of the reaction solution at 7.0 and the reaction temperature at 65 ℃ in the reaction process, and stopping adding the sulfuric acid solution immediately after the sodium silicate solution is added to obtain a silicon dioxide dispersion solution;
4) Will be 10m 3 Adding process water with the temperature of 65 ℃ into two reaction tanks, stirring and aging for 30min at the temperature of 65 ℃, adding 28.5 mass percent sulfuric acid solution to adjust the pH value of the system to 4.0, performing filter pressing, washing with the process water with the temperature of 45 ℃ until the conductivity of the washing water is less than or equal to 1000 mus/cm, and drying and crushing to obtain the silicon dioxide.
When tested (same test method as example 1), the silica of this comparative example had an RDA value of 168.58, a pcr value of 108.28, a whiteness of 98.62%, an apparent density of 0.41g/mL, a transparency of 90.3% (refractive index of 1.4390), a fluorine compatibility of 96.4%, and no noticeable grittiness when used in a toothpaste.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A method for preparing abrasive silica, comprising the steps of:
1) Uniformly mixing a sodium sulfate solution, a sodium hydroxide solution and a sodium silicate solution, heating to 50-65 ℃, and adding a sulfuric acid solution until the pH value of the system is 2.0-5.0 to obtain a reaction base solution;
2) Continuously adding a sodium silicate solution and a sulfuric acid solution into a reaction base solution to carry out a first acid-base parallel flow reaction, wherein the pH value of the reaction solution is kept between 2.0 and 5.0 and the reaction temperature is kept between 50 and 65 ℃ in the reaction process, so as to obtain a silicon dioxide primary product dispersion solution;
3) Heating the dispersion liquid of the primary product of the silicon dioxide to 65-70 ℃, adjusting the pH value to 6.5-7.5, continuously adding a sodium silicate solution and a sulfuric acid solution to perform a second acid-base parallel flow reaction, and keeping the pH value of the reaction liquid to 6.5-7.5 and the reaction temperature to 65-70 ℃ in the reaction process to obtain the silicon dioxide dispersion liquid;
4) Adding 65-70 ℃ water into the silicon dioxide dispersion liquid for aging, keeping the temperature of the silicon dioxide dispersion liquid at 65-70 ℃ in the aging process, adjusting the pH value of the silicon dioxide dispersion liquid to 3.0-4.0, performing filter pressing, washing with water at the temperature of more than or equal to 40 ℃ until the conductivity of washing water is less than or equal to 1000 mus/cm, and drying and crushing to obtain the friction type silicon dioxide.
2. A process for preparing a abraded silica as defined in claim 1 wherein: step 1), the volume ratio of the sodium sulfate solution to the sodium hydroxide solution to the sodium silicate solution is 20-30; the mass fraction of the sodium sulfate solution in the step 1) is 4.0-6.0%; step 1), the mass fraction of the sodium hydroxide solution is 0.5-1.0%; the mass fraction of the sodium silicate solution in the step 1) is 18-23%.
3. A process for preparing a abraded silica as defined in claim 1 wherein: step 2), the volume ratio of the sodium silicate solution to the sulfuric acid solution to the reaction base solution is 0.49-1.30; step 2), the mass fraction of the sodium silicate solution is 18-23%; the mass fraction of the sulfuric acid solution in the step 2) is 28.5-32%.
4. A process for preparing a abraded silica as defined in claim 3 wherein: and 2) the feeding speed ratio of the sodium silicate solution to the sulfuric acid solution is 2-7.5.
5. A process for preparing a abraded silica as defined in claim 1 wherein: step 3), the volume ratio of the sodium silicate solution to the sulfuric acid solution to the primary product dispersion liquid of silicon dioxide is 0.09-0.34; the mass fraction of the sodium silicate solution in the step 3) is 18-23%; the mass fraction of the sulfuric acid solution in the step 3) is 28.5-32%.
6. The process for preparing a abraded silica as claimed in claim 5, wherein: and 3), the feeding speed ratio of the sodium silicate solution to the sulfuric acid solution is 1.6-10.
7. The process for producing a friction-type silica according to any one of claims 1 to 6, wherein: the volume ratio of the water at 65-70 ℃ to the silicon dioxide dispersion liquid in the step 4) is 0.18-0.40.
8. The process for producing a friction-type silica according to any one of claims 1 to 6, wherein: and 4) the aging time is 20-40 min.
9. A abraded silica produced by the method of any one of claims 1 to 8.
10. A toothpaste comprising the abrasive silica of claim 9.
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Application publication date: 20221125 Assignee: GUANGZHOU FEIXUE MATERIAL TECHNOLOGY Co.,Ltd. Assignor: Jinsanjiang (Zhaoqing) silicon material Co.,Ltd. Contract record no.: X2023980039858 Denomination of invention: A friction type silica and its preparation method and application Granted publication date: 20230704 License type: Common License Record date: 20230818 |