CN117466305B - Calcium silicate with friction cleaning performance and preparation method thereof - Google Patents
Calcium silicate with friction cleaning performance and preparation method thereof Download PDFInfo
- Publication number
- CN117466305B CN117466305B CN202311669947.7A CN202311669947A CN117466305B CN 117466305 B CN117466305 B CN 117466305B CN 202311669947 A CN202311669947 A CN 202311669947A CN 117466305 B CN117466305 B CN 117466305B
- Authority
- CN
- China
- Prior art keywords
- sodium
- solution
- calcium
- calcium silicate
- silicate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000378 calcium silicate Substances 0.000 title claims abstract description 134
- 229910052918 calcium silicate Inorganic materials 0.000 title claims abstract description 134
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 title claims abstract description 134
- 238000004140 cleaning Methods 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 196
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 114
- 238000006243 chemical reaction Methods 0.000 claims abstract description 75
- 239000000463 material Substances 0.000 claims abstract description 74
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 73
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 59
- 239000000843 powder Substances 0.000 claims abstract description 56
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 50
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000006004 Quartz sand Substances 0.000 claims abstract description 32
- 238000003756 stirring Methods 0.000 claims abstract description 31
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 26
- 239000012266 salt solution Substances 0.000 claims abstract description 26
- 229940034610 toothpaste Drugs 0.000 claims abstract description 26
- 239000000606 toothpaste Substances 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 24
- 159000000007 calcium salts Chemical class 0.000 claims abstract description 16
- 239000007787 solid Substances 0.000 claims abstract description 16
- 159000000000 sodium salts Chemical class 0.000 claims abstract description 15
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 14
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 14
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 72
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 46
- 239000011780 sodium chloride Substances 0.000 claims description 36
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 claims description 33
- 239000001639 calcium acetate Substances 0.000 claims description 33
- 235000011092 calcium acetate Nutrition 0.000 claims description 33
- 229960005147 calcium acetate Drugs 0.000 claims description 33
- 238000001816 cooling Methods 0.000 claims description 33
- 239000002245 particle Substances 0.000 claims description 32
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 30
- 239000001632 sodium acetate Substances 0.000 claims description 30
- 235000017281 sodium acetate Nutrition 0.000 claims description 30
- 238000001914 filtration Methods 0.000 claims description 29
- 238000005406 washing Methods 0.000 claims description 25
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 23
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 17
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 17
- 235000011152 sodium sulphate Nutrition 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 15
- 239000001488 sodium phosphate Substances 0.000 claims description 14
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 14
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 14
- 235000007164 Oryza sativa Nutrition 0.000 claims description 13
- 235000009566 rice Nutrition 0.000 claims description 13
- 241000609240 Ambelania acida Species 0.000 claims description 10
- 241000196324 Embryophyta Species 0.000 claims description 10
- 239000010905 bagasse Substances 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 9
- 239000001110 calcium chloride Substances 0.000 claims description 7
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 7
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 4
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 4
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 4
- 239000011425 bamboo Substances 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 235000002639 sodium chloride Nutrition 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- 235000011008 sodium phosphates Nutrition 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 244000082204 Phyllostachys viridis Species 0.000 claims 1
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 239000003082 abrasive agent Substances 0.000 abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 1
- 229910052710 silicon Inorganic materials 0.000 abstract 1
- 239000010703 silicon Substances 0.000 abstract 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 14
- 229910001424 calcium ion Inorganic materials 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 14
- 239000002270 dispersing agent Substances 0.000 description 14
- 239000000706 filtrate Substances 0.000 description 14
- 241000209094 Oryza Species 0.000 description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 11
- 229910052802 copper Inorganic materials 0.000 description 11
- 239000010949 copper Substances 0.000 description 11
- 239000013049 sediment Substances 0.000 description 9
- 238000012360 testing method Methods 0.000 description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 241001330002 Bambuseae Species 0.000 description 3
- 229910018557 Si O Inorganic materials 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 3
- 229910008051 Si-OH Inorganic materials 0.000 description 2
- 229910006358 Si—OH Inorganic materials 0.000 description 2
- XAAHAAMILDNBPS-UHFFFAOYSA-L calcium hydrogenphosphate dihydrate Chemical compound O.O.[Ca+2].OP([O-])([O-])=O XAAHAAMILDNBPS-UHFFFAOYSA-L 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 240000000111 Saccharum officinarum Species 0.000 description 1
- 235000007201 Saccharum officinarum Nutrition 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 210000002268 wool Anatomy 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
- C01B33/20—Silicates
- C01B33/24—Alkaline-earth metal 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
- A61K2800/28—Rubbing or scrubbing compositions; Peeling or abrasive compositions; Containing exfoliants
-
- 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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
-
- 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
- C01P2006/82—Compositional purity water content
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Birds (AREA)
- Geology (AREA)
- Epidemiology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses calcium silicate with friction cleaning performance and capable of being used as toothpaste abrasive and a preparation method thereof, belonging to the field of oral cleaning care products; the preparation method of the calcium silicate comprises the following steps: step S1: mixing silicon-containing plant ash with sodium hydroxide solution for reaction to obtain water glass solution; or mixing quartz sand and sodium carbonate for reaction to obtain solid sodium silicate, and then dissolving the solid sodium silicate in water to obtain sodium silicate solution; or, reacting quartz sand with sodium hydroxide solution to obtain water glass solution; step S2: taking a sodium salt solution and a calcium salt solution; step S3: mixing and stirring the sodium salt solution, the water glass solution and the calcium salt solution for reaction to obtain a calcium silicate wet material, drying the calcium silicate wet material, and grinding to obtain calcium silicate powder. The novel calcium silicate abrasive agent prepared by the invention has compact structure and excellent abrasive performance, and meets the key performance index of toothpaste abrasive agent.
Description
Technical Field
The invention belongs to the field of oral cleaning care products, and particularly relates to calcium silicate with friction cleaning performance and capable of being used as a toothpaste abrasive and a preparation method thereof.
Background
The toothpaste abradant is one of the main raw materials of the toothpaste, and generally accounts for 20-50% of the formula.
Common toothpaste abrasives are natural calcium carbonate, dibasic calcium phosphate dihydrate, precipitated silica, aluminum hydroxide, light calcium carbonate, anhydrous dibasic calcium phosphate, etc., wherein natural calcium carbonate, dibasic calcium phosphate dihydrate, precipitated silica are currently the three most predominant abrasives. Conditions for use as a toothpaste abrasive should be: the abrasive should have proper hardness and friction value, uniform particle fineness, white appearance, no peculiar smell, comfortable taste, safety, no toxicity, small solubility and stable chemical property, and does not react with other components in the toothpaste.
At present, the preparation of the calcium silicate mainly comprises a high-temperature melting method, a hydrothermal precipitation method, a sol-gel method and the like; for example, calcium silicate can be prepared by calcining and melting calcium oxide and silicon dioxide at high temperature, but the calcium silicate prepared by the method is relatively hard and has relatively high energy consumption; for example, soluble calcium salts such as water glass, calcium chloride, calcium nitrate, calcium acetate and the like can be directly subjected to a hydrothermal method or a sol-gel method to prepare the calcium silicate, but the calcium silicate prepared by the methods basically has no friction performance and cannot be used as an abrasive in toothpaste.
Therefore, the research direction of the invention mainly aims at utilizing conventional quartz sand or renewable resources such as rice hull ash, bagasse ash and the like, and preparing the novel calcium silicate abrasive by using lower energy consumption and simple process technology, thereby enriching the raw materials of the toothpaste abrasive and promoting the green, environment-friendly and low-carbon sustainable development of the toothpaste industry.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a novel calcium silicate abrasive which is prepared by using conventional quartz sand and/or plant ash as raw materials and has certain abrasive cleaning performance and can be used as a toothpaste abrasive and a preparation method thereof.
In order to achieve the above purpose, the present invention discloses the following technical solutions:
in a first aspect, the invention discloses a method for preparing calcium silicate with friction cleaning performance, comprising the following steps:
step S1:
Mixing siliceous plant ash with sodium hydroxide solution, and reacting at a temperature of more than or equal to 90 ℃ to obtain sodium silicate solution;
Or alternatively, the first and second heat exchangers may be,
Mixing quartz sand and sodium carbonate, reacting at the temperature of more than or equal to 1200 ℃, cooling after the reaction to obtain solid sodium silicate, and dissolving the solid sodium silicate in water under the condition of steam pressurization to obtain a sodium silicate solution;
Or alternatively, the first and second heat exchangers may be,
Under the conditions that the vapor pressure is more than or equal to 0.6MPa and the temperature is more than or equal to 160 ℃, quartz sand reacts with sodium hydroxide solution, and filter residues are filtered to obtain sodium silicate solution;
step S2:
Dissolving soluble sodium salt in water to prepare sodium salt solution with concentration not less than 2 wt%;
dissolving soluble calcium salt in water to prepare calcium salt solution with concentration not less than 5 wt%;
step S3:
s3-1, mixing and stirring the sodium salt solution, the water glass solution and the calcium salt solution to obtain a mixed reactant;
S3-2, placing the mixed reactant at a temperature of more than or equal to 150 ℃ and a vapor pressure of more than or equal to 0.5MPa for reaction for 1-5h, and filtering to obtain a precipitate after the reaction to obtain a calcium silicate wet material;
S3-3, drying and grinding the wet calcium silicate material to obtain calcium silicate powder.
Preferably, the step S1 is to mix siliceous plant ash with sodium hydroxide solution, react at a temperature of more than or equal to 90 ℃, and obtain water glass solution through filtration, decolorization and washing.
Preferably, the siliceous plant ash in the step S1 is at least one of rice hull ash, bagasse ash, and bamboo ash;
The sodium hydroxide solution is sodium hydroxide solution with the concentration of 6-20wt%;
The mass ratio of the siliceous plant ash to the sodium hydroxide solution is 1 (2-6);
the mass ratio of the quartz sand to the sodium hydroxide solution is 1: (23-80).
Preferably, in the step S1, quartz sand and sodium carbonate are mixed, the mixture is reacted at the temperature of more than or equal to 1200 ℃, the reaction is carried out and then cooled to obtain solid water glass, and then the solid water glass is dissolved in water under the condition of steam pressurization to obtain a water glass solution, wherein the steam pressurization steam pressure is 0.43-0.50MPa.
Preferably, the quartz sand is quartz sand containing more than or equal to 99.0wt% of SiO 2;
The mass ratio of the quartz sand to the sodium carbonate in the step1 is 1: (0.8-1.5).
Preferably, the soluble sodium salt is at least one selected from sodium sulfate, sodium nitrate, sodium chloride, sodium acetate and sodium phosphate; the solute mass percentage of the sodium salt solution is 2-12%;
The soluble calcium salt is at least one selected from calcium nitrate, calcium chloride and calcium acetate; the solute mass percentage of the calcium salt solution is 5-20%.
Preferably, the volume ratio of the sodium salt solution, the water glass solution and the calcium salt solution in the step S3-1 is 1 (2.3-10): 0.6-4.
Preferably, the reaction temperature in the step S3-2 is 150-200 ℃, the vapor pressure is 0.5-1MPa, and the reaction time is 2-3h;
and step S3-2, washing the precipitate obtained by filtering after the reaction to obtain a calcium silicate wet material.
Preferably, the drying of the wet calcium silicate material in the step S3-3 is performed by the following method:
Drying the wet calcium silicate material at a temperature of more than or equal to 110 ℃ until the water content is less than or equal to 10%;
Or alternatively, the first and second heat exchangers may be,
Calcining the wet calcium silicate material at the temperature of more than or equal to 800 ℃ for 1-3h;
and (3) drying and grinding the wet calcium silicate material in the step (S3-3), wherein the particle size after grinding is 8-16 mu m.
In a second aspect, the invention discloses a calcium silicate having abrasive cleaning properties, prepared by any of the methods of preparation described above.
In a third aspect, the present invention discloses a toothpaste comprising a calcium silicate having abrasive cleaning properties according to the second aspect.
In the invention, the following components are added:
The key technical indexes of the calcium silicate prepared by the invention are as follows: the Whiteness (WG) is more than or equal to 96%, the pH value (5% suspension) is 8.0-10.5, the copper consumption (friction cleaning performance) is more than or equal to 2.0mg, and the technical indexes all meet the use requirements of the toothpaste abradant, and can be used as the toothpaste abradant.
In the preparation method, a sodium salt solution is added as a reaction medium, a large amount of electrolyte ions are provided in the reaction process, and calcium silicate generated by the reaction can generate stronger agglomeration when water glass solution and calcium salt solution are added, especially under the preferable specific adding proportion; the generated calcium silicate is compact in structure by combining a certain high temperature and a certain vapor pressure reaction condition, so that the friction cleaning performance of the calcium silicate is improved; especially, after the wet calcium silicate material is dried at high temperature, si-OH on the surface of the calcium silicate can be dehydrated, the arrangement among Si-O, si-O-Ca can be adjusted, the structure is more compact, and the compact structure ensures that the calcium silicate has better friction cleaning performance and is suitable for being used as a toothpaste abrasive.
The invention has the beneficial effects that:
1. The sodium salt solution, the water glass solution and the calcium salt solution have compact structures under the conditions of a certain adding proportion and high temperature above 150 ℃ and vapor pressure above 0.5MPa, and the friction cleaning performance of the calcium silicate is effectively improved.
2. The high-temperature drying dehydration can enable the structure of the calcium silicate to be more compact, and the friction performance of the friction agent is improved; especially, when the wet calcium silicate material is calcined at a high temperature of more than 800 ℃, the Si-OH on the surface of the calcium silicate can be dehydrated more thoroughly, the arrangement among Si-O, si-O-Ca is regulated, the structure is more compact, and the compact structure ensures that the calcium silicate has better friction cleaning performance.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in the following 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 description of the embodiments of the present invention will be presented in further detail with reference to the examples, which should be understood as being merely illustrative of the present invention and not limiting.
Preparation of example 1
Step S1, preparing water glass; the rice hull ash is put in sodium hydroxide solution with the concentration of 6 weight percent, and the mass ratio of the rice hull ash to the sodium hydroxide solution is 1:6, reacting at 90 ℃, and then filtering, decoloring and washing to obtain water glass solution;
Step S2, preparing a sodium sulfate solution and a calcium nitrate solution; a certain amount of sodium sulfate is taken and dissolved in water to prepare a sodium sulfate solution with the concentration of 2 weight percent. Dissolving a certain amount of calcium nitrate in water to prepare a calcium nitrate solution with the concentration of 20 wt%;
S3, preparing calcium silicate powder; taking the sodium sulfate solution prepared in the step S2 as a dispersing agent, and simultaneously adding the water glass solution prepared in the step S1 and the calcium nitrate solution prepared in the step S2 under the stirring condition, wherein the volume ratio of the sodium sulfate solution, the water glass solution and the calcium nitrate solution is 1:10:0.6, after stirring uniformly, transferring all the reaction materials into a pressure-resistant reaction tank, continuously reacting for 2 hours at the temperature of 150 ℃ and the vapor pressure of 0.5MPa, cooling to room temperature after the reaction, filtering reaction precipitate, repeatedly washing until filtrate does not contain calcium ions, obtaining a calcium silicate wet material, drying the calcium silicate wet material at the temperature of 110 ℃ until the water content is less than or equal to 10%, cooling, and crushing the calcium silicate wet material into particle powder with the particle size of 8-16 mu m through gas, thereby obtaining the calcium silicate powder of the embodiment 1.
Example 2 preparation
Step S1, preparing water glass; the bagasse ash is put in sodium hydroxide solution with the concentration of 7 weight percent, and the mass ratio of the bagasse ash to the sodium hydroxide solution is 1:4, reacting at 95 ℃, filtering, decolorizing and washing to obtain water glass solution;
s2, preparing a sodium chloride solution and a calcium chloride solution; a certain amount of sodium chloride is taken and dissolved in water to prepare a sodium chloride solution with the concentration of 3 weight percent. Dissolving a certain amount of calcium chloride in water to prepare a calcium chloride solution with the concentration of 6 wt%;
s3, preparing calcium silicate powder; taking the sodium chloride solution prepared in the step S2 as a dispersing agent, and simultaneously adding the sodium chloride solution prepared in the step S1 and the calcium chloride solution prepared in the step S2 under the stirring condition, wherein the volume ratio among the sodium chloride solution, the sodium chloride solution and the calcium chloride solution is 1:10:4, after stirring uniformly, transferring all the reaction materials into a pressure-resistant reaction tank, continuously reacting for 3 hours at 160 ℃ and under the vapor pressure of 0.6MPa, cooling to room temperature after the reaction, filtering reaction sediment, repeatedly washing until filtrate does not contain calcium ions, obtaining a calcium silicate wet material, drying the calcium silicate wet material at200 ℃ until the water content is less than or equal to 10%, and crushing the calcium silicate wet material into particle powder with the particle size of 8-16 mu m through gas after cooling, thereby obtaining the calcium silicate powder of the embodiment 2.
Example 3 preparation
Step S1, preparing water glass; the bamboo ash is put in sodium hydroxide solution with the concentration of 20 weight percent, and the mass ratio of the bamboo ash to the sodium hydroxide solution is 1:2, reacting at 100 ℃, and then filtering, decoloring and washing to obtain water glass solution;
S2, preparing a sodium phosphate solution and a calcium acetate solution; a certain amount of sodium phosphate is taken and dissolved in water to prepare a sodium phosphate solution with the concentration of 12 weight percent. Dissolving a certain amount of calcium acetate in water to prepare a calcium acetate solution with the concentration of 5 wt%;
S3, preparing calcium silicate powder; taking the sodium phosphate solution prepared in the step S2 as a dispersing agent, and simultaneously adding the sodium phosphate solution prepared in the step S1 and the calcium acetate solution prepared in the step S2 under the stirring condition, wherein the volume ratio of the sodium phosphate solution to the calcium acetate solution is 1:10:3, after stirring uniformly, transferring all the reaction materials into a pressure-resistant reaction tank, continuously reacting for 3 hours at the temperature of 200 ℃ and the vapor pressure of 1MPa, cooling to room temperature after the reaction, filtering reaction sediment, repeatedly washing until filtrate contains no calcium ions, obtaining a calcium silicate wet material, drying the calcium silicate wet material at the temperature of 200 ℃ until the water content is less than or equal to 10%, and crushing the calcium silicate wet material into particle powder with the particle size of 8-16 mu m through gas after cooling, thereby obtaining the calcium silicate powder of the embodiment 3.
Example 4 preparation
Step S1, preparing water glass; reacting quartz sand powder with the purity of 99.5% with sodium carbonate at the high temperature of 1300 ℃, wherein the mass ratio of the quartz sand powder to the sodium carbonate is 1:0.8, cooling after the reaction to obtain solid water glass, and redissolving the solid water glass in water under the vapor pressure condition of 0.43MPa to obtain a water glass solution;
s2, preparing a sodium acetate solution and a calcium chloride solution; a certain amount of sodium acetate is taken and dissolved in water to prepare sodium acetate solution with the concentration of 5 weight percent. Dissolving a certain amount of calcium chloride in water to prepare a calcium chloride solution with the concentration of 7 wt%;
S3, preparing calcium silicate powder; taking the sodium acetate solution prepared in the step S2 as a dispersing agent, and simultaneously adding the sodium acetate solution prepared in the step S1 and the calcium chloride solution prepared in the step S2 under the stirring condition, wherein the volume ratio among the sodium acetate solution, the sodium acetate solution and the calcium chloride solution is 1:2.3:4, after stirring uniformly, transferring all the reaction materials into a pressure-resistant reaction tank, continuously reacting for 4 hours at the temperature of 170 ℃ and the vapor pressure of 0.65MPa, cooling to room temperature after reaction, filtering reaction sediment, repeatedly washing until filtrate does not contain calcium ions, obtaining a calcium silicate wet material, drying the calcium silicate wet material at the temperature of 300 ℃, drying until the water content is less than or equal to 10%, and crushing the calcium silicate wet material into particle powder with the particle size of 8-16 mu m through gas after cooling, thereby obtaining the calcium silicate powder of the embodiment 4.
Example 5 preparation
Step S1, preparing water glass; reacting quartz sand powder with the purity of 99.0% with sodium carbonate at the high temperature of 1200 ℃, wherein the mass ratio of the quartz sand powder to the sodium carbonate is 1:1.5, cooling after the reaction to obtain solid water glass, and redissolving the solid water glass in water under the vapor pressure condition of 0.50MPa to obtain a water glass solution;
Step S2, preparing a sodium chloride solution and a calcium acetate solution; a certain amount of sodium chloride is taken and dissolved in water to prepare a sodium chloride solution with the concentration of 6 weight percent. Dissolving a certain amount of calcium acetate in water to prepare a 10wt% calcium acetate solution;
S3, preparing calcium silicate powder; taking the sodium chloride solution prepared in the step S2 as a dispersing agent, and simultaneously adding the sodium chloride solution prepared in the step S1 and the calcium acetate solution prepared in the step S2 under the stirring condition, wherein the volume ratio among the sodium chloride solution, the sodium chloride solution and the calcium acetate solution is 1:2.3:4, after uniformly stirring, transferring all the reaction materials into a pressure-resistant reaction tank, continuously reacting for 4 hours at the temperature of 170 ℃ and the vapor pressure of 0.65MPa, cooling to room temperature after the reaction, filtering reaction sediment, repeatedly washing until filtrate does not contain calcium ions, obtaining a calcium silicate wet material, drying the calcium silicate wet material at the temperature of 300 ℃, drying until the water content is less than or equal to 10%, and crushing the calcium silicate wet material into particle powder with the particle size of 8-16 mu m through gas after cooling, thereby obtaining the calcium silicate powder of the embodiment 5.
Example 6 preparation
Step S1, preparing water glass; reacting quartz sand with the purity of 99.3% with a sodium hydroxide solution with the concentration of 6wt% under the conditions of the vapor pressure of 0.70MPa and the temperature of 165 ℃, wherein the mass ratio of the quartz sand to the sodium hydroxide solution is 1:80, filtering to obtain water glass solution;
S2, preparing a sodium phosphate solution and a calcium acetate solution; a certain amount of sodium phosphate is taken and dissolved in water to prepare sodium phosphate solution with the concentration of 5 weight percent. Dissolving a certain amount of calcium acetate in water to prepare a calcium acetate solution with the concentration of 6 wt%;
S3, preparing calcium silicate powder; taking the sodium phosphate solution prepared in the step S2 as a dispersing agent, and simultaneously adding the sodium phosphate solution prepared in the step S1 and the calcium acetate solution prepared in the step S2 under the stirring condition, wherein the volume ratio of the sodium phosphate solution to the calcium acetate solution is 1:2.3:3, after stirring uniformly, transferring all the reaction materials into a pressure-resistant reaction tank, continuously reacting for 2.5 hours at the temperature of 180 ℃ and the vapor pressure of 0.85MPa, cooling to room temperature after the reaction, filtering reaction precipitate, repeatedly washing until filtrate does not contain calcium ions, obtaining a calcium silicate wet material, calcining the calcium silicate wet material at the temperature of 800 ℃, calcining for 3 hours, cooling, and crushing the calcium silicate wet material into particle powder with the particle size of 8-16 mu m through gas, thereby obtaining the calcium silicate powder of the example 6.
Example 7 preparation
Step S1, preparing water glass; reacting quartz sand with the purity of 99.3% with a sodium hydroxide solution with the concentration of 20wt% under the conditions of the vapor pressure of 0.60MPa and the temperature of 165 ℃, wherein the mass ratio of the quartz sand to the sodium hydroxide solution is 1:23, filtering to obtain water glass solution;
S2, preparing a sodium acetate solution and a calcium acetate solution; a certain amount of sodium acetate is taken and dissolved in water to prepare sodium acetate solution with the concentration of 6 weight percent. Dissolving a certain amount of calcium acetate in water to prepare a 10wt% calcium acetate solution;
S3, preparing calcium silicate powder; taking the sodium acetate solution prepared in the step S2 as a dispersing agent, and simultaneously adding the sodium acetate solution prepared in the step S1 and the calcium acetate solution prepared in the step S2 under the stirring condition, wherein the volume ratio among the sodium acetate solution, the sodium acetate solution and the calcium acetate solution is 1:5:2, after stirring uniformly, transferring all the reaction materials into a pressure-resistant reaction tank, continuously reacting for 3 hours at the temperature of 200 ℃ and the vapor pressure of 1MPa, cooling to room temperature after the reaction, filtering reaction sediment, repeatedly washing until filtrate contains no calcium ions, obtaining a calcium silicate wet material, calcining the calcium silicate wet material at the temperature of 800 ℃ for 3 hours, and crushing the calcium silicate wet material into particle powder with the particle size of 8-16 mu m through gas after cooling, thereby obtaining the calcium silicate powder of the example 7.
Example 8 preparation
Step S1, preparing water glass; the rice hull ash is put in sodium hydroxide solution with the concentration of 8 weight percent, and the mass ratio of the rice hull ash to the sodium hydroxide solution is 1:4, reacting at 95 ℃, filtering, decolorizing and washing to obtain water glass solution;
Step S2, preparing a sodium chloride solution and a calcium nitrate solution; a certain amount of sodium chloride is taken and dissolved in water to prepare a sodium chloride solution with the concentration of 8 weight percent. Dissolving a certain amount of calcium nitrate in water to prepare a calcium nitrate solution with the concentration of 8 wt%;
S3, preparing calcium silicate powder; taking the sodium chloride solution prepared in the step S2 as a dispersing agent, and simultaneously adding the sodium chloride solution prepared in the step S1 and the calcium nitrate solution prepared in the step S2 under the stirring condition, wherein the volume ratio of the sodium chloride solution to the calcium nitrate solution is 1:10:1, after stirring uniformly, transferring all the reaction materials into a pressure-resistant reaction tank, continuously reacting for 3 hours at the temperature of 155 ℃ and the vapor pressure of 0.5MPa, cooling to room temperature after the reaction, filtering reaction sediment, repeatedly washing until filtrate does not contain calcium ions, obtaining a calcium silicate wet material, calcining the calcium silicate wet material at the temperature of 850 ℃ for 2 hours, and crushing the calcium silicate wet material into particle powder with the particle size of 8-16 mu m through gas after cooling to obtain the calcium silicate powder of the embodiment 8.
Example 9 preparation
Step S1, preparing water glass; the bagasse ash is put in 10wt% sodium hydroxide solution, and the mass ratio of the bagasse ash to the sodium hydroxide solution is 1:4, reacting at 98 ℃, and then filtering, decoloring and washing to obtain water glass solution;
Step S2, preparing a sodium chloride solution and a calcium acetate solution; a certain amount of sodium chloride is taken and dissolved in water to prepare a sodium chloride solution with the concentration of 10 weight percent. Dissolving a certain amount of calcium acetate in water to prepare a calcium acetate solution with the concentration of 6 wt%;
S3, preparing calcium silicate powder; taking the sodium chloride solution prepared in the step S2 as a dispersing agent, and simultaneously adding the sodium chloride solution prepared in the step S1 and the calcium acetate solution prepared in the step S2 under the stirring condition, wherein the volume ratio among the sodium chloride solution, the sodium chloride solution and the calcium acetate solution is 1:10:1, after stirring uniformly, transferring all the reaction materials into a pressure-resistant reaction tank, continuously reacting for 3.5 hours at the temperature of 150 ℃ and the vapor pressure of 0.45MPa, cooling to room temperature after the reaction, filtering reaction precipitate, repeatedly washing until filtrate does not contain calcium ions, obtaining a calcium silicate wet material, calcining the calcium silicate wet material at the temperature of 900 ℃, calcining for 1 hour, cooling, and crushing the calcium silicate wet material into particle powder with the particle size of 8-16 mu m through gas, thereby obtaining the calcium silicate powder of the embodiment 9.
Preparation of comparative example 1
Step S1, preparing water glass; the rice hull ash is put in sodium hydroxide solution with the concentration of 6 weight percent, and the mass ratio of the rice hull ash to the sodium hydroxide solution is 1:6, reacting at 90 ℃, and then filtering, decoloring and washing to obtain water glass solution;
Step S2, preparing a sodium sulfate solution and a calcium nitrate solution; a certain amount of sodium sulfate is taken and dissolved in water to prepare a sodium sulfate solution with the concentration of 2 weight percent. Dissolving a certain amount of calcium nitrate in water to prepare a calcium nitrate solution with the concentration of 20 wt%;
S3, preparing calcium silicate powder; taking the sodium sulfate solution prepared in the step S2 as a dispersing agent, and simultaneously adding the water glass solution prepared in the step S1 and the calcium nitrate solution prepared in the step S2 under the stirring condition, wherein the volume ratio of the sodium sulfate solution, the water glass solution and the calcium nitrate solution is 1:10: and 0.6, uniformly stirring, transferring all the reaction materials into a pressure-resistant reaction tank, continuously reacting for 1 hour at the temperature of 130 ℃ and the vapor pressure of 0.3MPa, cooling to room temperature after the reaction, filtering reaction precipitate, repeatedly washing until filtrate does not contain calcium ions to obtain a calcium silicate wet material, drying the calcium silicate wet material at the temperature of 110 ℃, drying until the water content is less than or equal to 10%, cooling, and crushing the calcium silicate wet material into particle powder with the particle size of 8-16 mu m through gas to obtain the calcium silicate powder of comparative example 1.
Preparation of comparative example 2
Step S1, preparing water glass; the bagasse ash is put in sodium hydroxide solution with the concentration of 7 weight percent, and the mass ratio of the bagasse ash to the sodium hydroxide solution is 1:4, reacting at 95 ℃, filtering, decolorizing and washing to obtain water glass solution;
s2, preparing a sodium chloride solution and a calcium chloride solution; a certain amount of sodium chloride is taken and dissolved in water to prepare a sodium chloride solution with the concentration of 3 weight percent. Dissolving a certain amount of calcium chloride in water to prepare a calcium chloride solution with the concentration of 6 wt%;
S3, preparing calcium silicate powder; taking the sodium chloride solution prepared in the step S2 as a dispersing agent, and simultaneously adding the sodium chloride solution prepared in the step S1 and the calcium chloride solution prepared in the step S2 under the stirring condition, wherein the volume ratio among the sodium chloride solution, the sodium chloride solution and the calcium chloride solution is 1:10:4, after uniformly stirring, transferring all the reaction materials into a pressure-resistant reaction tank, continuously reacting for 1 hour at the temperature of 120 ℃ and the vapor pressure of 0.2MPa, cooling to room temperature after the reaction, filtering reaction sediment, repeatedly washing until filtrate does not contain calcium ions, obtaining a calcium silicate wet material, drying the calcium silicate wet material at the temperature of 110 ℃, drying until the water content is less than or equal to 10%, and crushing the calcium silicate wet material into particle powder with the particle size of 8-16 mu m through gas after cooling, thereby obtaining the calcium silicate powder of comparative example 2.
Preparation of comparative example 3
Step S1, preparing water glass; reacting quartz sand powder with the purity of 99.5% with sodium carbonate at the high temperature of 1300 ℃, wherein the mass ratio of the quartz sand powder to the sodium carbonate is 1:0.8, cooling after the reaction to obtain solid water glass, and redissolving the solid water glass in water under the vapor pressure condition of 0.43MPa to obtain a water glass solution;
s2, preparing a sodium acetate solution and a calcium chloride solution; a certain amount of sodium acetate is taken and dissolved in water to prepare sodium acetate solution with the concentration of 5 weight percent. Dissolving a certain amount of calcium chloride in water to prepare a calcium chloride solution with the concentration of 7 wt%;
S3, preparing calcium silicate powder; taking the sodium acetate solution prepared in the step S2 as a dispersing agent, and simultaneously adding the sodium acetate solution prepared in the step S1 and the calcium chloride solution prepared in the step S2 under the stirring condition, wherein the volume ratio among the sodium acetate solution, the sodium acetate solution and the calcium chloride solution is 1:2:1, after stirring uniformly, transferring all the reaction materials into a pressure-resistant reaction tank, continuously reacting for 4 hours at the temperature of 170 ℃ and the vapor pressure of 0.65MPa, cooling to room temperature after reaction, filtering reaction sediment, repeatedly washing until filtrate does not contain calcium ions, obtaining a calcium silicate wet material, drying the calcium silicate wet material at the temperature of 300 ℃, drying until the water content is less than or equal to 10%, and crushing the calcium silicate wet material into particle powder with the particle size of 8-16 mu m through gas after cooling, thereby obtaining the calcium silicate powder of the embodiment 4.
Preparation of comparative example 4
Step S1, preparing water glass; reacting quartz sand with the purity of 99.3% with a sodium hydroxide solution with the concentration of 20wt% under the conditions of the vapor pressure of 0.60MPa and the temperature of 165 ℃, wherein the mass ratio of the quartz sand to the sodium hydroxide solution is 1:23, filtering to obtain water glass solution;
S2, preparing a sodium acetate solution and a calcium acetate solution; a certain amount of sodium acetate is taken and dissolved in water to prepare sodium acetate solution with the concentration of 6 weight percent. Dissolving a certain amount of calcium acetate in water to prepare a 10wt% calcium acetate solution;
s3, preparing calcium silicate powder; taking the sodium acetate solution prepared in the step S2 as a dispersing agent, and simultaneously adding the sodium acetate solution prepared in the step S1 and the calcium acetate solution prepared in the step S2 under the stirring condition, wherein the volume ratio among the sodium acetate solution, the sodium acetate solution and the calcium acetate solution is 1:1:1, after stirring uniformly, transferring all the reaction materials into a pressure-resistant reaction tank, continuously reacting for 3 hours at the temperature of 200 ℃ and the vapor pressure of 1MPa, cooling to room temperature after the reaction, filtering reaction sediment, repeatedly washing until filtrate does not contain calcium ions, obtaining a calcium silicate wet material, calcining the calcium silicate wet material at the temperature of 800 ℃ for 3 hours, and crushing the calcium silicate wet material into particle powder with the particle size of 8-16 mu m through gas after cooling, thereby obtaining the calcium silicate powder of comparative example 4.
Preparation of comparative example 5
Step S1, preparing water glass; the rice hull ash is put in sodium hydroxide solution with the concentration of 6 weight percent, and the mass ratio of the rice hull ash to the sodium hydroxide solution is 1:6, reacting at 90 ℃, and then filtering, decoloring and washing to obtain water glass solution;
Step S2, preparing a sodium sulfate solution and a calcium nitrate solution; a certain amount of sodium sulfate is taken and dissolved in water to prepare a sodium sulfate solution with the concentration of 2 weight percent. Dissolving a certain amount of calcium nitrate in water to prepare a calcium nitrate solution with the concentration of 20 wt%;
S3, preparing calcium silicate powder; taking the sodium sulfate solution prepared in the step S2 as a dispersing agent, and simultaneously adding the water glass solution prepared in the step S1 and the calcium nitrate solution prepared in the step S2 under the stirring condition, wherein the volume ratio of the sodium sulfate solution, the water glass solution and the calcium nitrate solution is 1:10: and 0.6, uniformly stirring, transferring all the reaction materials into a pressure-resistant reaction tank, continuously reacting for 1 hour at the temperature of 130 ℃ and the vapor pressure of 0.3MPa, cooling to room temperature after the reaction, filtering reaction precipitate, repeatedly washing until filtrate does not contain calcium ions to obtain a calcium silicate wet material, drying the calcium silicate wet material at the temperature of 105 ℃ until the water content is less than or equal to 10%, cooling, and crushing the calcium silicate wet material into particle powder with the particle size of 8-16 mu m through gas to obtain the calcium silicate powder of comparative example 5.
Performance testing
(1) Technical indexes such as Whiteness (WG), pH value and the like are detected by referring to QB/T2346-2015 silica for toothpaste of oral cleaning care products, and the results are shown in table 1;
(2) The frictional cleaning performance of the calcium silicate powder was evaluated by copper loss values, and the results are shown in Table 1.
The method for measuring the copper loss value comprises the following steps: fixing a wool circular pad on a friction head of an instrument by adopting an excessively hard particle tester, taking a copper sheet to be subjected to abrasion test, namely the mass of the copper sheet is M1, loading the copper sheet to be subjected to abrasion test into a test groove, adding a dispersed calcium silicate powder aqueous dispersion (the mass ratio of calcium silicate powder to aqueous dispersion is 20:100), starting the instrument to perform abrasion test on the copper sheet for 1 ten thousand times, taking out the copper sheet after the test is finished, cleaning, drying and weighing, and measuring the copper sheet mass to be M2, wherein the copper loss value of the calcium silicate powder is M (mg), and M=M1-M2; theoretically, the larger M is, the larger the abrasion of the powder on the copper sheet is, which indicates that the better the friction cleaning performance is.
Table 1 examples, comparative examples test data
Analysis of results
1. According to the preparation method, the conventional quartz sand and/or siliceous plant ash can be utilized to prepare the calcium silicate abrasive meeting technical indexes.
2. As is clear from the comparison of examples 1 to 2 with comparative examples 1 to 2, under the high temperature of 150 ℃ or higher and the vapor pressure reaction condition of 0.5MPa or higher, the produced calcium silicate has a compact structure, and the friction cleaning performance of the calcium silicate is effectively improved.
3. As is clear from the comparison of example 1 and comparative examples 1 and 5, the high-temperature drying and dewatering can make the structure of the calcium silicate more compact, and improve the friction performance of the friction agent.
4. Examples 1-9 show that the wet calcium silicate material is calcined at high temperature over 800 deg.c to eliminate water from Si-OH on the surface of calcium silicate, regulate the arrangement of Si-O, si-O-Ca and compact structure to result in excellent friction and cleaning performance.
5. From the results of the performance tests of example 4 and comparative example 3, example 5 and comparative example 4, it is understood that the preferred volume ratio of the sodium salt solution, the water glass solution and the calcium salt solution of the present invention can effectively improve the friction cleaning performance of the calcium silicate abrasive.
The water glass adopted by the invention is derived from conventional quartz sand, and can also be derived from renewable resources such as rice hull ash, bagasse ash and the like; the novel calcium silicate abrasive prepared by the invention enriches the raw materials of the toothpaste abrasive, and is beneficial to promoting the development of the toothpaste industry; in particular, the renewable resources such as rice hull ash, sugarcane ash and the like are utilized to prepare the calcium silicate, which is beneficial to the green environmental protection and low carbon sustainable development of the toothpaste industry and the technical progress of the toothpaste industry.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A method for preparing calcium silicate for toothpaste abrasive with friction cleaning performance, which is characterized by comprising the following steps:
step S1:
Mixing siliceous plant ash with sodium hydroxide solution, and reacting at a temperature of more than or equal to 90 ℃ to obtain sodium silicate solution;
Or alternatively, the first and second heat exchangers may be,
Mixing quartz sand and sodium carbonate, reacting at the temperature of more than or equal to 1200 ℃, cooling after the reaction to obtain solid sodium silicate, and dissolving the solid sodium silicate in water under the condition of steam pressurization to obtain a sodium silicate solution;
Or alternatively, the first and second heat exchangers may be,
Under the conditions that the vapor pressure is more than or equal to 0.6MPa and the temperature is more than or equal to 160 ℃, quartz sand reacts with sodium hydroxide solution, and filter residues are filtered to obtain sodium silicate solution;
step S2:
Taking sodium salt solution with the solute mass percentage of 2-12%;
Taking a calcium salt solution with the solute mass percentage of 5-20%;
step S3:
s3-1, mixing and stirring the sodium salt solution, the water glass solution and the calcium salt solution to obtain a mixed reactant;
s3-2, placing the mixed reactant at the temperature of 150-200 ℃ and the vapor pressure of 0.5-1MPa for reaction for 2-3 hours, filtering the reaction product to obtain a precipitate, and washing the precipitate to obtain a wet calcium silicate material;
s3-3, drying and grinding the wet calcium silicate material to obtain calcium silicate powder;
The volume ratio of the sodium salt solution, the water glass solution and the calcium salt solution in the step S3-1 is 1 (2.3-10) (0.6-4);
the wet calcium silicate material in the step S3-3 is dried by the following method:
Drying the wet calcium silicate material at a temperature of more than or equal to 110 ℃ until the water content is less than or equal to 10%;
Or alternatively, the first and second heat exchangers may be,
Calcining the wet calcium silicate material at the temperature of more than or equal to 800 ℃ for 1-3h;
The sodium salt solution solute is at least one selected from sodium sulfate, sodium nitrate, sodium chloride, sodium acetate and sodium phosphate;
the solute of the calcium salt solution is at least one selected from calcium nitrate, calcium chloride and calcium acetate.
2. The method for preparing calcium silicate with friction cleaning performance for toothpaste abrasive according to claim 1, wherein the step S1 is to mix siliceous plant ash with sodium hydroxide solution, react at a temperature of not less than 90 ℃, filter, decolorize, wash to obtain sodium silicate solution;
The siliceous plant ash in the step S1 is at least one of rice hull ash, bagasse ash and bamboo ash;
The sodium hydroxide solution is sodium hydroxide solution with the concentration of 6-20wt%;
The mass ratio of the siliceous plant ash to the sodium hydroxide solution is 1 (2-6);
the mass ratio of the quartz sand to the sodium hydroxide solution is 1: (23-80).
3. The method for preparing calcium silicate for toothpaste abrasive with friction cleaning performance according to claim 1, wherein in the step S1, quartz sand and sodium carbonate are mixed, reacted at a temperature of not less than 1200 ℃, cooled after the reaction to obtain solid water glass, and then the solid water glass is dissolved in water under a steam pressurizing condition to obtain a water glass solution, wherein the steam pressurizing steam pressure is 0.43-0.50MPa.
4. The method for preparing calcium silicate for toothpaste abrasive having abrasive cleaning performance according to claim 1, wherein the quartz sand is quartz sand containing SiO 2 not less than 99.0 wt%;
The mass ratio of the quartz sand to the sodium carbonate in the step S1 is 1: (0.8-1.5).
5. The method for preparing calcium silicate for toothpaste abrasive having abrasive cleaning performance according to claim 1, wherein the wet calcium silicate material in step S3-3 is dried and then ground, and the ground particle size is 8-16 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311669947.7A CN117466305B (en) | 2023-12-07 | 2023-12-07 | Calcium silicate with friction cleaning performance and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311669947.7A CN117466305B (en) | 2023-12-07 | 2023-12-07 | Calcium silicate with friction cleaning performance and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN117466305A CN117466305A (en) | 2024-01-30 |
| CN117466305B true CN117466305B (en) | 2024-06-11 |
Family
ID=89629452
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311669947.7A Active CN117466305B (en) | 2023-12-07 | 2023-12-07 | Calcium silicate with friction cleaning performance and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117466305B (en) |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3132422A1 (en) * | 1981-08-17 | 1983-02-24 | Robert Bosch Gmbh, 7000 Stuttgart | Electrically insulating assembly aid for interfaces in high-voltage connection means |
| CN102020272A (en) * | 2009-09-17 | 2011-04-20 | 黑龙江万禾园油脂有限公司 | Production method for water glass and active carbon by using rice husk ash |
| CN102215913A (en) * | 2008-06-03 | 2011-10-12 | J.M.休伯有限公司 | Transparent silica gel/precipitated silica composite materials for dentifrices |
| CN103228245A (en) * | 2010-10-06 | 2013-07-31 | 可乐丽则武齿科株式会社 | Dental canaliculi sealing agent and method for producing same |
| CN107686118A (en) * | 2017-08-23 | 2018-02-13 | 内蒙古普诺思新材料科技有限公司 | A kind of method that liquid phase dynamic autoclaved technology method prepares calcium silicate powder |
| CN107892307A (en) * | 2017-11-29 | 2018-04-10 | 东北大学 | Utilize the method for soda lime sintering process red mud alkaline process synthetic calcium silicate |
| CN108191374A (en) * | 2018-04-02 | 2018-06-22 | 内蒙古普诺思新材料科技有限公司 | A kind of method for synthesizing lightweight calcium-silicate thermal insulation material |
| CN108821300A (en) * | 2018-08-06 | 2018-11-16 | 东北大学 | One kind preparing CaSiO by discarded silicon slag3Method |
| CN110769801A (en) * | 2017-06-07 | 2020-02-07 | 荷兰联合利华有限公司 | Oral care compositions |
| CN111704143A (en) * | 2020-03-06 | 2020-09-25 | 宣全 | Production process for preparing composite calcium silicate by using rice hull ash |
| CN113200553A (en) * | 2021-06-04 | 2021-08-03 | 金三江(肇庆)硅材料股份有限公司 | Calcium silicate and preparation method and application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MXPA05008191A (en) * | 2003-02-05 | 2006-02-17 | Fmc Corp | Toothpaste compositions with reduced abrasivity. |
-
2023
- 2023-12-07 CN CN202311669947.7A patent/CN117466305B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3132422A1 (en) * | 1981-08-17 | 1983-02-24 | Robert Bosch Gmbh, 7000 Stuttgart | Electrically insulating assembly aid for interfaces in high-voltage connection means |
| CN102215913A (en) * | 2008-06-03 | 2011-10-12 | J.M.休伯有限公司 | Transparent silica gel/precipitated silica composite materials for dentifrices |
| CN102020272A (en) * | 2009-09-17 | 2011-04-20 | 黑龙江万禾园油脂有限公司 | Production method for water glass and active carbon by using rice husk ash |
| CN103228245A (en) * | 2010-10-06 | 2013-07-31 | 可乐丽则武齿科株式会社 | Dental canaliculi sealing agent and method for producing same |
| CN110769801A (en) * | 2017-06-07 | 2020-02-07 | 荷兰联合利华有限公司 | Oral care compositions |
| CN107686118A (en) * | 2017-08-23 | 2018-02-13 | 内蒙古普诺思新材料科技有限公司 | A kind of method that liquid phase dynamic autoclaved technology method prepares calcium silicate powder |
| CN107892307A (en) * | 2017-11-29 | 2018-04-10 | 东北大学 | Utilize the method for soda lime sintering process red mud alkaline process synthetic calcium silicate |
| CN108191374A (en) * | 2018-04-02 | 2018-06-22 | 内蒙古普诺思新材料科技有限公司 | A kind of method for synthesizing lightweight calcium-silicate thermal insulation material |
| CN108821300A (en) * | 2018-08-06 | 2018-11-16 | 东北大学 | One kind preparing CaSiO by discarded silicon slag3Method |
| CN111704143A (en) * | 2020-03-06 | 2020-09-25 | 宣全 | Production process for preparing composite calcium silicate by using rice hull ash |
| CN113200553A (en) * | 2021-06-04 | 2021-08-03 | 金三江(肇庆)硅材料股份有限公司 | Calcium silicate and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| Medvecky, L et al..Effect of tetracalcium phosphate/monetite toothpaste on dentin remineralization and tubule occlusion in vitro.《DENTAL MATERIALS》.2017,第34卷(第3期),442-451. * |
| 丁积善等.单淀粉单磷酸盐牙膏.《日用化学品科学》.1980,(第2期),第56-57. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN117466305A (en) | 2024-01-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101423257B (en) | Method for preparing nano grade iron oxide red | |
| CN107686118B (en) | Method for preparing calcium silicate powder by liquid-phase dynamic hydrothermal synthesis method | |
| CN108083312B (en) | A kind of carbonization reactor and preparation small particle, polymolecularity, low oil factor nanometer calcium carbonate method | |
| CN104386726B (en) | A kind of solid state chemical reaction prepares the method for vaterite-type calcium carbonate microsphere | |
| CN106315573A (en) | Preparation method of modified graphene and cement composite material thereof | |
| CN103303929A (en) | Preparation method of high-transparency high-dispersity white carbon black | |
| CN103571334A (en) | Cerium oxide polishing powder and preparation method thereof | |
| CN113353962A (en) | Method for preparing active nano calcium carbonate at normal temperature and high concentration | |
| US4049781A (en) | Method of preparing loosely aggregated 200-500 millimicron silica | |
| CN117466305B (en) | Calcium silicate with friction cleaning performance and preparation method thereof | |
| CN114698646A (en) | Preparation method of flaky ellipsoidal zirconium phosphate silver-zinc-loaded antibacterial powder | |
| CN102329571B (en) | Rare earth and silicon compound precision type rare earth polishing powder and preparation method thereof | |
| US2996369A (en) | Zirconium oxide and process of making the same | |
| CN105271344A (en) | Preparation method of pine-cone-shaped calcite type micron-size calcium carbonate particles | |
| JP4785068B2 (en) | Synthetic amorphous aluminum bonded silicate and process for producing the same | |
| CN101450805B (en) | Novel process for synthesizing molecular sieve by calcining fly ash through wet alkalization | |
| CN116199270B (en) | Treatment process for reducing wastewater in cobalt oxide production process | |
| JP3020143B2 (en) | Method for producing desulfurizing agent | |
| CN108525668A (en) | The preparation method of the nano-fibre supported cobalt aluminum composite oxide of sepiolite | |
| CN113321221A (en) | Method for preparing white carbon black by using iron tailings | |
| CN104860344B (en) | Preparation method of spherical strontium carbonate | |
| JPS58104018A (en) | Manufacture of calcium silicate and its product | |
| CN100567171C (en) | A kind of method for preparing high specific surface area meso-porous nickelous oxide | |
| CN112723331A (en) | Preparation method of high-purity nanometer neodymium phosphate powder | |
| CN111747421A (en) | Method for improving activity of expanded perlite material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |