CN107720763B - A kind of preparation method of high dispersive silica - Google Patents

A kind of preparation method of high dispersive silica Download PDF

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CN107720763B
CN107720763B CN201711161602.5A CN201711161602A CN107720763B CN 107720763 B CN107720763 B CN 107720763B CN 201711161602 A CN201711161602 A CN 201711161602A CN 107720763 B CN107720763 B CN 107720763B
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silica
sulfuric acid
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CN107720763A (en
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庹文喜
林英光
张梦梅
胡荷燕
任振雪
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GUANGZHOU FEIXUE MATERIAL TECHNOLOGY Co Ltd
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    • 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
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/02—Inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/12—Water-insoluble compounds
    • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area

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Abstract

The present invention provides a kind of preparation method of high dispersive silica, and step includes: 1), by sodium metasilicate Na2O·nSiO2Add water to be modulated into sodium silicate solution, stir evenly, obtains sodium silicate solution；2) it is spare, to prepare metabisulfite solution stirring；3) it is spare, to prepare sulfuric acid solution；4) sodium silicate solution is added after, dissolving sodium hexametaphosphate dispersant；5) metabisulfite solution, is added into reaction kettle, heats, stirring, at the uniform velocity addition sulfuric acid solution；6) sodium silicate solution, is added and sulfuric acid solution carries out neutralization reaction, stops being added after sodium silicate solution addition, continues to add sulfuric acid solution；7), pressure filtration washing obtains product by being crushed crusher machine with air-flow after spray drying.The preparation method of high dispersive silica provided by the invention, the preparation method simple process, the dispersibility for obtaining silica is higher, is suitably applied daily use chemicals industry and does supporting surfactant or do dispersing agent applied to pharmaceuticals industry.

Description

A kind of preparation method of high dispersive silica
Technical field
The present invention relates to the preparation field of silica, in particular to a kind of preparation method of high dispersive silica.
Background technique
Silica is manufacture glass, quartz glass, waterglass, optical fiber, the important component of electronics industry, optics instrument The raw material of device, craftwork and refractory material is the important materials of scientific research.In recent years, silica is used for battery separator Material, partition pore-forming are made up of silica micropore itself and pore former the hole left after extraction or volatilization, This porous and detour structure, it is desirable that the advantages that its specific surface area is low, electrolyte storage characteristics are good.Silica has greatly well Tackifying effect is widely used in all trades and professions because it is with very high electrical insulating property and good dispersibility.To meet different use The requirement of the silica on way, certain fields require the dispersibility of silica high, and dispersed quality is to measure silica etc. One important indicator of grade.
There are mainly two types of the production methods of silica: vapor phase method and the precipitation method, and the silica of vapor phase method production is general Physical and chemical performance is all fine, but vapor phase method raw material are expensive, equipment requirement is high, technology is complicated, low output.The precipitation method mostly use sulphur Acid or hydrochloric acid and sodium metasilicate carry out neutralization reaction, and simple process, equipment and raw material are cheap, but product quality has with vapor phase method Larger difference.There are many precipitated silica manufacturers in the country, but most of product is all located in conventional tyre and system Collar domain, belongs to general silica, and dispersed quality is to measure an important indicator of silica grades, polymolecularity two Silica is mainly monopolized by giants such as French Rhodia, U.S. PPG, German Degussas in the world.
Summary of the invention
In conclusion it is necessary to provide a kind of preparation method of high dispersive silica, the preparation method works by the present invention Skill is simple, and the dispersibility for obtaining silica is higher, is suitably applied daily use chemicals industry and does supporting surfactant or be applied to Pharmaceuticals industry does dispersing agent.
A kind of preparation method of high dispersive silica, step include:
1), by sodium metasilicate Na2O·nSiO2Add water to be modulated into sodium silicate solution, stir evenly, obtains sodium silicate solution；
2) it is spare, to prepare metabisulfite solution stirring；
3) it is spare, to prepare sulfuric acid solution；
4) after, sodium hexametaphosphate dispersant is dissolved be added step 1) in sodium silicate solution in stir 30 minutes it is spare；
5) metabisulfite solution, is added into reaction kettle, heats, is added with stirring the resulting solution of step 4), stirs, at the uniform velocity Sulfuric acid solution is added and carries out acid-base neutralization reaction, stops acid adding when pH value reaches 8.5, is warming up to 85-95 DEG C；
6) sodium silicate solution, is added and sulfuric acid solution carries out neutralization reaction, keeping the pH value of reaction solution is 8.5, works as silicic acid Sodium solution stops being added after adding, and continues to add sulfuric acid solution, when pH value reaches 4-5, stops addition, continues to stir；
7) silica of formation, is subjected to pressure filtration washing, when salt content≤2% of washing water, after spray drying Being crushed to partial size with air-flow crusher is 4-6 μm.
Preferably, the preparation method of the high dispersive silica, step include:
1), by sodium metasilicate Na2O·nSiO2Add water to be modulated into the sodium silicate solution of 1.0-2.0mol/L, stirs 30min, obtain To sodium silicate solution；
2) metabisulfite solution that mass fraction is 1.4%-2.0%, is prepared, stirring 30 minutes spare；
3) sulfuric acid solution for, preparing 1.0-1.5mol/L is spare；
4), sodium hexametaphosphate dispersant is dissolved with water, then calgon dissolution is added to the silicic acid in step 1) Stirred in sodium solution 30 minutes it is spare, the quality of sodium hexametaphosphate dispersant accounts for the 0.01%-0.1% of sodium silicate solution quality；
5) 5-8m, is added into reaction kettle3Step 2 made from metabisulfite solution, be heated to 60 DEG C, low whipping speed is 5-10m is added under conditions of 20Hz3The resulting solution of step 4), after ten minutes, mixing speed increases to 50Hz, with 3- for stirring 4m3The speed of/h is added sulfuric acid solution and is reacted, and stops acid adding when pH value reaches 8.5, is warming up to 85-95 DEG C；
6) under conditions of, low whipping speed is 30Hz, with 11-13m3Sodium silicate solution and sulfuric acid solution is added in the speed of/h Equivalent acid-base neutralization reaction is carried out, keeping the pH value of reaction solution is 8.5, stop being added after sodium silicate solution addition, Again with 3-4m3The speed of/h adds sulfuric acid solution, when pH value reaches 4-5, stops addition, continues stirring 10 minutes；
7) silica of formation, is subjected to pressure filtration washing, when the salt content of washing water≤2%, passes through spray drying The silica that partial size is 4-6 μm is crushed to air-flow crusher afterwards.
Preferably, the sodium metasilicate Na2O·nSiO2In, the range of n is 3.3-3.45.
Preferably, the sulfuric acid solution concentration prepared in step 3 is 1.25mol/L.
Preferably, the mass fraction for the metabisulfite solution prepared in step 2 is 1.7%.
Preferably, in step 5, the rate of addition of sulfuric acid solution is 3.5m3/h。
Preferably, in step 4, sodium hexametaphosphate dispersant, which is dissolved sodium hexametaphosphate solution concentration obtained, with water is 60wt%.
Preferably, in step 4, the quality of sodium hexametaphosphate dispersant accounts for the 0.05% of sodium silicate solution quality.
Preferably, step 6 specifically: with 12m3It is 5-8m that volume, which is added, in the speed of/h3Sodium silicate solution and sulfuric acid solution into Row equivalent acid-base neutralization reaction, keeping the pH value of reaction solution is 8.5, stops being added after sodium silicate solution addition, then With 3.5m3The speed of/h adds sulfuric acid solution, when pH value reaches 4.5, stops addition, continues stirring 10 minutes.
Preferably, the specific steps of step 7 are as follows: the silica of formation is subjected to pressure filtration washing, when washing water conductivity ≤ 19000 μ s are 4-6 μm by being crushed to partial size with air-flow crusher after spray drying.
Compared with prior art, present invention has an advantage that
(1) preparation method of high dispersive silica of the present invention is simple, and process stabilizing, condition is controllable, and production cost is low, ring Border pollution is few, can industrialized production, can effectively improve silica in water with the dispersibility in nonpolar solvent.
(2) high dispersive silica of the present invention is high with the dispersibility in nonpolar solvent (such as n-hexane) in water, partial size At 4-7 μm, oil factor is 150~200ml/100g, apparent density≤0.2g/mL, specific surface area 300-450 ㎡/g, and pH value exists 6.5-8.5, dioxide-containing silica >=99%.
High dispersive silica of the present invention can be applied to daily use chemicals industry and do supporting surfactant or be applied to medical row Industry does dispersing agent.
Specific embodiment
Below with reference to preparation method of some specific embodiments to Aerosil 200 of the present invention do into The description of one step.Specific embodiment is that present invention be described in more detail, non-limiting protection scope of the present invention.
Feature used in the present invention is all from commercially available.
Embodiment 1
Silica is prepared according to the following steps:
1), by sodium metasilicate Na2O·nSiO2Add water to be modulated into the sodium silicate solution of 1.0mol/L, stirs 30min, obtain silicon Acid sodium solution；
2) metabisulfite solution that mass fraction is 1.4%, is prepared, stirring 30 minutes spare；
3) sulfuric acid solution for, preparing 1.0mol/L is spare；
4), sodium hexametaphosphate dispersant is dissolved with water, the sodium hexametaphosphate solution that concentration is 60wt% is made, then by six Sodium metaphosphate dissolution, which is added, stirs 30 minutes spare, quality of sodium hexametaphosphate dispersant into the sodium silicate solution in step 1) Account for the 0.01% of sodium silicate solution quality；
5) 5m, is added into reaction kettle3Step 2 made from concentration be 1.4% metabisulfite solution, be heated to 60 DEG C, 5m is added under conditions of being 20Hz in low whipping speed3The resulting solution of step 4), after ten minutes, mixing speed increases to for stirring 50Hz, with 3m3The speed of/h is added sulfuric acid solution and is reacted, and stops acid adding when pH value reaches 8.5, is warming up to 85 DEG C；
6) under conditions of, low whipping speed is 30Hz, with 11m3The speed of/h be added sodium silicate solution and sulfuric acid solution into Row equivalent acid-base neutralization reaction, keeping the pH value of reaction solution is 8.5, stops being added after sodium silicate solution addition, then With 3.5m3The speed of/h adds sulfuric acid solution, when pH value reaches 4, stops addition, continues stirring 10 minutes；
7) silica of formation, is subjected to pressure filtration washing, when the salt content of washing water is equal to 2%, by doing by spraying The silica that partial size is 4-6 μm is crushed to air-flow crusher after dry.
Embodiment 2
Silica is prepared according to the following steps:
1), by sodium metasilicate Na2O·nSiO2Add water to be modulated into the sodium silicate solution of 2.0mol/L, stirs 30min, obtain silicon Acid sodium solution；
2) metabisulfite solution that mass fraction is 2.0%, is prepared, stirring 30 minutes spare；
3) sulfuric acid solution for, preparing 1.5mol/L is spare；
4), sodium hexametaphosphate dispersant is dissolved with water, the sodium hexametaphosphate solution that concentration is 60wt% is made, then by six Sodium metaphosphate dissolution, which is added, stirs 30 minutes spare, quality of sodium hexametaphosphate dispersant into the sodium silicate solution in step 1) Account for the 0.1% of sodium silicate solution quality；
5) 8m, is added into reaction kettle3Step 2 made from concentration be 1.5% metabisulfite solution, be heated to 60 DEG C, 10m is added under conditions of being 20Hz in low whipping speed3The resulting solution of step 4), after ten minutes, mixing speed increases to for stirring 50Hz, with 4m3The speed of/h is added sulfuric acid solution and is reacted, and stops acid adding when pH value reaches 8.5, is warming up to 95 DEG C；
6) under conditions of, low whipping speed is 30Hz, with 13m3The speed of/h be added sodium silicate solution and sulfuric acid solution into Row equivalent acid-base neutralization reaction, keeping the pH value of reaction solution is 8.5, stops being added after sodium silicate solution addition, then With 4m3The speed of/h adds sulfuric acid solution, when pH value reaches 5, stops addition, continues stirring 10 minutes；
7) silica of formation, is subjected to pressure filtration washing, when the salt content of washing water is equal to 2%, by doing by spraying The silica that partial size is 4-6 μm is crushed to air-flow crusher after dry.
Embodiment 3
Silica is prepared according to the following steps:
1), by sodium metasilicate Na2O·nSiO2Add water to be modulated into the sodium silicate solution of 1.5mol/L, stirs 30min, obtain silicon Acid sodium solution；
2) metabisulfite solution that mass fraction is 1.7%, is prepared, stirring 30 minutes spare；
3) sulfuric acid solution for, preparing 1.25mol/L is spare；
4), sodium hexametaphosphate dispersant is dissolved with water, the sodium hexametaphosphate solution that concentration is 60wt% is made, then by six Sodium metaphosphate dissolution, which is added, stirs 30 minutes spare, quality of sodium hexametaphosphate dispersant into the sodium silicate solution in step 1) Account for the 0.05% of sodium silicate solution quality；
5) 6.5m, is added into reaction kettle3Concentration be 1.25% metabisulfite solution, be heated to 60 DEG C, stirring speed 8m is added under conditions of being 20Hz in degree3The resulting solution of step 4), after ten minutes, mixing speed increases to 50Hz for stirring, with 3.5m3The speed of/h is added sulfuric acid solution and is reacted, and stops acid adding when pH value reaches 8.5, is warming up to 90 DEG C；
6) under conditions of, low whipping speed is 30Hz, with 12m3The speed of/h be added sodium silicate solution and sulfuric acid solution into Row equivalent acid-base neutralization reaction, keeping the pH value of reaction solution is 8.5, stops being added after sodium silicate solution addition, then With 3.5m3The speed of/h adds sulfuric acid solution, when pH value reaches 4.5, stops addition, continues stirring 10 minutes；
7) silica of formation, is subjected to pressure filtration washing, when washing water conductivity≤19000 μ s, by doing by spraying The silica that partial size is 4-6 μm is crushed to air-flow crusher after dry.
Embodiment 4
Silica is prepared according to the following steps:
1), by sodium metasilicate Na2O·nSiO2Add water to be modulated into the sodium silicate solution of 1.5mol/L, stirs 30min, obtain silicon Acid sodium solution；
2) metabisulfite solution that mass fraction is 1.5%, is prepared, stirring 30 minutes spare；
3) sulfuric acid solution for, preparing 1.25mol/L is spare；
4), sodium hexametaphosphate dispersant is dissolved with water, the sodium hexametaphosphate solution that concentration is 60wt% is made, then by six Sodium metaphosphate dissolution, which is added, stirs 30 minutes spare, quality of sodium hexametaphosphate dispersant into the sodium silicate solution in step 1) Account for the 0.05% of sodium silicate solution quality；
5) 8m, is added into reaction kettle3Concentration be 1.5% metabisulfite solution, be heated to 60 DEG C, low whipping speed is 8m is added under conditions of 20Hz3The resulting solution of step 4), after ten minutes, mixing speed increases to 50Hz, with 3.5m for stirring3/h Speed be added sulfuric acid solution reacted, when pH value reach 8.5 when stop acid adding, be warming up to 90 DEG C；
6) under conditions of, low whipping speed is 30Hz, with 12m3The speed of/h be added sodium silicate solution and sulfuric acid solution into Row equivalent acid-base neutralization reaction, keeping the pH value of reaction solution is 8.5, stops being added after sodium silicate solution addition, then With 3.5m3The speed of/h adds sulfuric acid solution, when pH value reaches 4.5, stops addition, continues stirring 10 minutes；
7) silica of formation, is subjected to pressure filtration washing, when washing water conductivity≤19000 μ s, by doing by spraying The silica that partial size is 4-6 μm is crushed to air-flow crusher after dry.
Embodiment 5
Silica is prepared according to the following steps:
1), by sodium metasilicate Na2O·nSiO2Add water to be modulated into the sodium silicate solution of 1.5mol/L, stirs 30min, obtain silicon Acid sodium solution；
2) metabisulfite solution that mass fraction is 1.5%, is prepared, stirring 30 minutes spare；
3) sulfuric acid solution for, preparing 1.25mol/L is spare；
4), sodium hexametaphosphate dispersant is dissolved with water, the sodium hexametaphosphate solution that concentration is 60wt% is made, then by six Sodium metaphosphate dissolution, which is added, stirs 30 minutes spare, quality of sodium hexametaphosphate dispersant into the sodium silicate solution in step 1) Account for the 0.05% of sodium silicate solution quality；
5) 8m, is added into reaction kettle3Concentration be 1.5% metabisulfite solution, be heated to 60 DEG C, low whipping speed is 10m is added under conditions of 20Hz3The resulting solution of step 4), after ten minutes, mixing speed increases to 50Hz, with 3.5m for stirring3/h Speed be added sulfuric acid solution reacted, when pH value reach 8.5 when stop acid adding, be warming up to 90 DEG C；
6) under conditions of, low whipping speed is 30Hz, with 12m3The speed of/h be added sodium silicate solution and sulfuric acid solution into Row equivalent acid-base neutralization reaction, keeping the pH value of reaction solution is 8.5, stops being added after sodium silicate solution addition, then With 3.5m3The speed of/h adds sulfuric acid solution, when pH value reaches 4.5, stops addition, continues stirring 10 minutes；
7) silica of formation, is subjected to pressure filtration washing, when washing water conductivity≤19000 μ s, by doing by spraying The silica that partial size is 4-6 μm is crushed to air-flow crusher after dry.
Comparative example 1
Silica is prepared according to the following steps:
1), by sodium metasilicate Na2O·nSiO2Add water to be modulated into the sodium silicate solution of 1.5mol/L, stirs 30min, obtain silicon Acid sodium solution；
2) metabisulfite solution that mass fraction is 1.5%, is prepared, stirring 30 minutes spare；
3) sulfuric acid solution for, preparing 1.25mol/L is spare；
4) 8m, is added into reaction kettle3Step 2 made from concentration be 1.4% metabisulfite solution, be heated to 60 DEG C, 8m is added under conditions of being 20Hz in low whipping speed3The resulting solution of step 1), after ten minutes, mixing speed increases to for stirring 50Hz, with 3.5m3The speed of/h is added sulfuric acid solution and is reacted, and stops acid adding when pH value reaches 8.5, is warming up to 90 DEG C；
5) under conditions of, low whipping speed is 30Hz, with 12m3The speed of/h be added sodium silicate solution and sulfuric acid solution into Row equivalent acid-base neutralization reaction, keeping the pH value of reaction solution is 8.5, stops being added after sodium silicate solution addition, then With 3.5m3The speed of/h adds sulfuric acid solution, when pH value reaches 4.5, stops addition, continues stirring 10 minutes；
6) silica of formation, is subjected to pressure filtration washing, as the conductivity of washing water≤19000 μ s, by spraying The silica that partial size is 4-6 μm is crushed to air-flow crusher after drying.
Comparative example 2
Silica is prepared according to the following steps:
1), by sodium metasilicate Na2O·nSiO2Add water to be modulated into the sodium silicate solution of 1.5mol/L, stirs 30min, obtain silicon Acid sodium solution；
2) metabisulfite solution that mass fraction is 1.5%, is prepared, stirring 30 minutes spare；
3) sulfuric acid solution for, preparing 1.25mol/L is spare；
4), sodium hexametaphosphate dispersant is dissolved with water, the sodium hexametaphosphate solution that concentration is 60wt% is made, then by six Sodium metaphosphate dissolution, which is added, stirs 30 minutes spare, quality of sodium hexametaphosphate dispersant into the sodium silicate solution in step 1) Account for the 0.2% of sodium silicate solution quality；
5) 8m, is added into reaction kettle3Step 2 made from concentration be 1.5% metabisulfite solution, be heated to 60 DEG C, 8m is added under conditions of being 20Hz in low whipping speed3The resulting solution of step 4), after ten minutes, mixing speed increases to for stirring 50Hz, with 3.5m3The speed of/h is added sulfuric acid solution and is reacted, and stops acid adding when pH value reaches 8.5, is warming up to 90 DEG C；
6) under conditions of, low whipping speed is 30Hz, with 12m3The speed of/h be added sodium silicate solution and sulfuric acid solution into Row equivalent acid-base neutralization reaction, keeping the pH value of reaction solution is 8.5, stops being added after sodium silicate solution addition, then With 3.5m3The speed of/h adds sulfuric acid solution, when pH value reaches 4.5, stops addition, continues stirring 10 minutes；
7) silica of formation, is subjected to pressure filtration washing, as the conductivity of washing water≤19000 μ s, by spraying The silica that partial size is 4-6 μm is crushed to air-flow crusher after drying.
Comparative example 3
Silica is prepared according to the following steps:
1), by sodium metasilicate Na2O·nSiO2Add water to be modulated into the sodium silicate solution of 1.5mol/L, stirs 30min, obtain silicon Acid sodium solution；
2) metabisulfite solution that mass fraction is 1.5%, is prepared, stirring 30 minutes spare；
3) sulfuric acid solution for, preparing 1.25mol/L is spare；
4), sodium hexametaphosphate dispersant is dissolved with water, the sodium hexametaphosphate solution that concentration is 60wt% is made, then by six Sodium metaphosphate dissolution, which is added, stirs 30 minutes spare, quality of sodium hexametaphosphate dispersant into the sodium silicate solution in step 1) Account for the 0.005% of sodium silicate solution quality；
5) 8m, is added into reaction kettle3Concentration be 1.5% metabisulfite solution, be heated to 60 DEG C, low whipping speed is 8m is added under conditions of 20Hz3The resulting solution of step 4), after ten minutes, mixing speed increases to 50Hz, with 3.5m for stirring3/h Speed be added sulfuric acid solution reacted, when pH value reach 8.5 when stop acid adding, be warming up to 90 DEG C；
6) under conditions of, low whipping speed is 30Hz, with 12m3The speed of/h be added sodium silicate solution and sulfuric acid solution into Row equivalent acid-base neutralization reaction, keeping the pH value of reaction solution is 8.5, stops being added after sodium silicate solution addition, then With 3.5m3The speed of/h adds sulfuric acid solution, when pH value reaches 4.5, stops addition, continues stirring 10 minutes；
7) silica of formation, is subjected to pressure filtration washing, when washing water conductivity≤19000 μ s, by doing by spraying The silica that partial size is 4-6 μm is crushed to air-flow crusher after dry.
Comparative example 4
Silica is prepared according to the following steps:
1), by sodium metasilicate Na2O·nSiO2Add water to be modulated into the sodium silicate solution of 1.5mol/L, stirs 30min, obtain silicon Acid sodium solution；
2) metabisulfite solution that mass fraction is 1.5%, is prepared, stirring 30 minutes spare；
3) sulfuric acid solution for, preparing 1.25mol/L is spare；
4), sodium hexametaphosphate dispersant is dissolved with water, the sodium hexametaphosphate solution that concentration is 60wt% is made, then by six Sodium metaphosphate dissolution, which is added, stirs 30 minutes spare, quality of sodium hexametaphosphate dispersant into the sodium silicate solution in step 1) Account for the 0.05% of sodium silicate solution quality；
5) 8m, is added into reaction kettle3Concentration be 1.5% metabisulfite solution, be heated to 60 DEG C, low whipping speed is 12m is added under conditions of 20Hz3The resulting solution of step 4), after ten minutes, mixing speed increases to 50Hz, with 3.5m for stirring3/h Speed be added sulfuric acid solution reacted, when pH value reach 8.5 when stop acid adding, be warming up to 90 DEG C；
6) under conditions of, low whipping speed is 30Hz, with 12m3The speed of/h be added sodium silicate solution and sulfuric acid solution into Row equivalent acid-base neutralization reaction, keeping the pH value of reaction solution is 8.5, stops being added after sodium silicate solution addition, then With 3.5m3The speed of/h adds sulfuric acid solution, when pH value reaches 4.5, stops addition, continues stirring 10 minutes；
7) silica of formation, is subjected to pressure filtration washing, when washing water conductivity≤19000 μ s, by doing by spraying The silica that partial size is 4-6 μm is crushed to air-flow crusher after dry.
Comparative example 5
Silica is prepared according to the following steps:
1), by sodium metasilicate Na2O·nSiO2Add water to be modulated into the sodium silicate solution of 1.5mol/L, stirs 30min, obtain silicon Acid sodium solution；
2) metabisulfite solution that mass fraction is 1.5%, is prepared, stirring 30 minutes spare；
3) sulfuric acid solution for, preparing 1.25mol/L is spare；
4), sodium hexametaphosphate dispersant is dissolved with water, the sodium hexametaphosphate solution that concentration is 60wt% is made, then by six Sodium metaphosphate dissolution, which is added, stirs 30 minutes spare, quality of sodium hexametaphosphate dispersant into the sodium silicate solution in step 1) Account for the 0.05% of sodium silicate solution quality；
5) 8m, is added into reaction kettle3Concentration be 1.5% metabisulfite solution, be heated to 60 DEG C, low whipping speed is 12m is added under conditions of 20Hz3The resulting solution of step 4), after ten minutes, mixing speed increases to 50Hz, with 4.5m for stirring3/h Speed be added sulfuric acid solution reacted, when pH value reach 8.5 when stop acid adding, be warming up to 90 DEG C；
6) under conditions of, low whipping speed is 30Hz, with 12m3The speed of/h be added sodium silicate solution and sulfuric acid solution into Row equivalent acid-base neutralization reaction, keeping the pH value of reaction solution is 8.5, stops being added after sodium silicate solution addition, then With 3.5m3The speed of/h adds sulfuric acid solution, when pH value reaches 4.5, stops addition, continues stirring 10 minutes；
7) silica of formation, is subjected to pressure filtration washing, when washing water conductivity≤19000 μ s, by doing by spraying The silica that partial size is 4-6 μm is crushed to air-flow crusher after dry.
Comparative example 6
1), by sodium metasilicate Na2O·nSiO2Add water to be modulated into the sodium silicate solution of 1.5mol/L, stirs 30min, obtain silicon Acid sodium solution；
2) metabisulfite solution that mass fraction is 1.5%, is prepared, stirring 30 minutes spare；
3) sulfuric acid solution for, preparing 1.25mol/L is spare；
4), sodium hexametaphosphate dispersant is dissolved with water, the sodium hexametaphosphate solution that concentration is 60wt% is made, then by six Sodium metaphosphate dissolution, which is added, stirs 30 minutes spare, quality of sodium hexametaphosphate dispersant into the sodium silicate solution in step 1) Account for the 0.05% of sodium silicate solution quality；
5) 8m, is added into reaction kettle3Concentration be 1.5% metabisulfite solution, be heated to 60 DEG C, low whipping speed is 12m is added under conditions of 20Hz3The resulting solution of step 4), after ten minutes, mixing speed increases to 30Hz, with 4.5m for stirring3/h Speed be added sulfuric acid solution reacted, when pH value reach 8.5 when stop acid adding, be warming up to 90 DEG C；
6) under conditions of, low whipping speed is 30Hz, with 12m3The speed of/h be added sodium silicate solution and sulfuric acid solution into Row equivalent acid-base neutralization reaction, keeping the pH value of reaction solution is 8.5, stops being added after sodium silicate solution addition, then With 3.5m3The speed of/h adds sulfuric acid solution, when pH value reaches 4.5, stops addition, continues stirring 10 minutes；
7) silica of formation, is subjected to pressure filtration washing, when washing water conductivity≤19000 μ s, by doing by spraying The silica that partial size is 4-6 μm is crushed to air-flow crusher after dry.
Comparative example 7
1), by sodium metasilicate Na2O·nSiO2Add water to be modulated into the sodium silicate solution of 1.5mol/L, stirs 30min, obtain silicon Acid sodium solution；
2) metabisulfite solution that mass fraction is 1.5%, is prepared, stirring 30 minutes spare；
3) sulfuric acid solution for, preparing 1.25mol/L is spare；
4), sodium hexametaphosphate dispersant is dissolved with water, the sodium hexametaphosphate solution that concentration is 60wt% is made, then by six Sodium metaphosphate dissolution, which is added, stirs 30 minutes spare, quality of sodium hexametaphosphate dispersant into the sodium silicate solution in step 1) Account for the 0.05% of sodium silicate solution quality；
5) 8m, is added into reaction kettle3Concentration be 1.5% metabisulfite solution, be heated to 60 DEG C, low whipping speed is 12m is added under conditions of 20Hz3The resulting solution of step 4), after ten minutes, mixing speed increases to 50Hz, with 4.5m for stirring3/h Speed be added sulfuric acid solution reacted, when pH value reach 8.5 when stop acid adding, be warming up to 90 DEG C；
6) under conditions of, low whipping speed is 30Hz, with 13m3The speed of/h be added sodium silicate solution and sulfuric acid solution into Row equivalent acid-base neutralization reaction, keeping the pH value of reaction solution is 8.5, stops being added after sodium silicate solution addition, then With 3.5m3The speed of/h adds sulfuric acid solution, when pH value reaches 4.5, stops addition, continues stirring 10 minutes；
7) silica of formation, is subjected to pressure filtration washing, when washing water conductivity≤19000 μ s, by doing by spraying The silica that partial size is 4-6 μm is crushed to air-flow crusher after dry.
Embodiment 1-5 and silica made from comparative example 1-7 are tested for the property, test method is as follows:
Particle diameter distribution (D50)): laser diffractometry, (instrument BT-9300ST, Dandong Bai Te Instrument Ltd.)
Specific surface area: BET multiple spot specific surface area, test method are static nitrogen adsorption methods, using standard GB.T 19587- 2004 method is detected；Used instrument is the classic specific surface of JW-BK200B and Porosimetry.(Beijing is precise and tiny Gao Bo's science and technology Co., Ltd)
Oil factor test: Q/BT 2346-2015.
Apparent density: Q/BT 2346-2015.
PH value: Q/BT 2346-2015.
Dioxide-containing silica: Q/BT 2346-2015.
Dispersibility: laboratory method applies additive amount for nonpolar solvent (n-hexane) according to silica in industry 2.5%, investigate silica sample whether can be uniformly dispersed soilless sticking.
Embodiment 1-5 and the performance test results of comparative example 1-7 are listed in the following table.
Silica performance test table
The dosage of dispersing agent is increased in comparative example 2, although improving the dispersibility of silica, is increased into This, is unfavorable for industrialization.
From the foregoing, it will be observed that the dispersibility of silica made from method of the present invention is high, comprehensive performance is significantly higher than comparison Example is applicable in and is applied in excipient substance, is also applied for industrial production.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks Domain is included within the scope of the present invention.

Claims (9)

1. a kind of preparation method of high dispersive silica, step include:
1), by sodium metasilicate Na2O·nSiO2Add water to be modulated into the sodium silicate solution of 1.0-2.0mol/L, stirs 30min, obtain silicon Acid sodium solution；
2) metabisulfite solution that mass fraction is 1.4%-2.0%, is prepared, stirring 30 minutes spare；
3) sulfuric acid solution for, preparing 1.0-1.5mol/L is spare；
4), sodium hexametaphosphate dispersant is dissolved with water, then calgon dissolution addition is molten to the sodium metasilicate in step 1) Stirred in liquid 30 minutes it is spare, the quality of sodium hexametaphosphate dispersant accounts for the 0.01%-0.1% of sodium silicate solution quality；
5) 5-8m, is added into reaction kettle3Step 2 made from metabisulfite solution, be heated to 60 DEG C, low whipping speed 20Hz Under conditions of 5-10m is added3The resulting solution of step 4), after ten minutes, mixing speed increases to 50Hz, with 3-4m for stirring3/ h's Speed is added sulfuric acid solution and is reacted, and stops acid adding when pH value reaches 8.5, is warming up to 85-95 DEG C；
6) under conditions of, low whipping speed is 30Hz, with 11-13m3Sodium silicate solution is added in the speed of/h and sulfuric acid solution carries out Equivalent acid-base neutralization reaction, keeping the pH value of reaction solution is 8.5, stops being added after sodium silicate solution addition, then with 3-4m3The speed of/h adds sulfuric acid solution, when pH value reaches 4-5, stops addition, continues stirring 10 minutes；
7) silica of formation, is subjected to pressure filtration washing, as conductivity≤19000 μ s of washing water, after spray drying The silica that partial size is 4-6 μm is crushed to air-flow crusher.
2. the preparation method of high dispersive silica as described in claim 1, it is characterised in that:
The sodium metasilicate Na2O·nSiO2In, the range of n is 3.3-3.45.
3. the preparation method of high dispersive silica as claimed in claim 2, it is characterised in that:
The mass fraction for the metabisulfite solution prepared in step 2 is 1.7%.
4. the preparation method of high dispersive silica as claimed in claim 3, it is characterised in that:
The sulfuric acid solution concentration prepared in step 3 is 1.25mol/L.
5. the preparation method of high dispersive silica as claimed in claim 4, it is characterised in that:
In step 5, the rate of addition of sulfuric acid solution is 3.5m3/h。
6. the preparation method of high dispersive silica as claimed in claim 5, it is characterised in that:
In step 4, it is 60wt% that sodium hexametaphosphate dispersant, which is dissolved sodium hexametaphosphate solution concentration obtained, with water.
7. the preparation method of high dispersive silica as claimed in claim 6, it is characterised in that:
In step 4, the quality of sodium hexametaphosphate dispersant accounts for the 0.05% of sodium silicate solution quality.
8. the preparation method of high dispersive silica as claimed in claim 7, it is characterised in that:
Step 6 specifically: with 12m3It is 5-8m that volume, which is added, in the speed of/h3Sodium silicate solution and sulfuric acid solution carry out equivalent acid Alkali neutralization reaction, keeping the pH value of reaction solution is 8.5, stops being added after sodium silicate solution addition, then with 3.5m3/ h's Speed adds sulfuric acid solution, when pH value reaches 4.5, stops addition, continues stirring 10 minutes.
9. the preparation method of high dispersive silica as claimed in claim 8, it is characterised in that:
The specific steps of step 7 are as follows: the silica of formation is subjected to pressure filtration washing, as washing water conductivity≤19000 μ s, is led to Crossing and being crushed to partial size with air-flow crusher after being spray-dried is 4-6 μm.
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CN108840342B (en) * 2018-07-24 2019-04-30 广州市飞雪材料科技有限公司 A kind of Silica Using for Toothpaste and preparation method thereof having anti-microbial property
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1286648B1 (en) * 2000-06-07 2005-10-05 Rhodia Chimie Use of a high structure and dispersible precipitated silica as thickening or texturing agent in toothpaste compositions
CN103449458A (en) * 2013-08-21 2013-12-18 安徽确成硅化学有限公司 Preparation method of high-dispersivity white carbon black
CN105236429A (en) * 2015-09-14 2016-01-13 安徽确成硅化学有限公司 Ultrahighly-dispersed white carbon black preparation method
CN106276929A (en) * 2016-07-29 2017-01-04 广州市飞雪材料科技有限公司 A kind of preparation method of the type silicon dioxide that rubs

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1286648B1 (en) * 2000-06-07 2005-10-05 Rhodia Chimie Use of a high structure and dispersible precipitated silica as thickening or texturing agent in toothpaste compositions
CN103449458A (en) * 2013-08-21 2013-12-18 安徽确成硅化学有限公司 Preparation method of high-dispersivity white carbon black
CN105236429A (en) * 2015-09-14 2016-01-13 安徽确成硅化学有限公司 Ultrahighly-dispersed white carbon black preparation method
CN106276929A (en) * 2016-07-29 2017-01-04 广州市飞雪材料科技有限公司 A kind of preparation method of the type silicon dioxide that rubs

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