CN106009782A - Surface modified silicon dioxide particle preparation method - Google Patents
Surface modified silicon dioxide particle preparation method Download PDFInfo
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- CN106009782A CN106009782A CN201610338885.5A CN201610338885A CN106009782A CN 106009782 A CN106009782 A CN 106009782A CN 201610338885 A CN201610338885 A CN 201610338885A CN 106009782 A CN106009782 A CN 106009782A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/3072—Treatment with macro-molecular organic compounds
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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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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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Abstract
The invention belongs to the technical field of silicon dioxide and particularly relates to a surface modified silicon dioxide particle preparation method. The preparation method includes: S1, preparing a cationic polyacrylamide solution; S2, injecting a sodium bicarbonate solution and the cationic polyacrylamide solution into a reaction tank, controlling a stirring speed, dropwise adding a sodium silicate solution into the reaction tank at a normal temperature, adding a food-grade pigment solution when the sodium silicate solution is half added, and after the sodium silicate solution is completely added, stirring until a material system is converted into gel; S3, adding dilute sulfuric acid, and stopping adding the acid when a final pH value of the system is controlled to be 4-5; S4, subjecting silicon dioxide gel to filter pressing, washing, drying and grinding to obtain silicon dioxide particles. The surface modified silicon dioxide particle preparation method is simple, low in cost and low in pollution, and the silicon dioxide particles prepared according ot the method is low in density and long in suspension time.
Description
Technical field
The invention belongs to silicon dioxide technical field, be specifically related to the preparation method of a kind of surface modified silicon dioxide particle.
Background technology
Along with progress and the raising of people's material life of society, the consumption idea of people changes, and consumer is to product
Require more diversification, do not require nothing more than product quality high efficiency, also require that it has certain attractive in appearance.Silicon dioxide colour particles
Rate of dyeing is high, and coloring stabilized, nontoxic pollution-free, chemical and physical properties is stable, is the important interpolation of the household chemicalss such as toothpaste
Agent.The different color of product and outward appearance can be given by adding the silicon dioxide granule of different colours, strengthen the ornamental value of product.
Further, since it has certain hardness, possessing good clean-up performance, it surface activity in household chemicals such as with toothpaste
Agent can play synergism, so being widely used.
At present, above market, universal silicon dioxide granule density used is higher, and the suspension effect in the middle of solution is poor, causes it
In the household chemicals production processes such as toothpaste, it is susceptible to the phenomenon of sedimentation, causes the skewness of particle in the middle of system,
Instability in the mastic system of finished product.Chinese patent application CN 105016345A discloses a kind of colored dioxy of toothpaste suspension
The preparation method of SiClx particle, comprises the following steps: (1) adds dilute sulfuric acid in retort and stirs, and is simultaneously introduced PEG
And sodium dodecyl sulfate aqueous solution；(2) in retort, add water glass solution, be neutralized reaction while stirring, work as thing
When the pH value of material system reaches 3.0～4.0, adding food grade colorant solution, the pH value controlling reaction end is 4.0～5.0；
(3) continue to add dilute sulfuric acid in retort, add water glass solution after stirring, react while stirring to material system
Stop adding water glass solution after changing into gel, obtain gel；(4) gel is carried out filter pressing, obtain gel press cake, washing
Gel press cake, removes sulfate and the PEG of residual, is dried gel press cake, pulverizes, obtain silicon dioxide granule.Should
The silicon dioxide granule that invention is prepared has certain degree of hardness and relative density less, is 0.25～0.40g/ml, molten in toothpaste modulation
In liquid system, suspension time is 30～32min.But the suspension time of this invention silicon dioxide is the most undesirable, use two-step method anti-
Should, complex process；And using PEG and dodecyl sodium sulfate as modifying agent, consumption is big, and cost of material is high；Reaction
One of raw material is sulphuric acid, and consumption is big, not only easy corrosion reaction equipment, and can produce a large amount of sulfate, big for environment pollution.
To sum up, it is necessary to research and develop the preparation method of a kind of silicon dioxide granule, its technique is simple, and low cost is low in the pollution of the environment,
The silicon dioxide granule simultaneously prepared has certain hardness, and density is little and suspension time is long.
Summary of the invention
(as big compared with short, complex process, equipment corrosion, environmental pollution in suspension time in order to solve problems of the prior art
Deng), the invention provides the preparation method of a kind of surface modified silicon dioxide particle, it utilizes PAMC to two
Silicon oxide particle carries out surface modification, and prepared silicon dioxide granule density is little, is 0.20～0.30g/ml, at toothpaste solution body
In system, suspension time is up to 50～60min；And reactions steps is simple, sulfuric acid dosage greatly reduces, low in the pollution of the environment, produces into
This is low.
The preparation method of surface modified silicon dioxide particle that the present invention provides, specifically includes following steps:
S1, by fully dispersed for PAMC in aqueous, obtain PAMC solution；
S2, past retort inject sodium bicarbonate solution 4.5～5.5m3, it is subsequently adding PAMC solution 0.4～0.5m3,
Controlling mixing speed is 30～35hz, and stir-activating 10～15min is past according to the speed of 1500～2000L/h the most at normal temperatures
Retort drips water glass solution 4.8～5.8m3, when water glass solution dripping quantity reaches 2.0～3.0m3Time, add in retort
Food grade colorant solution, after water glass solution dropping, continues stirring until material system changes into gel；
S3, continuation add dilute sulfuric acid in retort, stir, and the endpoint pH of control system stops acid adding when being 4～5；
S4, the silica dioxide gel of formation is carried out filter pressing, wash gel press cake with water, to the silicon dioxide pigment after washing
Gel is dried, pulverizes, and prepares silicon dioxide granule.
Preferably, the mass concentration of described PAMC solution is 0.2～1.0%.
Preferably, the concentration of described sodium bicarbonate solution is 0.4～0.8M.
Preferably, the modulus of described water glass solution be 3.3, concentration be 0.4～0.8M.
Preferably, described food grade colorant solution is the sorbitol of food stage, glycerol or polyglycol solution, and its interpolation weight is
The 0.1～0.5% of sodium bicarbonate solution weight.
Preferably, the concentration of described dilute sulfuric acid is 0.5～1.0M.
In technical solution of the present invention, use waterglass and sodium bicarbonate as reaction raw materials, using PAMC as
Surface modifier, using food grade colorant as stain, controls mixing speed and the rate of addition of water glass solution, generates gel,
Again by the pH value of dropping dilute sulfuric acid regulation and control reaction end, after through filter pressing, wash, be dried, broken prepared have low-density,
The silicon dioxide colour particles of higher suspension performance.
Sodium bicarbonate and waterglass react, before sodium bicarbonate and waterglass react precipitation gel, in course of reaction constantly
Producing carbon dioxide, carbon dioxide has reaming effect, makes the silicon dioxide volume prepared loosen, and relative density is little；
And when adding dilute sulfuric acid regulation and control pH value after separating out gel, unnecessary sodium bicarbonate continues to react with dilute sulfuric acid, separate out substantial amounts of
Carbon dioxide so that silicon dioxide volume expands, and structure is more loose.It addition, add a small amount of cation polypropylene acyl
Amine is as surface modifier, and during silicon dioxide generates, PAMC enters partly into the inside of silicon dioxide
Structure, partial adsorbates, on the surface of silicon dioxide, is effectively combined with silicon dioxide granule so that silicon dioxide granule is with positive electricity
Lotus, and due to charge repulsion principle, silicon dioxide granule is extended further at the suspension time of solution system, reaches
50～60min.
Therefore, compared with prior art, present invention have an advantage that
(1) preparation method of surface modified silicon dioxide particle of the present invention use waterglass and sodium bicarbonate as reaction raw materials,
Dilute sulfuric acid drop reaction terminal, not only simplify production technology, and greatly reduces the consumption of sulphuric acid, so that sulfate
Discharge capacity reduces, and reduces environmental pollution, more environmentally-friendly.
(2) preparation method of surface modified silicon dioxide particle of the present invention utilizes PAMC to silicon dioxide granule
Carry out surface modification, in conjunction with waterglass and the reaction of sodium bicarbonate, control mixing speed and the rate of addition of water glass solution, system
Silicon dioxide granule density little, be 0.20～0.30g/ml, in toothpaste solution system, suspension time is up to 50～60min.
(3) the inventive method is simple, and process stabilizing, production cost is low, low in the pollution of the environment, can industrialized production；Prepare
Silicon dioxide granule has certain hardness and higher suspension performance, and density is little, can be widely applied in the household chemicalss such as toothpaste.
Detailed description of the invention
Describing the present invention in detail below in conjunction with specific embodiment, illustrative examples and explanation in this present invention are used for solving
Release the present invention, but not as a limitation of the invention.
Embodiment 1, the preparation method of surface modified silicon dioxide particle of the present invention
S1, by fully dispersed for PAMC in aqueous, obtain the cation polypropylene that mass concentration is 0.2%
Amide solution；
S2, past retort implantation concentration are the sodium bicarbonate solution 4.5m of 0.4M3, it is subsequently adding PAMC molten
Liquid 0.4m3, control mixing speed is 30hz, stir-activating 10min, past anti-according to the speed of 1500L/h the most at normal temperatures
Answer tank drips modulus be 3.3, concentration be the water glass solution 4.8m of 0.4M3, when water glass solution dripping quantity reaches 2.4m3Time,
Adding food stage green pigment sorbitol solution in retort, it adds weight is the 0.1% of sodium bicarbonate solution weight, water
After glass solution dropping, continue stirring until material system changes into gel；
S3, continuation are the dilute sulfuric acid of 0.5M toward addition concentration in retort, stir, and the endpoint pH controlling system is
Acid adding is stopped when 4；
S4, the silica dioxide gel of formation is carried out filter pressing, wash gel press cake with water and remove salt and the cation poly-third of residual
Acrylamide, is dried the silicon dioxide pigment gel after washing, pulverizes, and prepares silicon dioxide granule.
Embodiment 2, the preparation method of surface modified silicon dioxide particle of the present invention
S1, by fully dispersed for PAMC in aqueous, obtain the cation polypropylene that mass concentration is 1.0%
Amide solution；
S2, past retort implantation concentration are the sodium bicarbonate solution 5.5m of 0.8M3, it is subsequently adding PAMC molten
Liquid 0.5m3, control mixing speed is 35hz, stir-activating 15min, past anti-according to the speed of 2000L/h the most at normal temperatures
Answer tank drips modulus be 3.3, concentration be the water glass solution 5.8m of 0.8M3, when water glass solution dripping quantity reaches 3.0m3Time,
Adding Food-grade blue pigment glycerite in retort, it adds weight is the 0.5% of sodium bicarbonate solution weight, water glass
After the dropping of glass solution, continue stirring until material system changes into gel；
S3, continuation are the dilute sulfuric acid of 1.0M toward addition concentration in retort, stir, and the endpoint pH controlling system is
Acid adding is stopped when 5；
S4, the silica dioxide gel of formation is carried out filter pressing, wash gel press cake with water and remove salt and the cation poly-third of residual
Acrylamide, is dried the silicon dioxide pigment gel after washing, pulverizes, and prepares silicon dioxide granule.
Embodiment 3, the preparation method of surface modified silicon dioxide particle of the present invention
S1, by fully dispersed for PAMC in aqueous, obtain the cation polypropylene that mass concentration is 0.6%
Amide solution；
S2, past retort implantation concentration are the sodium bicarbonate solution 5.5m of 0.6M3, it is subsequently adding PAMC molten
Liquid 0.4m3, control mixing speed is 32hz, stir-activating 10min, past anti-according to the speed of 1800L/h the most at normal temperatures
Answer tank drips modulus be 3.3, concentration be the water glass solution 5.0m of 0.7M3, when water glass solution dripping quantity reaches 2.5m3Time,
Adding Food-grade blue pigment sorbitol solution in retort, it adds weight is the 0.2% of sodium bicarbonate solution weight, water
After glass solution dropping, continue stirring until material system changes into gel；
S3, continuation are the dilute sulfuric acid of 0.8M toward addition concentration in retort, stir, and the endpoint pH controlling system is
Acid adding is stopped when 5；
S4, the silica dioxide gel of formation is carried out filter pressing, wash gel press cake with water and remove salt and the cation poly-third of residual
Acrylamide, is dried the silicon dioxide pigment gel after washing, pulverizes, and prepares silicon dioxide granule.
Embodiment 4, the preparation method of surface modified silicon dioxide particle of the present invention
S1, by fully dispersed for PAMC in aqueous, obtain the cation polypropylene that mass concentration is 0.8%
Amide solution；
S2, past retort implantation concentration are the sodium bicarbonate solution 5.5m of 0.7M3, it is subsequently adding PAMC molten
Liquid 0.4m3, control mixing speed is 35hz, stir-activating 15min, past anti-according to the speed of 2000L/h the most at normal temperatures
Answer tank drips modulus be 3.3, concentration be the water glass solution 5.1m of 0.8M3, when water glass solution dripping quantity reaches 2.5m3Time,
Adding food stage red pigments polyglycol solution in retort, it adds weight is the 0.3% of sodium bicarbonate solution weight,
After water glass solution dropping, continue stirring until material system changes into gel；
S3, continuation are the dilute sulfuric acid of 0.6M toward addition concentration in retort, stir, and the endpoint pH controlling system is
Acid adding is stopped when 4；
S4, the silica dioxide gel of formation is carried out filter pressing, wash gel press cake with water and remove salt and the cation poly-third of residual
Acrylamide, is dried the silicon dioxide pigment gel after washing, pulverizes, and prepares silicon dioxide granule.
Embodiment 5, the preparation method of surface modified silicon dioxide particle of the present invention
S1, by fully dispersed for PAMC in aqueous, obtain the cation polypropylene that mass concentration is 0.8%
Amide solution；
S2, past retort implantation concentration are the sodium bicarbonate solution 4.5m of 0.6M3, it is subsequently adding PAMC molten
Liquid 0.4m3, control mixing speed is 35hz, stir-activating 15min, past anti-according to the speed of 2000L/h the most at normal temperatures
Answer tank drips modulus be 3.3, concentration be the water glass solution 5.8m of 0.5M3, when water glass solution dripping quantity reaches 3.0m3Time,
Adding food grade white pigment glycerite in retort, it adds weight is the 0.1% of sodium bicarbonate solution weight, water glass
After the dropping of glass solution, continue stirring until material system changes into gel；
S3, continuation are the dilute sulfuric acid of 0.6M toward addition concentration in retort, stir, and the endpoint pH controlling system is
Acid adding is stopped when 4；
S4, the silica dioxide gel of formation is carried out filter pressing, wash gel press cake with water and remove salt and the cation poly-third of residual
Acrylamide, is dried the silicon dioxide pigment gel after washing, pulverizes, and prepares silicon dioxide granule.
Comparative example 1,
Compared with Example 3, the difference of this comparative example is: controlling mixing speed in step S2 is 25hz, water glass solution
Rate of addition be 1200L/h.Other parameters and operation are with embodiment 3.This operation of result not only makes the response time extend,
Cost up, and occur that the time of gel also extends about 30min, the silicon dioxide density simultaneously prepared is big, for 0.70g/ml,
Suspension time is 21min.
Comparative example 2,
Compared with Example 3, the difference of this comparative example is: controlling mixing speed in step S2 is 40hz, water glass solution
Rate of addition be 2200L/h.Other parameters and operation are with embodiment 3.A large amount of foam is produced, not only during bearing reaction
Cause silicon dioxide granule dyeing difficulty, and the silicon dioxide hardness prepared is too low, does not possess friction clean-up performance.
Comparative example 3,
Compared with Example 3, the difference of this comparative example is: use PAMA as surface modifier, consumption
Constant.Other parameters and operation are with embodiment 3.
Comparative example 4,
Compared with Example 3, the difference of this comparative example is: use Dodecyl trimethyl ammonium chloride as surface modifier,
Consumption is constant.Other parameters and operation are with embodiment 3.
Comparative example 5,
Compared with Example 3, the difference of this comparative example is: using triethanolamine as surface modifier, consumption is constant.Its
His parameter and operation are with embodiment 3.
Test example
To the embodiment of the present invention 1～5, density and the suspension time of the silicon dioxide granule that comparative example 3～5 prepares detect,
Result see table 1.
Suspension time detection process steps is: first preparing test solution, the component of test solution and mass fraction thereof be: Pyrusussuriensis
Alcohol 40%, water 55.6%, CMC0.2%, take 90m test solution in the graduated cylinder of 200ml, add the above-mentioned titanium dioxide of 4g
After silicon particle, concussion uniformly, stands and starts timing.
Table 1 each silicon dioxide granule performance test results table
| Project | Density (g/ml) | Suspension time (min) |
| Embodiment 1 | 0.28 | 50 |
| Embodiment 2 | 0.20 | 55 |
| Embodiment 3 | 0.23 | 60 |
| Embodiment 4 | 0.25 | 57 |
| Embodiment 5 | 0.30 | 53 |
| Comparative example 3 | 0.58 | 15 |
| Comparative example 4 | 0.36 | 32 |
| Comparative example 5 | 0.32 | 28 |
From upper table 1, the density of the silicon dioxide granule prepared by the present invention is low, is 0.20～0.30g/ml, and when suspending
Between then up to 50～60min, hence it is evident that being longer than prior art, the silicon dioxide granule prepared by the present invention can keep moderate in addition
Hardness.
Comparative example 3 uses PAMA as surface modifier, and its density raises, and suspension time substantially shortens to
15min, illustrates to use PAMA can not improve the suspension of silicon dioxide granule in preparation method of the present invention
Energy；Comparative example 4 and comparative example 5 use different cationic surfactants (Dodecyl trimethyl ammonium chloride and triethanolamine)
As the surface modifier of the present invention, the suspendability of its prepared silicon dioxide granule is all not as good as the embodiment of the present invention 1～5.
The principle of above-described embodiment only illustrative present invention and effect thereof, not for limiting the present invention.Any it is familiar with this skill
Above-described embodiment all can be modified under the spirit and the scope of the present invention or change by the personage of art.Therefore, such as
All that in art, tool usually intellectual is completed under without departing from disclosed spirit and technological thought
Equivalence is modified or changes, and must be contained by the claim of the present invention.
Claims (6)
1. the preparation method of a surface modified silicon dioxide particle, it is characterised in that comprise the following steps:
S1, by fully dispersed for PAMC in aqueous, obtain PAMC solution；
S2, past retort inject sodium bicarbonate solution 4.5～5.5m3, it is subsequently adding PAMC solution 0.4～0.5m3,
Controlling mixing speed is 30～35hz, and stir-activating 10～15min is past according to the speed of 1500～2000L/h the most at normal temperatures
Retort drips water glass solution 4.8～5.8m3, when water glass solution dripping quantity reaches 2.0～3.0m3Time, add in retort
Food grade colorant solution, after water glass solution dropping, continues stirring until material system changes into gel；
S3, continuation add dilute sulfuric acid in retort, stir, and the endpoint pH of control system stops acid adding when being 4～5；
S4, the silica dioxide gel of formation is carried out filter pressing, wash gel press cake with water, to the silicon dioxide pigment after washing
Gel is dried, pulverizes, and prepares silicon dioxide granule.
2. the preparation method of surface modified silicon dioxide particle as claimed in claim 1, it is characterised in that described cation is gathered
The mass concentration of acrylamide solution is 0.2～1.0%.
3. the preparation method of surface modified silicon dioxide particle as claimed in claim 1, it is characterised in that described sodium bicarbonate
The concentration of solution is 0.4～0.8M.
4. the preparation method of surface modified silicon dioxide particle as claimed in claim 1, it is characterised in that described waterglass is molten
The modulus of liquid is 3.3, concentration is 0.4～0.8M.
5. the preparation method of surface modified silicon dioxide particle as claimed in claim 1, it is characterised in that described food stage color
Cellulose solution is the sorbitol of food stage, glycerol or polyglycol solution, and it adds weight is sodium bicarbonate solution weight
0.1～0.5%.
6. the preparation method of surface modified silicon dioxide particle as claimed in claim 1, it is characterised in that described dilute sulfuric acid
Concentration is 0.5～1.0M.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107445171A (en) * | 2017-06-30 | 2017-12-08 | 广州市飞雪材料科技有限公司 | A kind of preparation method of low index of refraction high transparency type silica |
| CN113968584A (en) * | 2021-10-28 | 2022-01-25 | 金三江(肇庆)硅材料股份有限公司 | Hollow spherical silicon dioxide and preparation method thereof |
| CN114479517A (en) * | 2021-12-30 | 2022-05-13 | 湖北三棵树新材料科技有限公司 | Artificial colored sand for improving stone-like coating workability and preparation method thereof |
| CN114477198A (en) * | 2022-02-25 | 2022-05-13 | 六盘水师范学院 | Method for preparing white carbon black by carbon dioxide |
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| CN114479517A (en) * | 2021-12-30 | 2022-05-13 | 湖北三棵树新材料科技有限公司 | Artificial colored sand for improving stone-like coating workability and preparation method thereof |
| CN114477198A (en) * | 2022-02-25 | 2022-05-13 | 六盘水师范学院 | Method for preparing white carbon black by carbon dioxide |
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| CN106009782B (en) | 2017-07-07 |
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