CN108557828A - A kind of preparation method of the special flatting silica of elastomeric paint - Google Patents
A kind of preparation method of the special flatting silica of elastomeric paint Download PDFInfo
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- CN108557828A CN108557828A CN201810487833.3A CN201810487833A CN108557828A CN 108557828 A CN108557828 A CN 108557828A CN 201810487833 A CN201810487833 A CN 201810487833A CN 108557828 A CN108557828 A CN 108557828A
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- preparation
- silica
- sodium metasilicate
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- flatting silica
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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
- C01B33/126—Preparation of silica of undetermined type
- C01B33/128—Preparation of silica of undetermined type by acidic treatment of aqueous silicate solutions
-
- 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
-
- 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
- C09C1/3081—Treatment with organo-silicon compounds
-
- 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
- C09C1/309—Combinations of treatments provided for in groups C09C1/3009 - C09C1/3081
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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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
- C01P2006/14—Pore volume
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The present invention relates to a kind of preparation methods for special flatting silica in elastomeric paint, in a kettle, sodium metasilicate and water are added, 45 DEG C are warming up to, under stirring, a concentration of 30% sulfuric acid is added, adjust pH value to 6 6.5, again plus ammonium hydroxide tune PH to 8.5 9.0, aging 50min then heat to 90 DEG C, certain density sodium metasilicate and sulfuric acid is added simultaneously, aging 50min, acid adding to PH are 45, are filtered, washed, dry, crushing and classification obtains finished product.Product has oil factor high, and good dispersion, feel is fine and smooth, the characteristics such as transparency height, rational technology, and production efficiency is high.
Description
Technical field
The invention belongs to powder body material technologies of preparing, more particularly to a kind of silica flatting silica for elastomeric paint delustring
Preparation method.
Background technology
The practical aggregation for very little silica grain of fine silica powder is unformed white powder.Silica
Flatting silica because be easily dispersed, extinction performance is good, it is small, to the mechanical property of film and chemically to interfere the transparency of film
The advantages that small, suspension is good in liquid coating, chemical inertness is high can be influenced, is widely used in coating.
The preparation of silica flatting silica mainly has the precipitation method, gel method and vapor phase method three categories.Vapor phase method and gel method
Production cost it is all higher.And specific surface area made from different production technologies differs, gel silica has structure height,
The features such as large specific surface area, large pore volume, and there is good transparency, disadvantage is that oil factor is low, high energy consumption, production cost
It is high.For the precipitation method because its is raw materials used extensively, cheap, production cost is low, and production procedure is simple, and reaction condition is mild, is current
The method for preparing pure superfine silicon dioxide micro mist being most widely used.The typical precipitation method prepare silica technique, main
If silicate solutions, which are added, in acidic precipitation agent generates precipitation, then by sediment heat resolve, finally obtains silica production
Product.Or use the method for distribution addition acidic precipitation agent to obtain the silica product of high-purity.Two prepared by the precipitation method
Silicon oxide powder has higher oil factor, but has the shortcomings that structure is poor, Kong Rong is smaller, poor transparency again, especially compares table
Area is usually only capable of reaching 170-200m2/ g, it is difficult to improve.
And with the improvement of people's living standards, the appearance requirement to daily necessities is higher and higher, more especially
It is frequently used for the position touched, it is desirable that spraying elastic handfeel paint, such as phone housing, mouse, MP3 shells, are no longer requirements
That icy, coarse, stiff feeling, but make one to feel a kind of soft smooth feeling, thus elastic handfeel paint
It comes into being.
In elastic handfeel paint, the selection of flatting silica is critically important, and different flatting silicas is affected to feel, excellent
Dispersion performance has very important influence to the sedimentation of paint.
Invention content
It is an object of the present invention to provide a kind of preparation method of the special flatting silica of elastomeric paint, flatting silica obtained is in elasticity
Extinction performance is high in paint, and dispersion performance is good, and surface smoothness is good, the good characteristics such as feel exquisiteness.The technical solution used is one
The preparation method of the kind special flatting silica of elastomeric paint, includes the following steps：
1）Raw material preparation, sodium metasilicate modulus is 3.3-3.4, iron content ＜ 200PPm, density 1.10-1.25g/ml；Sulfuric acid is dense
Degree is 25-35%；
2）Into reaction kettle plus water and sodium metasilicate, mixing and to adjust reactor temperature be 40-50 DEG C is added dropwise sulfuric acid, works as pH value
For 6.5-7.0 when, it is 8.0-9.0, aging 50min that ammonium hydroxide tune pH value, which is added, is warming up to 80-100 DEG C, while adding sodium metasilicate and sulphur
Acid makes pH value control in 8.0-9.0, and aging 50min, acid adding to PH values is 4-5；
3）Step 2）Reaction product through being filtered, washed, drying, crushing and classification obtains finished product.
Further, step 2）In for the first time the volume ratio of amount of water and sodium metasilicate be 1.5-3:1；Secondary plus sodium metasilicate amount
With for the first time plus sodium metasilicate volume ratio be 1.5-2:1.
Further, step 3）Reaction paste is filtered, washed, silica filter cake is obtained, then reslurry is made
Dimethyl silicone polymer and acrylic acid block its polymers is added in aaerosol solution thereto, then dry, crushing and classification.
Further, a concentration of the 20% of ammonium hydroxide.
The silica elastomeric paint special utility flatting silica of gained of the invention has oil factor high, and extinction is good, and surface is refreshing
The features such as cunning, feel is fine and smooth.Its technical indicator is as follows：
Beneficial effects of the present invention are：
1, only with water as reaction dissolvent, first low-temp reaction obtains the micelle of high stability, forms more gap, and lead to
Crossing secondary charging makes the reactant colloidal particle Brownian movement of first time aggravate, and collision frequency increases, and aggregation velocity is accelerated, and silicon is made
Acid particles are grown up, and are formed the larger primary particle of grain size, are formed simultaneously the aggregation of short texture, so that silica pore is held and are increased
Greatly.
2, in the silica suspension before being spray-dried, adding hole constitution controller effectively improves precipitation
The pore structure of silica inhibits the generation of the small micelle of reaction process, reduces micro pore volume, obtains macropore appearance, high oil absorption value
Silica product.
3, the silicon dioxide granule of gained is subjected to ultra-fine grinding, and be classified, obtain particle diameter distribution Relatively centralized.
Specific implementation mode
The following examples can make those skilled in the art that the present invention be more fully understood, but not limit in any way
The present invention.
Embodiment 1
In 5000L in the reaction kettle of stirring, the sodium silicate solution that 1000L water and 480L is added stirs evenly, and is warming up to 45 DEG C,
30% sulfuric acid is added dropwise into solution with the speed of 4L/min under stirring until pH value is 6.0-7.0, stirs 30min, adds
The ammonium hydroxide tune pH value for entering 20% is continuously heating to 90 DEG C to 8-9, aging 50min, at this temperature, while being added into reaction kettle
Flow is the sodium metasilicate 820L and sulfuric acid of 0.55L/min, and it is 8-9 to keep the pH value of solution, continues aging 50min, has reacted
Bi Jixu acid addings to pH value is 4-5, and reaction paste is filtered, washed, and obtains silica filter cake, it is molten that suspension is made in reslurry
Dimethyl silicone polymer and acrylic acid block its polymers is added in liquid thereto, then dry, crushing and classification.
Embodiment 2
In 5000L in the reaction kettle of stirring, the sodium silicate solution that 1000L water and 500L is added stirs evenly, and is warming up to 40 DEG C,
30% sulfuric acid is added dropwise into solution with the speed of 5L/min under stirring until pH value is 6.0-7.0, stirs 30min, adds
The ammonium hydroxide tune pH value for entering 20% is continuously heating to 85 DEG C to 8-9, aging 50min, at this temperature, while being added into reaction kettle
Flow is the sodium metasilicate 750L and sulfuric acid of 0.55L/min, and it is 8-9 to keep the pH value of solution, continues aging 50min, has reacted
Bi Jixu acid addings to pH value is 4-5, and reaction paste is filtered, washed, and obtains silica filter cake, it is molten that suspension is made in reslurry
Dimethyl silicone polymer and acrylic acid block its polymers is added in liquid thereto, then dry, crushing and classification.
Embodiment 3
In 5000L in the reaction kettle of stirring, the sodium silicate solution that 1000L water and 400L is added stirs evenly, and is warming up to 45 DEG C,
25% sulfuric acid is added dropwise into solution with the speed of 4L/min under stirring until pH value is 6.0-7.0, stirs 30min, adds
The ammonium hydroxide tune pH value for entering 20% is continuously heating to 100 DEG C to 8-9, aging 50min, at this temperature, while adding into reaction kettle
Inbound traffics are the sodium metasilicate 1000L and sulfuric acid of 0.55L/min, and it is 8-9 to keep the pH value of solution, continues aging 50min, reaction
It is 4-5 to finish continuation acid adding to pH value, and reaction paste is filtered, washed, silica filter cake is obtained, suspension is made in reslurry
Dimethyl silicone polymer and acrylic acid block its polymers is added in solution thereto, then dry, crushing and classification.
Embodiment 4
In 5000L in the reaction kettle of stirring, the sodium silicate solution that 1500L water and 500L is added stirs evenly, and is warming up to 45 DEG C,
30% sulfuric acid is added dropwise into solution with the speed of 4L/min under stirring until pH value is 6.0-7.0, stirs 30min, adds
The ammonium hydroxide tune pH value for entering 20% is continuously heating to 90 DEG C to 8-9, aging 50min, at this temperature, while being added into reaction kettle
Flow is the sodium metasilicate 800L and sulfuric acid of 0.55L/min, and it is 8-9 to keep the pH value of solution, continues aging 50min, has reacted
Bi Jixu acid addings to pH value is 4-5, and reaction paste is filtered, washed, and obtains silica filter cake, it is molten that suspension is made in reslurry
Dimethyl silicone polymer and acrylic acid block its polymers is added in liquid thereto, then dry, crushing and classification.
Embodiment 5
In 5000L in the reaction kettle of stirring, the sodium silicate solution that 1200L water and 800L is added stirs evenly, and is warming up to 45 DEG C,
30% sulfuric acid is added dropwise into solution with the speed of 6L/min under stirring until pH value is 6.0-7.0, stirs 30min, adds
The ammonium hydroxide tune pH value for entering 20% is continuously heating to 95 DEG C to 8-9, aging 50min, at this temperature, while being added into reaction kettle
Flow is the sodium metasilicate 1200L and sulfuric acid of 0.6L/min, and it is 8-9 to keep the pH value of solution, continues aging 50min, has reacted
Bi Jixu acid addings to pH value is 4-5, and reaction paste is filtered, washed, and obtains silica filter cake, it is molten that suspension is made in reslurry
Dimethyl silicone polymer and acrylic acid block its polymers is added in liquid thereto, then dry, crushing and classification.
Embodiment 6
In 5000L in the reaction kettle of stirring, the sodium silicate solution that 1000L water and 450L is added stirs evenly, and is warming up to 45 DEG C,
30% sulfuric acid is added dropwise into solution with the speed of 4L/min under stirring until pH value is 6.0-7.0, stirs 30min, adds
The ammonium hydroxide tune pH value for entering 20% is continuously heating to 90 DEG C to 8-9, aging 50min, at this temperature, while being added into reaction kettle
Flow is the sodium metasilicate 800L and sulfuric acid of 0.5L/min, and it is 8-9 to keep the pH value of solution, continues aging 50min, reaction finishes
It is 4-5 to continue acid adding to pH value, and reaction paste is filtered, washed, and obtains silica filter cake, it is molten that suspension is made in reslurry
Dimethyl silicone polymer and acrylic acid block its polymers is added in liquid thereto, then dry, crushing and classification.
Test result is listed as follows：
It will be understood by those skilled in the art that above example is only exemplary embodiment, in the spirit and model without departing substantially from the present invention
In the case of enclosing, a variety of variations can be carried out, replaced and changed.
Claims (7)
1. a kind of preparation method of the special flatting silica of elastomeric paint, includes the following steps：
1）Raw material preparation, sodium metasilicate modulus is 3.3-3.4, iron content ＜ 200PPm, density are 1.10-1.25 g/ml；Sulfuric acid is dense
Degree is 25-35%；
2）Into reaction kettle plus water and sodium metasilicate, mixing and to adjust reactor temperature be 40-50 DEG C is added dropwise sulfuric acid, works as pH value
For 6.5-7.0 when, it is 8.0-9.0, aging 50min that ammonium hydroxide tune pH value, which is added, is warming up to 80-100 DEG C, while adding sodium metasilicate and sulphur
Acid makes pH value control in 8.0-9.0, and aging 50min, acid adding to PH values is 4-5；
3）Step 2）Reaction product through being filtered, washed, drying, crushing and classification obtains finished product.
2. the preparation method of the special flatting silica of elastomeric paint according to claim 1, it is characterised in that：Step 2）In for the first time plus
Water and the volume ratio of sodium metasilicate are 1.5-3:1；It is secondary to add the amount of sodium metasilicate and the volume ratio of sodium metasilicate is added to be 1.5-2 for the first time:
1。
3. the preparation method of the special flatting silica of elastomeric paint according to claim 1, it is characterised in that：Step 3）By reaction slurry
Material is filtered, washed, and obtains silica filter cake, and then aaerosol solution is made in reslurry, and polydimethylsiloxanes are added thereto
Alkane and acrylic acid block its polymers, then dry, crushing and classification.
4. the preparation method of the special flatting silica of elastomeric paint according to claim 1, it is characterised in that：Ammonium hydroxide it is a concentration of
20%。
5. the preparation method of the special flatting silica of elastomeric paint according to claim 1, it is characterised in that：Obtained silica
BET is 250m2/g。
6. the preparation method of the special flatting silica of elastomeric paint according to claim 1, it is characterised in that：Obtained silica
Kong Rongwei 1.40-1.60ml/g.
7. the preparation method of the special flatting silica of elastomeric paint according to claim 1, it is characterised in that：Obtained silica
DBP is 360g/100g.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110564270A (en) * | 2019-08-23 | 2019-12-13 | 广州凌玮科技股份有限公司 | Antirust UV (ultraviolet) curing coating |
| CN110591497A (en) * | 2019-08-23 | 2019-12-20 | 广州凌玮科技股份有限公司 | Steel antirust coating |
| CN110591498A (en) * | 2019-08-23 | 2019-12-20 | 广州凌玮科技股份有限公司 | Water-based antirust primer and application thereof |
| CN110591416A (en) * | 2019-08-23 | 2019-12-20 | 广州凌玮科技股份有限公司 | Preparation method of amorphous silicon dioxide antirust pigment |
| CN110616002A (en) * | 2019-08-23 | 2019-12-27 | 广州凌玮科技股份有限公司 | Antirust powder containing alcohol amine modified amorphous silicon dioxide and production method thereof |
| CN110616021A (en) * | 2019-08-23 | 2019-12-27 | 广州凌玮科技股份有限公司 | Water-based primer-topcoat integrated paint and preparation method and application thereof |
| CN110628256A (en) * | 2019-08-23 | 2019-12-31 | 广州凌玮科技股份有限公司 | Preparation method of amorphous silicon dioxide antirust pigment |
| CN110628300A (en) * | 2019-08-23 | 2019-12-31 | 广州凌玮科技股份有限公司 | Solvent-free antirust primer-topcoat paint and preparation method and application thereof |
| CN110643253A (en) * | 2019-08-23 | 2020-01-03 | 广州凌玮科技股份有限公司 | Oily antirust primer and application thereof |
| WO2020071539A1 (en) * | 2018-10-05 | 2020-04-09 | 富士化学工業株式会社 | Porous silica particle composition |
| CN111573683A (en) * | 2020-07-09 | 2020-08-25 | 福建省南平嘉茂纳米科技发展有限公司 | Preparation method of silica with high specific surface area and low oil absorption value and product thereof |
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| WO2020071539A1 (en) * | 2018-10-05 | 2020-04-09 | 富士化学工業株式会社 | Porous silica particle composition |
| JP7471675B2 (en) | 2018-10-05 | 2024-04-22 | 富士化学工業株式会社 | Porous silica particle composition |
| JP7124107B2 (en) | 2018-10-05 | 2022-08-23 | 富士化学工業株式会社 | Porous silica particle composition |
| JPWO2020071539A1 (en) * | 2018-10-05 | 2021-09-02 | 富士化学工業株式会社 | Porous silica particle composition |
| CN110591416A (en) * | 2019-08-23 | 2019-12-20 | 广州凌玮科技股份有限公司 | Preparation method of amorphous silicon dioxide antirust pigment |
| CN110616021A (en) * | 2019-08-23 | 2019-12-27 | 广州凌玮科技股份有限公司 | Water-based primer-topcoat integrated paint and preparation method and application thereof |
| CN110628256A (en) * | 2019-08-23 | 2019-12-31 | 广州凌玮科技股份有限公司 | Preparation method of amorphous silicon dioxide antirust pigment |
| CN110628300A (en) * | 2019-08-23 | 2019-12-31 | 广州凌玮科技股份有限公司 | Solvent-free antirust primer-topcoat paint and preparation method and application thereof |
| CN110643253A (en) * | 2019-08-23 | 2020-01-03 | 广州凌玮科技股份有限公司 | Oily antirust primer and application thereof |
| CN110616002A (en) * | 2019-08-23 | 2019-12-27 | 广州凌玮科技股份有限公司 | Antirust powder containing alcohol amine modified amorphous silicon dioxide and production method thereof |
| CN110564270A (en) * | 2019-08-23 | 2019-12-13 | 广州凌玮科技股份有限公司 | Antirust UV (ultraviolet) curing coating |
| CN110591498A (en) * | 2019-08-23 | 2019-12-20 | 广州凌玮科技股份有限公司 | Water-based antirust primer and application thereof |
| CN110591497A (en) * | 2019-08-23 | 2019-12-20 | 广州凌玮科技股份有限公司 | Steel antirust coating |
| CN111573683A (en) * | 2020-07-09 | 2020-08-25 | 福建省南平嘉茂纳米科技发展有限公司 | Preparation method of silica with high specific surface area and low oil absorption value and product thereof |
| CN111573683B (en) * | 2020-07-09 | 2021-12-28 | 福建省南平嘉茂纳米科技发展有限公司 | Preparation method of silica with high specific surface area and low oil absorption value and product thereof |
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