CN107011719A - A kind of preparation method of hydrophobic superfine silicon dioxide for coating agent - Google Patents
A kind of preparation method of hydrophobic superfine silicon dioxide for coating agent Download PDFInfo
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- CN107011719A CN107011719A CN201710308643.6A CN201710308643A CN107011719A CN 107011719 A CN107011719 A CN 107011719A CN 201710308643 A CN201710308643 A CN 201710308643A CN 107011719 A CN107011719 A CN 107011719A
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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
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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
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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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
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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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
- C09C3/12—Treatment with organosilicon compounds
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- Life Sciences & Earth Sciences (AREA)
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- Pigments, Carbon Blacks, Or Wood Stains (AREA)
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Abstract
The invention discloses a kind of preparation method of the hydrophobic superfine silicon dioxide for coating agent, comprise the following steps：(1) the dry powder-shaped silica of 3~7 μm of the dry powder-shaped silica of 8~12 μm of particle diameter and particle diameter is put into glass container and be well mixed；(2) aqueous formic acid of percentage by weight 2% is mixed with methanol, formic acid methyl alcohol mixed liquor is poured slowly into glass container, be kept stirring for state 20~40 minutes；(3) hydrophobically modified silane coupler is atomized, it is then uniform to spray into glass container, at the uniform velocity stir, make raw material fully reaction 30~60 minutes at 40~70 DEG C of reaction temperature；(4) product sealing is placed after reacting, and is aged 3~6 hours；(5) by the drying materials after ageing, air flow super obtains finished product.A kind of preparation method of hydrophobic superfine silicon dioxide for coating agent of the present invention, makes coating agent surface silica dioxide have the state for having out-of-flatness while hydrophobic performance again.
Description
Technical field
The present invention relates to a kind of preparation method of the hydrophobic superfine silicon dioxide for coating agent, belong to coating agent technology neck
Domain.
Background technology
Haze has turned into be influenceed and puzzlement China and people's work and the significant problem lived.We are national
Haze problem is paid much attention to, multi-faceted progress management and control and improvement in terms of technical elements, the material and in terms of policy.According to Chinese Ministry of Environmental Protection
Investigation find, haze formation main matter in include sulfide and nitric acid thing.The source of these materials mainly includes
The flue gas of coal heating, vehicle exhaust and each steam power plant and Industrial Boiler discharge in people's life.
There is a kind of plasma oxidation environmental protection equipment of combined catalyst at present, be adapted to handle sulfur-bearing tail gas containing nitre,
Effect can reach the new standard of country.But catalyst is due to its own characteristic, it is impossible to effective with plasma oxidation environmental protection equipment
Strong bonded by the combination with coating agent, it is necessary to effectively could be securely attached on environmental protection equipment.Due to combining in coating
The catalyst amounts of layer surface are directly proportional to the efficiency of vent gas treatment, so the surface texture of coating agent needs to reach there is out-of-flatness
Undulating state distribution so that increase coating layer surface area.While ensuring that catalyst is firmly effectively combined, make catalysis
It is attached to coating layer surface to agent maximum.And add the different hydrophobic silica of particle diameter can reach surface distributed have fluctuating not
The requirement of level state.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the hydrophobic superfine silicon dioxide for coating agent, make coating
Agent surface silica dioxide has the state for having out-of-flatness while hydrophobic performance again, and it is simple to prepare the process of hydrophobic silica
Folk prescription just, can be adapted to large-scale industrial production, and obtained hydrophobic silica uniform particle sizes, pore structure is stable, and hydrophobic performance is steady
It is fixed.
In order to solve the above technical problems, a kind of preparation side of hydrophobic superfine silicon dioxide for coating agent of the present invention
Method, the preparation method comprises the following steps：
(1) by dry powder-shaped silica that dry powder-shaped silica that particle diameter is 8 μm~12 μm and particle diameter are 3 μm~7 μm
It is put into glass container and is well mixed；
(2) aqueous formic acid of percentage by weight 2% is mixed with methanol, obtains formic acid methyl alcohol mixed liquor, by formic acid
Methyl alcohol mixed liquor is poured slowly into glass container, is kept stirring for state 20~40 minutes；
(3) hydrophobically modified silane coupler is atomized, it is then uniform to spray into glass container, at the uniform velocity stir, make original
Material fully reaction 30~60 minutes at 40~70 DEG C of reaction temperature；
(4) product sealing is placed after reacting, and is aged 3~6 hours；
(5) by the drying materials after ageing, air flow super is then carried out, finished product is obtained.
Preferably, silica is precipitated silica, sol-gal process silica in the step (1).
Preferably, the weight of the dry powder-shaped silica of 8 μm~12 μm of particle diameter is particle diameter 3 μm~7 in the step (1)
μm 0.5~2 times of dry powder-shaped silica.
Preferably, by 2% aqueous formic acid and methanol according to weight ratio (1~3) in the step (2):(3~8)
Ratio is mixed, and the weight of formic acid methyl alcohol mixed liquor is the 10%~30% of the weight of different-grain diameter silica mixture.
Preferably, by 2% aqueous formic acid and methanol according to weight ratio (1~2) in the step (2):(5~6)
Ratio is mixed.
Preferably, hydrophobically modified silane coupler uses 3- aminopropyl triethoxysilanes, N- in the step (3)
(2- aminoethyl -3- aminopropyls) methyl dimethoxysilane, N- (2- aminoethyl -3- aminopropyls) trimethoxy silane, 2- (3,4-
Epoxycyclohexyl) ethyl triethoxysilane, 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane, vinyl triethoxyl silicon
Alkane, vinyl front three oxosilane, MTMS, n-propyl trimethoxy silane, n-octytriethoxysilane, two
Methyl dimethoxy oxygen machine silane, phenyltrimethoxysila,e or HMDO.
Preferably, the addition of hydrophobically modified silane coupler is mixed for different-grain diameter silica in the step (3)
The 30%~70% of the weight of compound.
A kind of preparation method of hydrophobic superfine silicon dioxide for coating agent of the present invention, the preparation method includes as follows
Step：(1) dry powder-shaped silica that particle diameter is 8 μm~12 μm and dry powder-shaped silica that particle diameter is 3 μm~7 μm are put into
It is well mixed in glass container；(2) aqueous formic acid of percentage by weight 2% is mixed with methanol, obtains formic acid methanol and mix
Liquid is closed, formic acid methyl alcohol mixed liquor is poured slowly into glass container, state is kept stirring for 20~40 minutes；(3) by hydrophobically modified
Silane coupler is atomized, then uniform to spray into glass container, is at the uniform velocity stirred, is made raw material at 40~70 DEG C of reaction temperature
Fully reaction 30~60 minutes；(4) product sealing is placed after reacting, and is aged 3~6 hours；(5) material after ageing is dried
It is dry, air flow super is then carried out, finished product is obtained, coating agent surface silica dioxide is had while hydrophobic performance has not again
Smooth state, and it is simple and convenient to prepare the process of hydrophobic silica, can be adapted to large-scale industrial production, it is obtained hydrophobic
Silica uniform particle sizes, pore structure is stable, and hydrophobic performance is stable.
Embodiment
Embodiment of the present invention is described in detail with reference to specific embodiment.It should be appreciated that the reality of the present invention
Apply and be not limited to the following examples, any formal accommodation and/or change made to the present invention fall within this hair
Bright protection domain.
Embodiment 1
A kind of preparation method of hydrophobic superfine silicon dioxide for coating agent, the preparation method comprises the following steps：
(1) it is 3 μm~7 μm dry by dry powder-shaped precipitated silica that 5Kg particle diameters are 8 μm~12 μm and 5Kg particle diameters
Powdery precipitates method silica is put into glass container and is well mixed；
(2) 2% aqueous formic acid and methanol are compared 2 according to weight:5 ratio is mixed, and obtains the mixing of formic acid methanol
Liquid, formic acid methyl alcohol mixed liquor is poured slowly into glass container, and the weight of formic acid methyl alcohol mixed liquor is different-grain diameter silica
The 15% of the weight of mixture, is kept stirring for state 30 minutes；
(3) hydrophobically modified silane coupler 3- aminopropyl triethoxysilanes are atomized, then reacted by being atomized
Device is uniformly sprayed into glass container, and the addition of hydrophobically modified silane coupler is the weight of different-grain diameter silica mixture
30%, at the uniform velocity stir, make the fully reaction 60 minutes at 40 DEG C of reaction temperature of each raw material；
(4) ageing 4 hours is placed in product sealing after reacting；
(5) by the drying materials after ageing, air flow super is then carried out, finished product is obtained.
The characteristic of hydrophobic superfine silicon dioxide finished product is shown in Table 1.
Embodiment 2
A kind of preparation method of hydrophobic superfine silicon dioxide for coating agent, the preparation method comprises the following steps：
(1) it is 3 μm~7 μm by dry powder-shaped sol-gal process silica and 5Kg particle diameters that 10Kg particle diameters are 8 μm~12 μm
Dry powder-shaped sol-gal process silica be put into glass container be well mixed；
(2) 2% aqueous formic acid and methanol are compared 1 according to weight:6 ratio is mixed, and obtains the mixing of formic acid methanol
Liquid, formic acid methyl alcohol mixed liquor is poured slowly into glass container, and the weight of formic acid methyl alcohol mixed liquor is different-grain diameter silica
The 20% of the weight of mixture, is kept stirring for state 20 minutes；
(3) hydrophobically modified silane coupler N- (2- aminoethyl -3- aminopropyls) methyl dimethoxysilane is atomized,
Then uniformly sprayed into by being atomized reactor in glass container, the addition of hydrophobically modified silane coupler is different-grain diameter dioxy
The 50% of the weight of SiClx mixture, is at the uniform velocity stirred, and makes the fully reaction 30 minutes at 50 DEG C of reaction temperature of each raw material；
(4) ageing 5 hours is placed in product sealing after reacting；
(5) by the drying materials after ageing, air flow super is then carried out, finished product is obtained.
The characteristic of hydrophobic superfine silicon dioxide finished product is shown in Table 1.
Embodiment 3
A kind of preparation method of hydrophobic superfine silicon dioxide for coating agent, the preparation method comprises the following steps：
(1) it is 3 μm~7 μm dry by dry powder-shaped precipitated silica that 5Kg particle diameters are 8 μm~12 μm and 10Kg particle diameters
Powdery sol-gal process silica is put into glass container and is well mixed；
(2) 2% aqueous formic acid and methanol are compared 1 according to weight:8 ratio is mixed, and obtains the mixing of formic acid methanol
Liquid, formic acid methyl alcohol mixed liquor is poured slowly into glass container, and the weight of formic acid methyl alcohol mixed liquor is different-grain diameter silica
The 25% of the weight of mixture, is kept stirring for state 40 minutes；
(3) hydrophobically modified silane coupler 2- (3,4- epoxycyclohexyl) ethyl triethoxysilane is atomized, so
Uniformly sprayed into afterwards by being atomized reactor in glass container, the addition of hydrophobically modified silane coupler is different-grain diameter titanium dioxide
The 70% of the weight of silicon mixture, is at the uniform velocity stirred, and makes the fully reaction 50 minutes at 60 DEG C of reaction temperature of each raw material；
(4) ageing 6 hours is placed in product sealing after reacting；
(5) by the drying materials after ageing, air flow super is then carried out, finished product is obtained.
The characteristic of hydrophobic superfine silicon dioxide finished product is shown in Table 1.
Embodiment 4
A kind of preparation method of hydrophobic superfine silicon dioxide for coating agent, the preparation method comprises the following steps：
(1) it is 3 μm~7 μ by dry powder-shaped sol-gal process silica and 5Kg particle diameters that 7.5Kg particle diameters are 8 μm~12 μm
M dry powder-shaped precipitated silica is put into glass container and is well mixed；
(2) 2% aqueous formic acid and methanol are compared 1 according to weight:3 ratio is mixed, and obtains the mixing of formic acid methanol
Liquid, formic acid methyl alcohol mixed liquor is poured slowly into glass container, and the weight of formic acid methyl alcohol mixed liquor is different-grain diameter silica
The 30% of the weight of mixture, is kept stirring for state 25 minutes；
(3) hydrophobically modified silane coupling agent vinyl triethoxysilane is atomized, then by being atomized reactor
Uniform to spray into glass container, the addition of hydrophobically modified silane coupler is the weight of different-grain diameter silica mixture
40%, at the uniform velocity stir, make the fully reaction 45 minutes at 70 DEG C of reaction temperature of each raw material；
(4) ageing 3 hours is placed in product sealing after reacting；
(5) by the drying materials after ageing, air flow super is then carried out, finished product is obtained.
The characteristic of hydrophobic superfine silicon dioxide finished product is shown in Table 1.
Embodiment 5
A kind of preparation method of hydrophobic superfine silicon dioxide for coating agent, the preparation method comprises the following steps：
(1) it is 3 μm~7 μm by dry powder-shaped sol-gal process silica and 5Kg particle diameters that 5Kg particle diameters are 8 μm~12 μm
Dry powder-shaped precipitated silica be put into glass container be well mixed；
(2) 2% aqueous formic acid and methanol are compared 1 according to weight:1 ratio is mixed, and obtains the mixing of formic acid methanol
Liquid, formic acid methyl alcohol mixed liquor is poured slowly into glass container, and the weight of formic acid methyl alcohol mixed liquor is different-grain diameter silica
The 10% of the weight of mixture, is kept stirring for state 35 minutes；
(3) hydrophobically modified silane coupler n-propyl trimethoxy silane is atomized, then by being atomized reactor
Uniform to spray into glass container, the addition of hydrophobically modified silane coupler is the weight of different-grain diameter silica mixture
60%, at the uniform velocity stir, make the fully reaction 40 minutes at 55 DEG C of reaction temperature of each raw material；
(4) ageing 4.5 hours is placed in product sealing after reacting；
(5) by the drying materials after ageing, air flow super is then carried out, finished product is obtained.
The characteristic of hydrophobic superfine silicon dioxide finished product is shown in Table 1.
Hydrophobically modified in a kind of preparation method of hydrophobic superfine silicon dioxide for coating agent of the invention is silane coupled
Agent can also use N- (2- aminoethyl -3- aminopropyls) trimethoxy silane, 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicon
Alkane, vinyl front three oxosilane, MTMS, n-octytriethoxysilane, dimethylformamide dimethyl oxygen machine silane, benzene
Base trimethoxy silane or HMDO.
Table 1
Claims (7)
1. the preparation method of a kind of hydrophobic superfine silicon dioxide for coating agent, it is characterised in that the preparation method is included such as
Lower step：
(1) dry powder-shaped silica that particle diameter is 8 μm~12 μm and dry powder-shaped silica that particle diameter is 3 μm~7 μm are put into
It is well mixed in glass container；
(2) aqueous formic acid of percentage by weight 2% is mixed with methanol, obtains formic acid methyl alcohol mixed liquor, by formic acid methanol
Mixed liquor is poured slowly into glass container, is kept stirring for state 20~40 minutes；
(3) hydrophobically modified silane coupler is atomized, it is then uniform to spray into glass container, at the uniform velocity stir, raw material is existed
Fully reacted 30~60 minutes at 40~70 DEG C of reaction temperature；
(4) product sealing is placed after reacting, and is aged 3~6 hours；
(5) by the drying materials after ageing, air flow super is then carried out, finished product is obtained.
2. a kind of preparation method of hydrophobic superfine silicon dioxide for coating agent according to claim 1, its feature exists
In silica is precipitated silica, sol-gal process silica in the step (1).
3. a kind of preparation method of hydrophobic superfine silicon dioxide for coating agent according to claim 1, its feature exists
In the weight of the dry powder-shaped silica of 8 μm~12 μm of particle diameter is the dry powder-shaped dioxy of 3 μm~7 μm of particle diameter in the step (1)
0.5~2 times of SiClx.
4. a kind of preparation method of hydrophobic superfine silicon dioxide for coating agent according to claim 1, its feature exists
In by 2% aqueous formic acid and methanol according to weight ratio (1~3) in the step (2):The ratio of (3~8) is mixed, first
The weight of sour methyl alcohol mixed liquor is the weight of different-grain diameter silica mixture
10%~30%.
5. a kind of preparation method of hydrophobic superfine silicon dioxide for coating agent according to claim 4, its feature exists
In by 2% aqueous formic acid and methanol according to weight ratio (1~2) in the step (2):The ratio of (5~6) is mixed.
6. a kind of preparation method of hydrophobic superfine silicon dioxide for coating agent according to claim 1, its feature exists
In hydrophobically modified silane coupler uses 3- aminopropyl triethoxysilanes, N- (2- aminoethyl -3- ammonia third in the step (3)
Base) methyl dimethoxysilane, N- (2- aminoethyl -3- aminopropyls) trimethoxy silane, 2- (3,4- epoxycyclohexyl) ethyl
Triethoxysilane, 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane, VTES, vinyl trimethoxy
Silane, MTMS, n-propyl trimethoxy silane, n-octytriethoxysilane, dimethylformamide dimethyl oxygen machine silicon
Alkane, phenyltrimethoxysila,e or HMDO.
7. a kind of preparation method of hydrophobic superfine silicon dioxide for coating agent according to claim 1, its feature exists
In the addition of hydrophobically modified silane coupler is the weight of different-grain diameter silica mixture in the step (3)
30%~70%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107722792A (en) * | 2017-11-13 | 2018-02-23 | 吉林大学 | A kind of preparation method with high anticorrosive property energy epoxy coating |
| CN110387145A (en) * | 2019-07-18 | 2019-10-29 | 常州大学 | A kind of preparation method of the high abrasion white carbon black for butadiene-styrene rubber reinforcement |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107722792A (en) * | 2017-11-13 | 2018-02-23 | 吉林大学 | A kind of preparation method with high anticorrosive property energy epoxy coating |
| CN110387145A (en) * | 2019-07-18 | 2019-10-29 | 常州大学 | A kind of preparation method of the high abrasion white carbon black for butadiene-styrene rubber reinforcement |
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