CN108441026A - A kind of dewatering nano hydrated SiO 2 and its preparation method and application - Google Patents
A kind of dewatering nano hydrated SiO 2 and its preparation method and application Download PDFInfo
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- CN108441026A CN108441026A CN201810376804.XA CN201810376804A CN108441026A CN 108441026 A CN108441026 A CN 108441026A CN 201810376804 A CN201810376804 A CN 201810376804A CN 108441026 A CN108441026 A CN 108441026A
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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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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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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- 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
- C09D7/66—Additives characterised by particle size
- C09D7/67—Particle size smaller than 100 nm
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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Abstract
The present invention relates to nano hydrated silica, and in particular to a kind of dewatering nano hydrated SiO 2 and its preparation method and application.Reaction kettle is preheated to 126 DEG C or more, nano hydrated silica is added in reaction kettle, then silazane is added dropwise, the weight ratio of nano hydrated silica and silazane is 10:1, at 126~135 DEG C, the reaction time is 1.5~2h, removes ammonia simultaneously during the reaction, and dewatering nano hydrated SiO 2 is made for reaction temperature control.Nano hydrated silica is reacted with silazane generates trimethyl silane dewatering nano hydrated SiO 2 and ammonia, eliminates nano hydrated silica interior hydroxyl, is transformed into lipophile.
Description
Technical field
The present invention relates to nano hydrated silica, and in particular to a kind of dewatering nano hydrated SiO 2 and its preparation side
Method and application.
Background technology
Nano hydrated silica is also known as Nano carbon white, nano hydrated silica be widely used in rubber reinforcing filler,
The various fields such as ink thickeners, sprayed on material, delustering agent, since there are a large amount of activity hydroxies, tools for nano hydrated silica
There is hydrophily, limit its use scope, when applying in reinforcement silicon rubber, ink, paint, coating, adhesive and fluid sealant
Be required for before field carrying out hydrophobicity processing, currently, the production method that nano hydrated silicon dioxide drainage is modified had it is more
Kind, but can remaining bi-products and the not high disadvantage of degree of substitution in their generally existing products.
Invention content
The technical problem to be solved by the present invention is to：There is provided it is a kind of there is no by-product, hydrophobic performance is good, has a wide range of application
Dewatering nano hydrated SiO 2 and its preparation method and application.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：A kind of dewatering nano hydrated SiO 2
Preparation method, preheating reaction kettle to 126 DEG C or more, nano hydrated silica is added in reaction kettle, then silicon nitrogen is added dropwise
The weight ratio of alkane, the nano hydrated silica and silazane is 10:1~2, reaction temperature is controlled at 126~135 DEG C, instead
It is 1.5~2h between seasonable, removes ammonia simultaneously during the reaction, dewatering nano hydrated SiO 2 is made.
The beneficial effects of the present invention are：Silazane, silazane elder generation vapour is added dropwise in reaction kettle of the temperature more than 126 DEG C
To change, silazane and nano hydrated silica are actually gas-solid reaction, have enough uniformitys and degree of mixing, are swift in response,
Nano hydrated silica, which is reacted with silazane under specific temperature and appointed condition, generates the hydration of trimethyl silane dewatering nano
Silica and ammonia eliminate nano hydrated silica interior hydroxyl, are transformed into lipophile, to making such as high temperature resistant oiliness
Coating and environmental protection all expand and deepen its purposes and field in terms of absorbing waste oil product, remaining ammonia removes, and product is made to reach
The index needed to neutral or client, and other by-products are not present in reaction kettle, production efficiency is high.
The present invention also provides dewatering nano hydrations prepared by a kind of preparation method of above-mentioned dewatering nano hydrated SiO 2
Silica.
The present invention also provides a kind of above-mentioned dewatering nano hydrated SiO 2s in ink, wall covering, adhesive and sealing
Application in glue.
The beneficial effects of the present invention are：
(1) the dewatering nano hydrated SiO 2 that the present invention develops main function in ink is rheology control, improves ground
Level ground paint weatherability, stability, scratch resistance, improve coating flow leveling and coating as a result, can preferably extend product makes
Use the time limit.
(2) the dewatering nano hydrated SiO 2 that the present invention develops is applied in wall covering, and main function is to prevent coating
Sagging improves the flatness of construction surface.Aerosil is adsorbed on powdery paints surface, forms displaceable layers, prevents powder
Coating absorbs moisture, prevents from luming, and improves the mobility of powdery paints and aesthetic.
(3) the dewatering nano hydrated SiO 2 developed of the present invention is in adhesive and fluid sealant, because its is excellent hydrophobic
Performance is preferably combined with organic solvent so substantially increasing adhesive strength and leakproofness.
Specific implementation mode
To explain the technical content, the achieved purpose and the effect of the present invention in detail, it is explained below in conjunction with embodiment.
The design of most critical of the present invention is：Nano hydrated silica is with silazane under specific temperature and appointed condition
Reaction generates trimethyl silane dewatering nano hydrated SiO 2 and ammonia, eliminates nano hydrated silica interior hydroxyl,
It is transformed into lipophile, other by-products is not present in reaction kettle, production efficiency is high.
The present invention provides a kind of preparation method of dewatering nano hydrated SiO 2, preheating reaction kettle to 126 DEG C or more,
Nano hydrated silica is added in reaction kettle, then silazane is added dropwise, the weight of the nano hydrated silica and silazane
Amount is than being 10:1~2, at 126~135 DEG C, the reaction time is 1.5~2h, is removed simultaneously during the reaction for reaction temperature control
Dewatering nano hydrated SiO 2 is made in ammonia.
The present invention chemical equation be：(CH3)3Si-NH-Si(CH3)3+2R3SiOH→2R3SiO-Si(CH3)3+
NH3↑, reaction temperature is 126~135 DEG C.
As can be seen from the above description, the beneficial effects of the present invention are：Silicon nitrogen is added dropwise in reaction kettle of the temperature more than 126 DEG C
Alkane, silazane first vaporize, and silazane and nano hydrated silica are actually gas-solid reaction, there is enough uniformitys and mixing
Degree, is swift in response, and nano hydrated silica, which is reacted with silazane under specific temperature and appointed condition, generates trimethyl silane
Dewatering nano hydrated SiO 2 and ammonia eliminate nano hydrated silica interior hydroxyl, are transformed into lipophile, to making
All expand and deepen its purposes and field in terms of absorbing waste oil product such as high temperature resistant oil paint and environmental protection, remaining ammonia is logical
The method for crossing vacuumize process removes, and so that product is reached neutral or client's needs indexs, and it is secondary that other are not present in reaction kettle
Product, production efficiency are high.
Further, the gas valve of reaction kettle is opened during the reaction, and the ammonia of generation enters tail gas absorption spray
Tower, after reaction, remaining ammonia is removed using vacuum suction mode in reaction kettle, vacuum degree be -0.03MPa~-
0.01MPa。
Seen from the above description, ammonia is removed by the way of vacuumizing, vacuum degree is -0.03MPa~-0.01MPa, can
To completely remove the ammonia in reaction kettle.
Further, the gas valve of reaction kettle is opened during the reaction, and the ammonia of generation enters tail gas absorption spray
Tower, after reaction, the remaining ammonia in the reaction kettle also can be used high temperature mode and remove, and temperature is controlled 126 DEG C~130
℃。
Further, the spray liquid in the tail gas absorption spray column use mass fraction for 5~10% diluted acid water.
Further, the diluted acid water is dilute hydrochloric acid water.
Further, preheating reaction kettle is to 126~135 DEG C.
Seen from the above description, preheating reaction kettle can not only ensure that silazane vaporizes, but also can protect to 126~135 DEG C
Nano hydrated silica is demonstrate,proved smoothly quickly to be reacted with silazane.
Further, the rate of addition of the silazane is 500ml/min.
The present invention also provides dewatering nano hydrations prepared by a kind of preparation method of above-mentioned dewatering nano hydrated SiO 2
Silica.
The present invention also provides a kind of above-mentioned dewatering nano hydrated SiO 2s in ink, wall covering, adhesive and sealing
Application in glue.
As can be seen from the above description, the beneficial effects of the present invention are：
(1) the dewatering nano hydrated SiO 2 that the present invention develops main function in ink is rheology control, improves ground
Level ground paint weatherability, stability, scratch resistance, improve coating flow leveling and coating as a result, can preferably extend product makes
Use the time limit.
(2) the dewatering nano hydrated SiO 2 that the present invention develops is applied in wall covering, and main function is to prevent coating
Sagging improves the flatness of construction surface.Aerosil is adsorbed on powdery paints surface, forms displaceable layers, prevents powder
Coating absorbs moisture, prevents from luming, and improves the mobility of powdery paints and aesthetic.(3) the dewatering nano water that the present invention develops
Silica is closed in adhesive and fluid sealant, because its excellent hydrophobic performance is preferably combined with organic solvent so carrying significantly
High adhesive strength and leakproofness.
Embodiment 1
A kind of preparation method of dewatering nano hydrated SiO 2, preheating reaction kettle are added to 126 DEG C in reaction kettle
The nano hydrated silica of 500g, then 50g silazane is slowly added dropwise, the weight ratio of the nano hydrated silica and silazane
It is 10:1, reaction temperature is controlled at 126 DEG C, reaction time 1.5h, opens the gas valve of reaction kettle, production during the reaction
Raw ammonia enters tail gas absorption spray column, the spray liquid in the tail gas absorption spray column use mass fraction for 5% it is dilute
Hydrochloric acid water, after reaction, remaining ammonia is removed using vacuum suction mode in reaction kettle, and vacuum degree is -0.03MPa, system
Obtain dewatering nano hydrated SiO 2.
The present invention also provides a kind of above-mentioned dewatering nano hydrated SiO 2s in ink, wall covering, adhesive and sealing
Application in glue.
Embodiment 2
A kind of preparation method of dewatering nano hydrated SiO 2, preheating reaction kettle are added to 130 DEG C in reaction kettle
The nano hydrated silica of 500g, then 75g silazane is added dropwise, the weight ratio of the nano hydrated silica and silazane is
10:1.5, reaction temperature is controlled at 130 DEG C, reaction time 1.8h, opens the gas valve of reaction kettle, production during the reaction
Raw ammonia enters tail gas absorption spray column, the spray liquid in the tail gas absorption spray column use mass fraction for 8% it is dilute
Hydrochloric acid water, after reaction, remaining ammonia is removed using vacuum suction mode in reaction kettle, and vacuum degree is -0.02MPa, system
Obtain dewatering nano hydrated SiO 2.
Embodiment 3
A kind of preparation method of dewatering nano hydrated SiO 2, preheating reaction kettle are added to 135 DEG C in reaction kettle
The nano hydrated silica of 500g, then 100g silazane is added dropwise, the weight ratio of the nano hydrated silica and silazane is
10:2, reaction temperature is controlled at 135 DEG C, reaction time 2h, opens the gas valve of reaction kettle during the reaction, generation
Ammonia enters tail gas absorption spray column, the spray liquid in the tail gas absorption spray column use mass fraction for 10% dilute hydrochloric acid
Water, after reaction, remaining ammonia is removed using high temperature mode in reaction kettle, and temperature is controlled at 126 DEG C~130 DEG C, is made
Dewatering nano hydrated SiO 2.
Comparative example 1
The method for preparing dewatering nano hydrated SiO 2：Using 5% emulsifier and 15% hydrated SiO 2 suspension
In 1 ︰, 3 ratios in 80 DEG C of temperature and 3 hours time hybrid reactions, and pH 7~12 is being adjusted with organic base, through drying, ground
Grind the hydrophobic nano hydrated SiO 2 of production.
Comparative example 2
The method for preparing dewatering nano hydrated SiO 2：Hydrated SiO 2 wet gel (moisture content 86%) is added to
In reaction kettle, and the temperature of 90 DEG C of agitating and heating heating, it is 2.5 to be adjusted to modified required pH with dilute sulfuric acid, adds quality
The modifying agent that score is 3% is such as：Silane coupling A 171 is modified reaction, controls 2 small the reaction times, finally washes, is dry
It is dry, crush, be packaged to be hydrophobic nano hydrated SiO 2.
The hydrophobic silicic aerogels prepared by dewatering nano hydrated SiO 2 comparative example 1 provided by the present invention and comparative example 2
Compare hydrophobicity result such as the following table 1
1 hydrophobicity of table compares
| Product | Hydrophobicity/% |
| Embodiment 1 (10% silazane) | 78.2 |
| Embodiment 2 (15% silazane) | 79.8 |
| Embodiment 3 (20% silazane) | 80.3 |
| Comparative example 1 | 58.1 |
| Comparative example 2 | 56.3 |
Note：Dewatering nano is hydrated two by the hydrophobic degree that hydrophobicity method system measures product using general Ethanol Method
Silica is placed in 25ml water, and absolute ethyl alcohol is slowly added dropwise until dewatering nano hydrated SiO 2 powder is completely immersed in solution
Until, record the volume V (ml) used in absolute ethyl alcohol.
Hydrophobicity=(V/V+25) × 100%
The dewatering nano prepared by dewatering nano hydrated SiO 2 provided by the present invention and comparative example 1 and comparative example 2
The Comparison study result such as the following table 2 of silica in ink, wall covering, adhesive and fluid sealant
2 application performance of table compares
As known from Table 1, it adds 10% silazane and adds the dewatering nano that 15% silazane and 20% silazane are produced
Hydrated SiO 2 product influences less downstream product, but considers that the ductility of inventive method is still included in as a comparison, this
The hydrophobicity for inventing the dewatering nano hydrated SiO 2 prepared is much larger than comparative example 1 and comparative example 2.
Dewatering nano hydrated SiO 2 produced by the invention and comparison hydrophobic silicic aerogels have been investigated simultaneously in ink, metope
Application effect in coating, adhesive and fluid sealant, the dewatering nano hydration titanium dioxide that as can be seen from Table 2 prepared by the present invention
Silicon is applied to be uniformly mixed in ink, wall covering, adhesive and fluid sealant, and product stability is good, has apparent superiority.
In conclusion the preparation method of dewatering nano hydrated SiO 2 provided by the invention, in temperature more than 126 DEG C
Silazane is added dropwise in reaction kettle, silazane first vaporizes, and silazane and nano hydrated silica are actually gas-solid reaction, there is foot
Enough uniformitys and degree of mixing, are swift in response, and nano hydrated silica is anti-under specific temperature and appointed condition with silazane
Trimethyl silane dewatering nano hydrated SiO 2 and ammonia should be generated, nano hydrated silica interior hydroxyl is eliminated, is turned
Become lipophile, to make as high temperature resistant oil paint and environmental protection absorb waste oil product in terms of all expand and deepen its purposes with
Field, remaining ammonia are removed by the method for vacuumize process, so that product is reached neutral or client's needs indexs, and react
Other by-products are not present in kettle, production efficiency is high.
Example the above is only the implementation of the present invention is not intended to limit the scope of the invention, every to utilize this hair
Equivalents made by bright description are applied directly or indirectly in relevant technical field, are similarly included in this hair
In bright scope of patent protection.
Claims (9)
1. a kind of preparation method of dewatering nano hydrated SiO 2, which is characterized in that preheating reaction kettle to 126 DEG C or more,
Nano hydrated silica is added in reaction kettle, then silazane is added dropwise, the weight of the nano hydrated silica and silazane
Amount is than being 10:1~2, at 126~135 DEG C, the reaction time is 1.5~2h, is removed simultaneously during the reaction for reaction temperature control
Dewatering nano hydrated SiO 2 is made in ammonia.
2. the preparation method of dewatering nano hydrated SiO 2 according to claim 1, which is characterized in that in reaction process
The middle gas valve for opening reaction kettle, the ammonia of generation enters tail gas absorption spray column, after reaction, remaining in reaction kettle
Ammonia is removed using vacuum suction mode, and vacuum degree is -0.03MPa~-0.01MPa.
3. the preparation method of dewatering nano hydrated SiO 2 according to claim 1, which is characterized in that in reaction process
The middle gas valve for opening reaction kettle, the ammonia of generation enters tail gas absorption spray column, after reaction, in the reaction kettle
Remaining ammonia also can be used high temperature mode and remove, and temperature is controlled at 126 DEG C~130 DEG C.
4. the preparation method of dewatering nano hydrated SiO 2 according to claim 2 or 3, which is characterized in that the tail
Spray liquid in aspiration spray column use mass fraction for 5~10% diluted acid water.
5. the preparation method of dewatering nano hydrated SiO 2 according to claim 4, which is characterized in that the diluted acid water
For dilute hydrochloric acid water.
6. the preparation method of dewatering nano hydrated SiO 2 according to claim 1, which is characterized in that pre-add thermal response
Kettle is to 126~135 DEG C.
7. the preparation method of dewatering nano hydrated SiO 2 according to claim 1, which is characterized in that the silazane
Rate of addition be 500ml/min.
8. a kind of dredge according to prepared by the preparation method of claim 1~7 any one of them dewatering nano hydrated SiO 2
The nano hydrated silica of water.
9. a kind of dewatering nano hydrated SiO 2 according to claim 8 is in ink, wall covering, adhesive and sealing
Application in glue.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110330790A (en) * | 2019-06-25 | 2019-10-15 | 湖南华曙高科技有限责任公司 | It is a kind of for laser sintered polyamide fire proofing preparation method |
| CN111019400A (en) * | 2019-12-25 | 2020-04-17 | 烟台大学 | Silicon dioxide surface modification method based on homogeneous reaction system |
| CN114836057A (en) * | 2022-04-07 | 2022-08-02 | 福建远翔新材料股份有限公司 | Preparation method of nano hydrated silicon dioxide super-hydrophobic modification |
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| CN1687246A (en) * | 2005-03-28 | 2005-10-26 | 广州吉必时科技实业有限公司 | Method for preparing hydrophobic type nano silicon dioxide thruogh continuous surface treatment |
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2018
- 2018-04-25 CN CN201810376804.XA patent/CN108441026A/en active Pending
Patent Citations (1)
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| CN1687246A (en) * | 2005-03-28 | 2005-10-26 | 广州吉必时科技实业有限公司 | Method for preparing hydrophobic type nano silicon dioxide thruogh continuous surface treatment |
Non-Patent Citations (1)
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| 赵临襄等: "《化学制药工艺学》", 31 August 2015, 中国医药科技出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110330790A (en) * | 2019-06-25 | 2019-10-15 | 湖南华曙高科技有限责任公司 | It is a kind of for laser sintered polyamide fire proofing preparation method |
| CN111019400A (en) * | 2019-12-25 | 2020-04-17 | 烟台大学 | Silicon dioxide surface modification method based on homogeneous reaction system |
| CN114836057A (en) * | 2022-04-07 | 2022-08-02 | 福建远翔新材料股份有限公司 | Preparation method of nano hydrated silicon dioxide super-hydrophobic modification |
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Application publication date: 20180824 |