CN112831201B - Preparation method of siliceous inorganic nano-permeable concrete structure protective coating - Google Patents
Preparation method of siliceous inorganic nano-permeable concrete structure protective coating Download PDFInfo
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- CN112831201B CN112831201B CN202110004964.3A CN202110004964A CN112831201B CN 112831201 B CN112831201 B CN 112831201B CN 202110004964 A CN202110004964 A CN 202110004964A CN 112831201 B CN112831201 B CN 112831201B
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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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
- C04B41/5035—Silica
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/60—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
- C04B41/61—Coating or impregnation
- C04B41/65—Coating or impregnation with inorganic materials
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- Aftertreatments Of Artificial And Natural Stones (AREA)
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Abstract
The invention discloses a preparation method of siliceous inorganic nano-penetration type protective coating for a concrete structure, which comprises the following steps: mixing hydrogen and oxygen in proportion, and introducing the mixture into a sodium silicate solution in a first reaction kettle; removing water from the silicon tetrachloride liquid, rectifying and treating by using a molecular sieve to obtain silicon tetrachloride gas containing peroxide; introducing the obtained gas into a first reaction kettle, heating and pressurizing, and reacting for 30 minutes; introducing pure air into the first reaction kettle for gas replacement; introducing the product of the first reaction kettle into an alkaline washing tower and a drying tower, and then conveying the product to a second reaction kettle; adding ethanol into the second reaction kettle, heating to 80 ℃, introducing a gamma-methacryloxypropyltrimethoxysilane solution, and reacting for 1-1.5 hours; separating, washing and drying the product; and dissolving the obtained solid particles in water to prepare the protective coating. The coating has the advantages of strong permeability, freeze-thaw resistance, acid and alkali resistance, good protection effect, strong cohesiveness and durability, simple preparation and construction and low cost.
Description
Technical Field
The invention relates to the field of protective coatings, in particular to a preparation method of a siliceous inorganic nano-permeable protective coating for a concrete structure.
Background
The protection of the surface of the concrete structure under the environmental conditions of chemical erosion, freeze-thaw damage, chloride salt and the like is an important measure for ensuring the durability of the concrete structure, and the specification of railway concrete structure durability repair and protection puts forward a clear requirement.
The coating of protective materials on the surface of a concrete structure is a common protective measure at present, and the protective materials comprise two major types, namely organic and inorganic materials. Wherein, the organic protective material has poor durability and weak caking property, needs to be repeatedly constructed at regular intervals and has higher cost; the inorganic protective material has large particles, and has weak permeability to concrete structures with small pores, and is difficult to form a protective layer with a certain thickness, so the protective effect is poor.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a siliceous inorganic nano-penetration protective coating which can penetrate into structures such as concrete and has good protective performance.
A preparation method of siliceous inorganic nano-penetration type protective coating for concrete structure comprises the following steps:
mixing hydrogen and oxygen according to the volume ratio of 1:1.5, and introducing the mixture into a sodium silicate solution in a first reaction kettle;
and (3) carrying out water removal, rectification and molecular sieve treatment on the silicon tetrachloride liquid to obtain silicon tetrachloride gas containing a small amount of peroxide.
Introducing the silicon tetrachloride gas containing a small amount of peroxide into a sodium silicate solution in the first reaction kettle, wherein the molar ratio of the silicon tetrachloride gas to hydrogen to oxygen is (1-1.5) to 1:1.5, controlling the flow rates of the silicon tetrachloride gas to hydrogen to oxygen, controlling the heating temperature to 1500 ℃, controlling the pressure to be 1.8-2.0 Mpa, and keeping the reaction time for 30 minutes;
introducing pure air into the first reaction kettle, replacing the gas in the reaction kettle and keeping the safety pressure of the reaction kettle;
sequentially introducing a reaction product in the first reaction kettle into an alkaline washing tower and a drying tower, then conveying the reaction product to a second reaction kettle, adding ethanol into the second reaction kettle, enabling the mass ratio of the reaction product to the ethanol to be 1:3, mixing the reaction product and the ethanol by adopting ultrasonic waves, then heating to 80 ℃, slowly introducing a gamma-methacryloxypropyltrimethoxysilane solution, reacting for 1-1.5 hours, and controlling the crystal form;
performing cyclone separation, washing and drying on the product in the second reaction kettle to obtain solid particles;
and (3) dissolving the solid particles in a proper amount of water according to construction requirements to obtain the siliceous inorganic nano-penetration protective coating.
The content of peroxide in the silicon tetrachloride gas is less than or equal to 0.1 wt%.
Preferably, during the rectification process of the silicon tetrachloride liquid, rectifying and purifying the distilled components for 2-3 times;
preferably, after the mixed gas of hydrogen and oxygen is introduced into the first reaction kettle and blown for 30 minutes, the silicon tetrachloride gas containing a small amount of peroxide is introduced into the sodium silicate solution in the first reaction kettle.
Preferably, the hydrogen and oxygen gases are pressurized, dried and purified before being mixed.
Preferably, the gamma-methacryloxypropyltrimethoxysilane solution is an alcoholic solution of gamma-methacryloxypropyltrimethoxysilane.
Preferably, the molar ratio of silicon tetrachloride gas, hydrogen and oxygen is 1:1: 1.5.
Preferably, the pH of the solution is controlled to 8 when the solid particles are dissolved in a suitable amount of water.
The invention also provides application of the siliceous inorganic nano-penetration protective coating prepared by the preparation method in the aspect of concrete structure protection.
Preferably, the mass fraction of the solute in the protective coating is 20-25%.
The invention has the following beneficial effects:
1. the siliceous inorganic nano penetration type protective coating can react with alkaline substances in concrete to form silicon crystals which are firmly embedded into pores of a concrete structure to form an inseparable shielding layer, so that the compactness of the surface of the concrete is enhanced, and the silicon crystals are hard and play a role in reinforcing the concrete structure.
2. The coating has the advantages that the main material is nano-scale, small in size and strong in permeability, can fill capillary pores in concrete materials, and has performance such as freeze-thaw resistance, acid and alkali resistance, chloride ion absorption reduction rate and the like which are improved by 20-50% compared with the existing common protective materials such as silane and the like, and the protective effect is good;
3. the coating has a large specific surface area of a main material, can improve the comprehensive performance of a concrete interface and optimize an interface structure, and has good cohesiveness and strong durability with inorganic and organic materials;
4. the preparation method and the construction process of the invention are simple, have low cost, do not contain heavy metal, are nontoxic, nonflammable, nonvolatile, and harmless to the construction environment;
5. the protective coating prepared by the invention has the advantages of small dosage, high efficiency, environmental protection and the like. Compared with other products, the protective coating has better protective effect on the coating.
Detailed Description
The production method of the present invention is explained in detail below.
The preparation method of the siliceous inorganic nano-penetration type protective coating for the concrete structure comprises the following steps:
mixing hydrogen and oxygen according to the volume ratio of 1:1.5, pressurizing, drying, removing impurities, and introducing into a sodium silicate solution in a first reaction kettle;
and (3) the silicon tetrachloride liquid is subjected to dehydration, rectification and molecular sieve treatment to obtain silicon tetrachloride gas containing a small amount of peroxide (the temperature is maintained above the boiling point of silicon tetrachloride after the molecular sieve treatment). In the step, the content of silicon tetrachloride in the gas chromatography is not less than 99.9 wt%, and the content of peroxide is not more than 0.1 wt%. The small amount of peroxide is generated through side reaction and is obtained by reacting silicon tetrachloride with water and oxygen.
And (3) sending the silicon tetrachloride gas containing a small amount of peroxide to the sodium silicate solution in the first reaction kettle. The volume ratio of the silicon tetrachloride gas to the hydrogen to the oxygen is (1-1.5): 1: 1.5. in the process, the flow rates of silicon tetrachloride gas, hydrogen and oxygen are controlled, the specific flow rates are determined by equipment and the feeding amount, the feeding ratio and the equipment pressure are ensured, the heating temperature is controlled at 1500 ℃, the pressure is controlled at 1.8-2.0 Mpa, and the reaction time is 30 minutes.
In the above process, sodium silicate is used in an excess amount, an excess of 30 wt% being suggested. In one embodiment of the invention, the molar ratio of silicon tetrachloride gas, hydrogen and oxygen is 1:1: 1.5.
The following reactions take place in the first reaction vessel:
SiCl4+2H2O＝SiO2+4HCl,
Na2SiO3+2HCl＝H2SiO3+2NaCl,
H2SiO3＝SiO2+H2O，
the product silica is obtained.
And then, replacing gas in the reaction kettle with pure air (only by keeping the safety pressure of the reaction kettle), introducing the product in the first reaction kettle into an alkaline washing tower and a drying tower in sequence, removing organic matters and water in the product, and then sending the product into a second reaction kettle.
And adding ethanol into the second reaction kettle. In one embodiment of the invention, the product: the mass ratio of ethanol is 1:3, and mixing by using ultrasonic waves. Heating the second reaction kettle to 80 ℃, slowly introducing a gamma-methacryloxypropyltrimethoxysilane (gamma-MAPS) solution (the solvent is a miscible organic solvent, and alcohols are adopted in the embodiment of the invention), treating for 1-1.5 hours, and performing crystal form control.
And then, sequentially introducing the product in the second reaction kettle into a cyclone separator, a washing tower and a drying tower to obtain solid particles with the particle size of 10-20 nm.
According to the construction requirement, the solid particles are dissolved in a proper amount of water to obtain the siliceous inorganic nano penetration type protective coating.
The siliceous inorganic nano-penetration protective coating can be used for the protective treatment of concrete structures. Preferably, the mass fraction of the solute in the protective coating is 20-25%. When the solid particles are dissolved in an appropriate amount of water, the pH of the solution is controlled to 8.
When the protective coating is used, the coating is coated on the surface of a material to be protected and dried.
The performance test results of the siliceous inorganic nano-penetration type concrete structure protective coating prepared according to one embodiment of the invention are shown in the following table:
from the test data in the table above, it can be seen that:
1. the siliceous inorganic nano-permeable concrete structure protective coating can be firmly embedded into pores of a concrete structure to form an inseparable shielding layer, so that the compactness of the surface of the concrete is enhanced, and the concrete structure is reinforced;
2. the coating has good performance of freeze thawing resistance, acid and alkali resistance, chloride ion absorption reduction rate and the like, so that the coating has good protection effect;
3. the coating has good acid and alkali resistance, and can not generate surface pulverization and crack after long-term use.
Claims (10)
1. A preparation method of siliceous inorganic nano-penetration type protective coating for concrete structure comprises the following steps:
mixing hydrogen and oxygen according to the volume ratio of 1:1.5, and introducing the mixture into a sodium silicate solution in a first reaction kettle;
carrying out water removal, rectification and molecular sieve treatment on the silicon tetrachloride liquid to obtain silicon tetrachloride gas containing a small amount of peroxide;
introducing the silicon tetrachloride gas containing a small amount of peroxide into a sodium silicate solution in the first reaction kettle, wherein the molar ratio of the silicon tetrachloride gas to hydrogen to oxygen is (1-1.5) to 1:1.5, controlling the flow rates of the silicon tetrachloride gas to hydrogen to oxygen, controlling the heating temperature to 1500 ℃, controlling the pressure to be 1.8-2.0 Mpa, and keeping the reaction time for 30 minutes;
introducing pure air into the first reaction kettle, replacing the gas in the reaction kettle and keeping the safety pressure of the reaction kettle;
sequentially introducing a reaction product in the first reaction kettle into an alkaline washing tower and a drying tower, then conveying the reaction product to a second reaction kettle, adding ethanol into the second reaction kettle, enabling the mass ratio of the reaction product to the ethanol to be 1:3, mixing the reaction product and the ethanol by adopting ultrasonic waves, then heating to 80 ℃, slowly introducing a gamma-methacryloxypropyltrimethoxysilane solution, reacting for 1-1.5 hours, and controlling the crystal form;
performing cyclone separation, washing and drying on the product in the second reaction kettle to obtain solid particles;
and (3) dissolving the solid particles in a proper amount of water according to construction requirements to obtain the inorganic nano permeable protective coating.
2. The method of claim 1, wherein: the content of peroxide in the silicon tetrachloride gas is less than or equal to 0.1 wt%.
3. The method of claim 1, wherein: and in the process of rectifying the silicon tetrachloride liquid, rectifying and purifying the distilled components for 2-3 times.
4. The method of claim 1, wherein: and after the mixed gas of the hydrogen and the oxygen is introduced into the first reaction kettle and blown for 30 minutes, introducing the silicon tetrachloride gas containing a small amount of peroxide into the sodium silicate solution in the first reaction kettle.
5. The method of claim 1, wherein: the hydrogen and the oxygen are pressurized, dried and subjected to impurity removal before being mixed.
6. The method of claim 1, wherein: the gamma-methacryloxypropyltrimethoxysilane solution is an alcoholic solution of gamma-methacryloxypropyltrimethoxysilane.
7. The method of claim 1, wherein: the molar ratio of the silicon tetrachloride gas to the hydrogen to the oxygen is 1:1: 1.5.
8. The method of claim 1, wherein: when the solid particles are dissolved in an appropriate amount of water, the pH of the solution is controlled to 8.
9. The application of the siliceous inorganic nano-penetration protective coating prepared by the preparation method of any one of claims 1 to 8 in the protection of concrete structures.
10. Use according to claim 9, characterized in that: the mass fraction of solute in the protective coating is 20-25%.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1590292A (en) * | 2004-06-10 | 2005-03-09 | 江南大学 | Chemical gas phase sedimentation preparation method of nano silicone dioxide |
| CN101117281A (en) * | 2006-08-04 | 2008-02-06 | 朱珦珦 | Concrete protection sol |
| CN103964892A (en) * | 2014-04-29 | 2014-08-06 | 青岛理工大学 | Silica sol-organosilicone monomer capillary crystalline waterproof material and preparation method thereof |
| CN106634241A (en) * | 2016-12-14 | 2017-05-10 | 山东电力建设第工程公司 | Coating for prolonging service life of concrete wall surface |
| CN109912248A (en) * | 2019-02-27 | 2019-06-21 | 詹仰东 | A kind of nano modification silicate penetration crystalline material and its application method |
| CN109988443A (en) * | 2019-04-01 | 2019-07-09 | 傅自豪 | A kind of environment protection multifunctional inorganic dry powder painting and its application method |
-
2021
- 2021-01-04 CN CN202110004964.3A patent/CN112831201B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1590292A (en) * | 2004-06-10 | 2005-03-09 | 江南大学 | Chemical gas phase sedimentation preparation method of nano silicone dioxide |
| CN101117281A (en) * | 2006-08-04 | 2008-02-06 | 朱珦珦 | Concrete protection sol |
| CN103964892A (en) * | 2014-04-29 | 2014-08-06 | 青岛理工大学 | Silica sol-organosilicone monomer capillary crystalline waterproof material and preparation method thereof |
| CN106634241A (en) * | 2016-12-14 | 2017-05-10 | 山东电力建设第工程公司 | Coating for prolonging service life of concrete wall surface |
| CN109912248A (en) * | 2019-02-27 | 2019-06-21 | 詹仰东 | A kind of nano modification silicate penetration crystalline material and its application method |
| CN109988443A (en) * | 2019-04-01 | 2019-07-09 | 傅自豪 | A kind of environment protection multifunctional inorganic dry powder painting and its application method |
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