CN108247820B - Magnesium oxychloride cement with super-hydrophobic surface and nano-casting preparation process thereof - Google Patents
Magnesium oxychloride cement with super-hydrophobic surface and nano-casting preparation process thereof Download PDFInfo
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- CN108247820B CN108247820B CN201810046131.1A CN201810046131A CN108247820B CN 108247820 B CN108247820 B CN 108247820B CN 201810046131 A CN201810046131 A CN 201810046131A CN 108247820 B CN108247820 B CN 108247820B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B7/00—Moulds; Cores; Mandrels
- B28B7/36—Linings or coatings, e.g. removable, absorbent linings, permanent anti-stick coatings; Linings becoming a non-permanent layer of the moulded article
- B28B7/364—Linings or coatings, e.g. removable, absorbent linings, permanent anti-stick coatings; Linings becoming a non-permanent layer of the moulded article of plastic material or rubber
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
- B28B11/245—Curing concrete articles
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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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/30—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing magnesium cements or similar cements
- C04B28/32—Magnesium oxychloride cements, e.g. Sorel cement
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- Ceramic Engineering (AREA)
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Abstract
The invention discloses magnesium oxychloride cement with a super-hydrophobic surface and a nano-casting preparation process thereof, belonging to the technical field of preparation of functional cement-based materials. The invention firstly proposes to prepare a material with a special pore structure on the surface in a nano-scale range as a template, introduce a magnesium oxychloride cement precursor into pores of the material, and finally obtain the magnesium oxychloride cement with the super-hydrophobic surface and the controllable microstructure by utilizing the nano-confinement effect of the template material and combining the hydration growth process of the cement. On the premise of ensuring the internal structure, strength, wear resistance and other service performances of the magnesium oxychloride cement, the invention successfully constructs the super-hydrophobic structure on the surface of the magnesium oxychloride cement, the static contact angle of the surface can reach 142 degrees, water can freely flow on the surface of the product without wetting, and the water resistance of the product can be effectively improved.
Description
Technical Field
The invention belongs to the technical field of functional cement-based materials, and particularly relates to magnesium oxychloride cement with a super-hydrophobic surface and a nano-casting preparation process thereof.
Background
The magnesium oxychloride cement is a new type of magnesian air-hardening gelled material formed by mixing light-burned magnesium oxide and magnesium chloride aqueous solution according to a certain proportion. The magnesium oxychloride cement has incomparable advantages compared with the common Portland cement: 1) the production process is simple, sintering and drying are not needed, energy consumption is reduced, and the material belongs to a green environment-friendly material; 2) the setting and hardening speed is high; 3) the adhesive property is excellent, and the adhesive has good adhesive force with some organic or inorganic aggregates; 4) the wear resistance and corrosion resistance are good, the wear resistance of the magnesium cement is 3 times of that of the common portland cement, the filtrate of the magnesium cement slurry is alkalescent, and common metal materials can be corroded by the filtrate; 5) good heat insulation and flame retardance, the heat conductivity coefficient of the magnesium cement is only 0.14-0.23W/(m.k), and the raw materials of the magnesium cement are MgO and MgCl2Are non-flammable, thus giving it good flame retardancy. Although the magnesium oxychloride cement has been used in construction and decoration fields due to its advantages, its water resistance is also very bad, especially for common magnesiteThe 28d strength of the magnesium product is lost by 70-80% after being soaked in water, which limits the further development and breakthrough of the magnesium product in the fields of buildings and the like.
The main methods for improving the poor water resistance of magnesium oxychloride cement at present comprise: 1) adding a modified water repellent agent; 2) and coating the outer layer of the waterproof coating. Although the water resistance of the magnesium oxychloride cement can be improved to different degrees by the incorporation of organic, inorganic and other composite modifiers, the other properties of the magnesium oxychloride cement can be influenced to different degrees by the introduction of the modifiers. Although the method for coating the outer layer of the waterproof coating can greatly improve the water resistance of the waterproof coating, the waterproof coating is greatly restricted by the environmental temperature, the mechanical property of the coating is influenced by the molding environmental temperature and the temperature, the flatness of the base surface is influenced, the thickness of the coating is uneven, most of waterproof coating materials contain organic matters, and some of the waterproof coating materials are even toxic and can seriously pollute the environment.
Disclosure of Invention
The invention aims to solve the problems that the water resistance of magnesium oxychloride cement is poor, the service performance of the magnesium oxychloride cement is easily influenced or the magnesium oxychloride cement is restricted by the environmental temperature by the existing modification or protection method, and the like, and provides the magnesium oxychloride cement with the super-hydrophobic surface and the preparation method thereof, wherein a nano casting method is adopted to combine the hydration characteristics of the magnesium oxychloride cement to construct a super-hydrophobic structure on the surface of the magnesium oxychloride cement, and the water resistance of the magnesium oxychloride cement is effectively improved on the premise of ensuring the service performances such as the internal structure, the strength, the wear resistance and the like of the magnesium oxychloride; and the related preparation process is extremely simple, has low requirements on equipment, and is suitable for popularization and application.
In order to achieve the purpose, the invention adopts the technical scheme that:
the magnesium oxychloride cement with super-hydrophobic surface is prepared by adopting a nano casting method and combining the hydration characteristics of magnesium oxychloride cement to construct a super-hydrophobic structure on the surface of the magnesium oxychloride cement.
In the scheme, the contact angle of the super-hydrophobic surface is 124-142 degrees, and the minimum contact angle hysteresis reaches 3 degrees.
In the above scheme, the nano-casting method mainly comprises the following steps: the nano-casting method mainly comprises the following steps: uniformly coating silica gel on the surface of the sand paper, solidifying and drying, and removing the sand paper to obtain a silica gel template with a sand paper negative film structure; and placing the silica gel template in a mold, enabling one surface with the sand paper negative film structure to face the direction of the slurry to be cast, pouring magnesium oxychloride cement slurry into the mold with the silica gel template, and molding and maintaining to obtain the magnesium oxychloride cement with the super-hydrophobic surface.
In the scheme, the magnesium oxychloride cement paste is prepared from a magnesium chloride solution with the mass concentration of 20-29% and light-burned magnesia.
The nano-casting preparation process of the magnesium oxychloride cement with the super-hydrophobic surface comprises the following steps:
1) preparing a silica gel template; blending silica gel and a curing agent to obtain silica gel, uniformly coating the silica gel on the surface of abrasive paper, drying, removing the abrasive paper, and then carrying out ultrasonic cleaning and drying to obtain a silica gel template with an abrasive paper negative film structure;
2) assembling a mould; placing the obtained silica gel template in a double-layer mold, enabling one surface with a sand paper negative film structure to face the direction of the slurry to be cast, and clamping the mold;
3) pouring and forming; pouring and forming; preparing magnesium oxychloride cement paste, pouring the magnesium oxychloride cement paste into a mold provided with a silica gel template, and molding and protecting with oxygen to obtain the magnesium oxychloride cement with the super-hydrophobic surface.
In the scheme, the mass ratio of the silica gel to the curing agent is 50-10: 1.
In the above scheme, the silica gel is a mold silica gel; the curing agent is a silica gel curing agent.
In the scheme, the sand paper can be common waterproof sand paper.
Preferably, the sand paper can be selected to have the mesh number of 150 and 1000.
More preferably, the sandpaper is No.240(240 mesh), and the super-hydrophobic surface contact angle of the magnesium oxychloride cement prepared under the condition of the sandpaper is 142 degrees, and the contact angle hysteresis is 3 degrees.
In the scheme, the magnesium oxychloride cement paste is prepared from a magnesium chloride solution with the mass concentration of 20-28.9% and light-burned magnesium oxide according to the mass ratio of (2-1) to 1.
Preferably, the mass ratio of the magnesium chloride solution to the light-burned magnesium oxide is (1.01-1.15): 1.
The magnesium oxychloride cement with the super-hydrophobic surface prepared according to the scheme has the surface contact angle of 142 degrees and the minimum contact angle retardation of 3 degrees, and water drops can slide on the surface of a product without wetting; the contact angle delays the difference value of the advancing rolling angle and the retreating rolling angle, and the super-hydrophobic surface is generally below 5 degrees, so that the water drop slides freely.
The principle of the invention is as follows: the invention realizes the basic molding of the surface of the magnesium oxychloride cement by utilizing the nanometer confinement function of the silica gel template, and then combines the 518-phase needle-rod-shaped structure of the magnesium oxychloride cement formed in the hydration process in the formed nanometer convex area to finally form a multi-level composite coarse structure, thereby realizing the construction of the super-hydrophobic functional structure on the surface of the hydrophilic inorganic material and effectively ensuring the internal structure, the strength, the wear resistance and other service performances of the magnesium oxychloride cement.
Compared with the prior art, the invention has the beneficial effects that:
1) the invention firstly proposes that a super-hydrophobic surface is constructed on the surface of the magnesium oxychloride cement product by combining the hydration characteristics of the magnesium oxychloride cement by adopting a nano casting method, can effectively improve the water resistance of the magnesium oxychloride cement product on the premise of ensuring the internal structure and the service performances such as strength, wear resistance and the like, and provides a brand new idea for improving the problem of poor water resistance of the magnesium oxychloride cement.
2) The method comprises the steps of taking sand paper with larger surface roughness as a primary template, coating silica gel on the surface of the sand paper, solidifying and separating to obtain the silica gel template with a sand paper negative film structure, then taking the sand paper negative film structure as a secondary template, casting magnesium oxychloride cement paste, and constructing a multi-stage composite coarse structure on the surface of magnesium oxychloride cement by utilizing the nano confinement effect of a template material and combining the hydration growth process of the cement, wherein the multi-stage composite coarse structure can show excellent super-hydrophobic performance.
3) The preparation process is simple and controllable, and can be used for producing products with large super-hydrophobic surfaces and can be quickly designed and produced according to specific requirements.
4) The raw materials related by the invention are wide in source, the silica gel template can be repeatedly recycled, and the cost is saved; the preparation method is simple, has good repeatability and is suitable for popularization and application.
Detailed Description
For further understanding of the present invention, embodiments of the present invention will be described below with reference to specific examples, but the scope of the present invention is not limited to these examples.
In the following examples, the mold silica gel and the silica gel curing agent are both provided by Zhili materials science and technology Limited, Shenzhen.
Example 1
The preparation method of the magnesium oxychloride cement with the super-hydrophobic surface comprises the following steps:
1) preparing 80g of silica gel from the mold silica gel and a curing agent according to the mass ratio of 50: 1; spreading 230 x 280mm No.240(240 mesh) sand paper on plate glass, uniformly coating the prepared silica gel on the surface of the sand paper, separating after 24 hours to obtain a silica gel template, and ultrasonically cleaning and drying;
2) placing the obtained silica gel template in a double-layer mold, enabling one surface with a sand paper negative film structure to face the direction of the slurry to be cast, and tightly clamping an upper layer of grinding tool and a lower layer of grinding tool of the mold;
3) preparing a magnesium chloride solution with the mass concentration of 28.92%, uniformly stirring 304.36g of the magnesium chloride solution and 300g of light-burned magnesium oxide in a beaker to obtain magnesium oxychloride cement slurry, then pouring the magnesium oxychloride cement slurry into a grinding tool, curing at room temperature for 1d, then taking down the grinding tool on the upper layer, continuing curing at room temperature for 7 days, and taking out to obtain the magnesium oxychloride cement with the super-hydrophobic surface.
And (3) taking 10 interfaces of the obtained magnesium oxychloride cement product with the super-hydrophobic surface to perform static water contact angle test, and measuring that the contact angle is 142 degrees and the contact angle hysteresis is 3 degrees.
The strength loss of the obtained magnesium oxychloride cement product with the super-hydrophobic surface after the 28d strength is 5% after soaking in water.
Example 2
The preparation method of the magnesium oxychloride cement with the super-hydrophobic surface comprises the following steps:
1) preparing 80g of silica gel from the mold silica gel and a curing agent according to the mass ratio of 50: 1; spreading 230 x 280mm W10 sand paper (1000 mesh) on plate glass, uniformly coating the prepared silica gel on the surface of the sand paper, separating after 24 hours to obtain a silica gel template, and ultrasonically cleaning and airing the silica gel template;
2) placing the obtained silica gel template in a double-layer mold, enabling one surface with a sand paper negative film structure to face the direction of the slurry to be cast, and tightly clamping an upper layer of grinding tool and a lower layer of grinding tool of the mold;
3) preparing a magnesium chloride solution with the mass concentration of 28.92%, uniformly stirring 304.36g of the magnesium chloride solution and 300g of light-burned magnesium oxide in a beaker to obtain magnesium oxychloride cement slurry, then pouring the magnesium oxychloride cement slurry into a grinding tool, curing at room temperature for 1d, then taking down the grinding tool on the upper layer, continuing curing at room temperature for 7 days, and taking out to obtain the magnesium oxychloride cement with the super-hydrophobic surface.
And (3) taking 10 interfaces of the obtained magnesium oxychloride cement product with the super-hydrophobic surface to perform static water contact angle test, and measuring that the contact angle is 128 degrees and the contact angle hysteresis is 7 degrees.
The strength loss of the obtained magnesium oxychloride cement product with the super-hydrophobic surface after 28d strength is 8% after soaking in water.
Example 3
The preparation method of the magnesium oxychloride cement with the super-hydrophobic surface comprises the following steps:
1) preparing 80g of silica gel from the mold silica gel and a curing agent according to the mass ratio of 50: 1; spreading 230 x 280mm NO.600 sand paper (600 mesh) on plate glass, uniformly coating the prepared silica gel on the surface of the sand paper, separating after 24 hours to obtain a silica gel template, and ultrasonically cleaning and airing the silica gel template;
2) placing the obtained silica gel template in a double-layer mold, enabling one surface with a sand paper negative film structure to face the direction of the slurry to be cast, and tightly clamping an upper layer of grinding tool and a lower layer of grinding tool of the mold;
3) preparing a magnesium chloride solution with the mass concentration of 28.92%, uniformly stirring 304.36g of the magnesium chloride solution and 300g of light-burned magnesium oxide in a beaker to obtain magnesium oxychloride cement slurry, then pouring the magnesium oxychloride cement slurry into a grinding tool, curing at room temperature for 1d, then taking down the grinding tool on the upper layer, continuing curing at room temperature for 7 days, and taking out to obtain the magnesium oxychloride cement with the super-hydrophobic surface.
And (3) taking 10 interfaces of the obtained magnesium oxychloride cement product with the super-hydrophobic surface to perform static water contact angle test, and measuring that the contact angle is 126 degrees and the contact angle hysteresis is 7 degrees.
The resulting magnesium oxychloride cement product with a superhydrophobic surface exhibited a 28d strength loss of 8% upon immersion in water.
Example 4
The preparation method of the magnesium oxychloride cement with the super-hydrophobic surface comprises the following steps:
1) preparing 80g of silica gel from the mold silica gel and a curing agent according to the mass ratio of 50: 1; spreading 230 x 280mm NO.360 sand paper (360 meshes) on flat glass, uniformly coating the prepared silica gel on the surface of the sand paper, separating after 24 hours to obtain a silica gel template, and ultrasonically cleaning and airing the silica gel template;
2) placing the obtained silica gel template in an upper and a lower double-layer molds, enabling one surface with a sand paper negative film structure to face the direction of the slurry to be cast, and tightly clamping the upper and the lower layers of molds;
3) preparing a magnesium chloride solution with the mass concentration of 28.92%, uniformly stirring 304.36g of the magnesium chloride solution and 300g of light-burned magnesium oxide in a beaker to obtain magnesium oxychloride cement slurry, then pouring the magnesium oxychloride cement slurry into a grinding tool, curing at room temperature for 1d, then taking down the grinding tool on the upper layer, continuing curing at room temperature for 7 days, and taking out to obtain the magnesium oxychloride cement with the super-hydrophobic surface.
And (3) taking 10 interfaces of the obtained magnesium oxychloride cement product with the super-hydrophobic surface to perform static water contact angle test, and measuring that the contact angle is 136 degrees and the contact angle hysteresis is 4 degrees.
The 28d strength of the obtained magnesium oxychloride cement product with the super-hydrophobic surface loses 6 percent of the strength after being soaked in water.
Example 5
The preparation method of the magnesium oxychloride cement with the super-hydrophobic surface comprises the following steps:
1) preparing 80g of silica gel from the mold silica gel and a curing agent according to the mass ratio of 50: 1; spreading 230 x 280mm NO.240 sand paper (240 meshes) on flat glass, uniformly coating the prepared silica gel on the surface of the sand paper, separating after 24 hours to obtain a silica gel template, and ultrasonically cleaning and airing the silica gel template;
2) placing the obtained silica gel template in a double-layer mold, enabling one surface with a sand paper negative film structure to face the direction of the slurry to be cast, and tightly clamping an upper layer of grinding tool and a lower layer of grinding tool of the mold;
3) preparing a magnesium chloride solution with the mass concentration of 28.92%, uniformly stirring 320.36g of the magnesium chloride solution and 280g of light-burned magnesium oxide in a beaker to obtain magnesium oxychloride cement slurry, then pouring the magnesium oxychloride cement slurry into a grinding tool, curing at room temperature for 1d, then taking down the grinding tool on the upper layer, continuing curing at room temperature for 7 days, and taking out to obtain the magnesium oxychloride cement with the super-hydrophobic surface.
And (3) taking 10 interfaces of the obtained magnesium oxychloride cement product with the super-hydrophobic surface to perform static water contact angle test, and measuring that the contact angle is 125 degrees and the contact angle hysteresis is 8 degrees.
The 28d strength of the obtained magnesium oxychloride cement product with the super-hydrophobic surface loses 8 percent of the strength after being soaked in water.
Example 6
The preparation method of the magnesium oxychloride cement with the super-hydrophobic surface comprises the following steps:
1) preparing 80g of silica gel from the mold silica gel and a curing agent according to the mass ratio of 50: 1; spreading 230 x 280mm NO.240 sand paper (240 meshes) on flat glass, uniformly coating the prepared silica gel on the surface of the sand paper, separating after 24 hours to obtain a silica gel template, and ultrasonically cleaning and airing the silica gel template;
2) placing the obtained silica gel template in a double-layer mold, enabling one surface with a sand paper negative film structure to face the direction of the slurry to be cast, and tightly clamping an upper layer of grinding tool and a lower layer of grinding tool of the mold;
3) preparing a magnesium chloride solution with the mass concentration of 28.92%, uniformly stirring 280g of the magnesium chloride solution and 320g of light-burned magnesium oxide in a beaker to obtain magnesium oxychloride cement paste, then pouring the magnesium oxychloride cement paste into a grinding tool, curing at room temperature for 1d, then taking down the grinding tool on the upper layer, continuing curing at room temperature for 7 days, and taking out to obtain the magnesium oxychloride cement with the super-hydrophobic surface.
And (3) taking 10 interfaces of the obtained magnesium oxychloride cement product with the super-hydrophobic surface to perform static water contact angle test, and measuring that the contact angle is 124 degrees and the contact angle hysteresis is 8 degrees.
The 28d strength of the obtained magnesium oxychloride cement product with the super-hydrophobic surface loses 8 percent of the strength after being soaked in water.
Comparative example 1
The magnesium oxychloride cement paste obtained in example 1 was directly cast using 240 mesh (240 mesh) sandpaper as a template, and the upper layer abrasive was removed after 1 day of curing at room temperature, so that effective demolding could not be performed.
Comparative example 2
Ordinary portland cement is used to replace the magnesium oxychloride cement paste in the comparative example 1, the upper layer grinding tool is taken down after the curing is carried out for 1d at room temperature, the curing is carried out for 7 days at room temperature, the contact angle of the surface of the obtained portland cement is lower than 20 degrees, and the obtained portland cement basically cannot exert hydrophobic property.
The above description is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various modifications and concepts without departing from the inventive concept of the present invention, and all such modifications and concepts fall within the scope of the present invention.
Claims (8)
1. The magnesium oxychloride cement with the super-hydrophobic surface is characterized in that a super-hydrophobic structure is constructed on the surface of the magnesium oxychloride cement by adopting a nano casting method;
the nano-casting method mainly comprises the following steps: uniformly coating the silica gel on the surface of the abrasive paper, curing and drying, and removing the abrasive paper to obtain a silica gel template with a sand paper negative film structure; and placing the silica gel template in a mold, enabling one surface with the sand paper negative film structure to face the direction of the slurry to be cast, pouring magnesium oxychloride cement slurry into the mold with the silica gel template, and molding and maintaining to obtain the magnesium oxychloride cement with the super-hydrophobic surface.
2. The magnesium oxychloride cement of claim 1, wherein the contact angle of the super-hydrophobic surface is 124-142 °, and the contact angle hysteresis is at least 3 °.
3. The nano-casting preparation process of magnesium oxychloride cement with a super-hydrophobic surface as claimed in claim 1 or 2, which is characterized by comprising the following steps:
1) preparing a silica gel template; blending silica gel and a curing agent to obtain silica gel, then uniformly coating the silica gel on the surface of abrasive paper, removing the abrasive paper after drying, and carrying out ultrasonic cleaning and drying to obtain a silica gel template with a negative film structure of the abrasive paper;
2) assembling a mould; placing the obtained silica gel template in a double-layer mold, and enabling one surface with a sand paper negative film structure to face the direction of the slurry to be cast, and clamping the mold;
3) pouring and forming; preparing magnesium oxychloride cement paste, pouring the magnesium oxychloride cement paste into a mold provided with a silica gel template, and molding and maintaining the magnesium oxychloride cement paste to obtain the magnesium oxychloride cement with the super-hydrophobic surface.
4. The nano-casting preparation process according to claim 3, wherein the mass ratio of the silica gel to the curing agent is 50-10: 1.
5. The nano-casting preparation process according to claim 3, wherein the silica gel is a mold silica gel; the curing agent is a silica gel curing agent.
6. The nano-casting preparation process of claim 3, wherein the sandpaper is water-resistant sandpaper.
7. The nano-casting preparation process according to claim 3, wherein the magnesium oxychloride cement paste is prepared from a magnesium chloride solution with a mass concentration of 20-29% and light-burned magnesium oxide according to a mass ratio of (2-1): 1.
8. The nano-casting preparation process according to claim 7, wherein the mass ratio of the magnesium chloride solution to the light-burned magnesium oxide is (1.01-1.15): 1.
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