CN112892507A - Device and method for preparing film-covered self-healing material - Google Patents

Device and method for preparing film-covered self-healing material Download PDF

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Publication number
CN112892507A
CN112892507A CN202110066898.2A CN202110066898A CN112892507A CN 112892507 A CN112892507 A CN 112892507A CN 202110066898 A CN202110066898 A CN 202110066898A CN 112892507 A CN112892507 A CN 112892507A
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self
healing material
adsorption
film
hollow connecting
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CN112892507B (en
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王险峰
杜冠宏
陈少聪
朱继华
邢锋
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Shenzhen University
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Shenzhen University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/32Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3202Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
    • B01J20/3204Inorganic carriers, supports or substrates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/10Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/16Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the fluid carrier
    • B01D15/163Pressure or speed conditioning
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/10Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/20Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/006Coating of the granules without description of the process or the device by which the granules are obtained
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/32Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3214Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the method for obtaining this coating or impregnating
    • B01J20/3225Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the method for obtaining this coating or impregnating involving a post-treatment of the coated or impregnated product
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/32Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3234Inorganic material layers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/32Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3287Layers in the form of a liquid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/32Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3291Characterised by the shape of the carrier, the coating or the obtained coated product
    • B01J20/3293Coatings on a core, the core being particle or fiber shaped, e.g. encapsulated particles, coated fibers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/006Processes utilising sub-atmospheric pressure; Apparatus therefor

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Materials For Medical Uses (AREA)

Abstract

The invention relates to the technical field of preparation and film covering of self-healing materials, and provides a device for preparing a film-covered self-healing material. The device for laminating the self-healing material provided by the invention can be used for preparing the self-healing material and laminating the prepared self-healing material, is simple and easy to obtain, and can greatly reduce the investment of equipment funds for preparing and laminating the self-healing material. Experimental results show that when the device provided by the invention is used for preparing the self-healing material, the adsorption capacity can reach more than 90% of the maximum adsorption capacity of the carrier. The film coating device for the self-healing material provided by the invention can obtain a film layer of 78.5 microns after coating the self-healing material, and can effectively prevent ions in the self-healing material solution from diffusing.

Description

Device and method for preparing film-covered self-healing material
Technical Field
The invention relates to the technical field of preparation and film covering of self-healing materials, in particular to a device and a method for preparing a film-covered self-healing material.
Background
Concrete is one of the most widely used building materials in the world today. However, the tensile strength of concrete is limited, cracks are easy to appear in the using process, once the concrete starts to generate micro cracks and expands towards macro cracks, the building appearance is influenced, and the bearing capacity of the concrete structure is reduced. And the crack provides a channel into the concrete to accelerate the invasion of aggressive substances such as chloride ions, sulfate ions, carbon dioxide and the like, which accelerates the carbonization and steel bar corrosion of the concrete, further leads to over-expansion, reduces the structural durability and greatly shortens the service life of the concrete. Therefore, the concept of self-healing concrete has been proposed. When the concrete cracks, the self-repairing system embedded in the concrete can automatically repair the cracks, and the whole functionality of the structure is partially recovered and even improved.
The ceramsite has a porous structure and has the property of storing and slowly releasing adsorbed substances. Research shows that the ceramsite is used for adsorbing the self-repairing material and is used as a carrier of the self-repairing material, so that a large amount of loss of the self-repairing material before cracks appear is reduced, and the healing capacity of the self-repairing material is fully exerted. However, the existing self-repairing means based on ceramsite as a carrier of the self-healing material still has certain defects. Firstly, although ceramsite has better adsorption capacity compared with other aggregates as a lightweight aggregate, the self-repairing material preserved by the existing natural soaking adsorption is still limited. Secondly, the ceramsite adsorbing the self-healing material still has the property of slowly releasing adsorbed substances, and the existing technology is used for coating the ceramsite so as to better retain the self-healing material until cracks are spread; the prior art, for example, chinese patent CN 110227793 discloses a film covering device, which needs to mix and heat raw sand and each film covering material in a sand mixer, and needs to use an expensive device, and the operation method is complicated. Therefore, a device for preparing a film-covered self-healing material, which can enable the ceramsite to sufficiently adsorb the self-healing material, is needed.
Disclosure of Invention
The invention aims to provide a device and a method for preparing a film covering self-healing material. The device provided by the invention can be used for preparing the self-healing material and also can be used for coating the prepared self-healing material.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a device for preparing a film-covered self-healing material, which comprises a detachable adsorption device and a film covering device;
the adsorption device comprises a vacuum component and an adsorption component;
the adsorption component comprises a vacuum gas-pumping head, a top cover, a hollow connecting device and a circular groove which are sequentially arranged from top to bottom;
the upper end of the vacuum pumping head is connected with the vacuum assembly through a hose;
the bottom of the hollow connecting device is provided with a gauze;
the hollow connecting device is connected with the circular groove through a rotary thread;
the film covering device comprises a placing platform and a receiving groove vertically placed below the placing platform; the receiving groove is a circular groove in the adsorption component;
the placing platform comprises a support and a hollow connecting device horizontally placed on the support, and the hollow connecting device is a hollow connecting device in the adsorption component.
Preferably, the upper end of the top cover is provided with a mouth convex groove, and the top cover is connected with the vacuum pumping head through the mouth convex groove.
Preferably, the outer wall of the hollow connecting means and the inner wall of the circular groove are provided with mutually engaging rotary threads.
The invention also provides a preparation method of the film-covered self-healing material, the device adopting the technical scheme is prepared, and the preparation method comprises the following steps:
(1) placing the carrier and the self-repairing material solution in a circular groove of an adsorption device;
(2) the round groove and the hollow connecting device are connected through the rotary screw threads, so that the gauze is positioned below the liquid level of the self-repairing material solution;
(3) coating sealing materials on contact surfaces of the vacuum air pumping head, the top cover with the opening convex groove and the hollow connecting device for sealing, and performing air pumping by using a vacuum assembly for adsorption to obtain a self-healing material;
(4) disassembling the hollow connecting device of the adsorption device and assembling the circular groove into a laminating device, and flatly paving the self-healing material prepared in the step (3) on the gauze in the laminating device;
(5) and pouring the film coating material on the self-healing material for film coating to obtain the film coating self-healing material.
Preferably, the carrier in step (1) comprises one or more of ceramsite, pumice, expanded perlite and zeolite.
Preferably, the self-healing material solution in the step (1) includes one or more of a potassium carbonate solution, an ammonium carbonate solution and a potassium silicate solution.
Preferably, the mass concentration of the self-repairing material solution is 10-20%.
Preferably, the pore size of the gauze in the step (2) is smaller than the particle size of the carrier in the step (1).
Preferably, the step (5) is repeated to pour the coating material on the self-healing material, and the coating operation is performed to prepare the coating self-healing material with different coating thicknesses.
Preferably, the coating material in the step (5) includes epoxy resin or polyvinyl alcohol.
The invention provides a device for preparing a film-covered self-healing material, which comprises a detachable adsorption device and a film covering device; the adsorption device comprises a vacuum component and an adsorption component; the adsorption component comprises a vacuum gas-pumping head, a top cover, a hollow connecting device and a circular groove which are sequentially arranged from top to bottom; the upper end of the vacuum pumping head is connected with the vacuum assembly through a hose; the bottom of the hollow connecting device is provided with a gauze; the hollow connecting device is connected with the circular groove through a rotary thread; the film covering device comprises a placing platform and a receiving groove vertically placed below the placing platform; the receiving groove is a circular groove in the adsorption component; the placing platform comprises a support and a hollow connecting device horizontally placed on the support, and the hollow connecting device is a hollow connecting device in the adsorption component. The device for preparing the film-coated self-healing material comprises a detachable adsorption device and a film-coated device, when the device is used for preparing the film-coated self-healing material, a hollow connecting device in an adsorption assembly is connected with a circular groove through a rotary screw thread, so that on one hand, the adsorption assembly can be ensured to form a vacuum environment after being assembled, and negative pressure is formed under the vacuum device, so that a carrier is promoted to adsorb a self-healing material solution; on the other hand, the gauze can be ensured to be soaked in the self-repairing material solution after the circular groove passes through the rotating screw thread, the carrier can be completely soaked in the self-repairing material solution by utilizing the action of the gauze, the carrier is ensured to uniformly adsorb the self-repairing material solution, and the adsorption capacity of the self-repairing material solution in the carrier can be further improved; the hollow connecting device and the circular groove in the absorption device can be used for forming the film covering device after being detached, when the film covering device is used for covering the film on the self-healing material, the self-healing material can be supported by the aid of the gauze, and the film covering of the self-healing material can be realized by means of the characteristic that redundant film covering materials can seep downwards. Experimental results show that when the device provided by the invention is used for preparing the self-healing material, the adsorption capacity can reach more than 90% of the maximum adsorption capacity of a carrier, a 78.5 micron film layer can be obtained after the self-healing material is coated, and the diffusion of ions in the self-healing material solution can be effectively prevented.
The device for laminating the self-healing material provided by the invention can be used for preparing the self-healing material, and can be assembled by utilizing the hollow connecting device and the circular groove in the device for preparing the self-healing material after the device for preparing the self-healing material is disassembled for laminating the prepared self-healing material.
Drawings
FIG. 1 is a schematic view of an adsorption assembly of an adsorption device in an apparatus for preparing a coated self-healing material according to the present invention;
in the figure, 1 is a vacuum pumping head, 2 is a top cover, 3 is a hollow connecting device, 4 is a gauze, 5 is a rotary thread, and 6 is a circular groove;
FIG. 2 is a schematic view of an apparatus for preparing a coated self-healing material according to the present invention;
in the figure, 7 is a hose, 8 is a vacuum pump, and 9 is a barometer;
FIG. 3 is a schematic view of a laminating device in the apparatus for preparing a laminated self-healing material according to the present invention;
in the figure, 3 is a hollow connecting device, 4 is a gauze, 10 is a bracket, 11 is a base, and 6 is a receiving groove;
fig. 4 is an SEM image of the coating film self-healing material prepared in example 2 of the present invention;
fig. 5 is a chlorine ion diffusion curve diagram of the film-covering self-healing material prepared in simulation example 2 of the present invention.
Detailed Description
The invention provides a device for preparing a film-covered self-healing material, which comprises a detachable adsorption device and a film covering device;
the adsorption device comprises a vacuum component and an adsorption component;
the adsorption component comprises a vacuum gas-pumping head, a top cover, a hollow connecting device and a circular groove which are sequentially arranged from top to bottom;
the upper end of the vacuum pumping head is connected with the vacuum assembly through a hose;
the bottom of the hollow connecting device is provided with a gauze;
the hollow connecting device is connected with the circular groove through a rotary thread;
the film covering device comprises a placing platform and a receiving groove vertically placed below the placing platform; the receiving groove is a circular groove in the adsorption component;
the placing platform comprises a support and a hollow connecting device horizontally placed on the support, and the hollow connecting device is a hollow connecting device in the adsorption component.
The device for preparing the film-coated self-healing material comprises a detachable adsorption device and a film-coated device.
In the present invention, the adsorption apparatus includes a vacuum assembly and an adsorption assembly.
As shown in fig. 1, in the present invention, the adsorption assembly includes a vacuum pumping head 1, a top cover 2, a hollow connection device 3, and a circular groove 6, which are sequentially disposed from top to bottom.
In the present invention, the adsorption assembly includes a vacuum pumping head 1. The type and the source of the vacuum pumping head are not specially limited, and the vacuum pumping head can be adjusted according to the use requirement.
In the invention, the upper end of the vacuum pumping head is connected with the vacuum assembly through the hose, and air in the adsorption assembly can be pumped out along the hose during the vacuum pumping.
In the present invention, the adsorption assembly includes a top cover 2 disposed below the vacuum pumping head 1. In one embodiment of the invention, the upper end of the top cover is provided with a mouth convex groove, and the top cover is connected with the vacuum pumping head through the mouth convex groove. In the invention, the top cover can be connected with the vacuum pumping head and is tightly connected with the hollow connecting device.
In the present invention, the suction assembly comprises a hollow connection means 3 arranged below the top cover 2. In one embodiment of the invention, as shown in fig. 1, the outer wall of the hollow connecting means 3 is provided 5 with a rotating thread. In the invention, the rotating threads arranged on the outer wall of the hollow connecting device are meshed with the rotating threads arranged on the inner wall of the circular groove, so that a vacuum environment can be formed after the adsorption assembly is assembled, negative pressure is formed under a vacuum device, and the adsorption of the self-repairing material solution by the carrier is promoted.
In the present invention, the suction assembly comprises a gauze 4 arranged at the bottom of the hollow connecting means 3. The type and the source of the gauze are not specially limited, and the gauze can be adjusted according to the particle size of the selected carrier when used for preparing the film-coated self-healing material, so that the diameter of the gauze is smaller than the particle size of the carrier. In the invention, when the device for preparing the self-healing material is used for preparing the self-healing material, the carrier is soaked in the self-healing material solution by the gauze.
In the present invention, the suction assembly comprises a circular groove 6 arranged below the hollow connection means 3. In one embodiment of the invention, as shown in fig. 1, the inner wall of the circular groove is provided with a rotating thread 5. In the invention, the rotating threads arranged on the outer wall of the hollow connecting device and the inner wall of the circular groove are mutually meshed, so that a vacuum environment can be formed after the adsorption assembly is assembled, negative pressure is formed under a vacuum device, and the adsorption of the self-repairing material solution by the carrier is promoted.
In one embodiment of the invention, the vacuum assembly comprises a vacuum pump 8. The vacuum pump has no special limitation on the type and the source, and can provide a vacuum environment for the adsorption assembly.
In one embodiment of the invention, as shown in fig. 2, the vacuum assembly comprises a gas pressure gauge 9. In the invention, the barometer and the vacuum pump can display the vacuum degree of the vacuum pump when the vacuum pump is used, so that the vacuum degree in the adsorption assembly can be controlled.
In the present invention, the upper end of the vacuum pumping head 1 is connected with a vacuum assembly through a hose 7. The source of the type of the hose is not particularly limited, and the hose can be connected with the upper end of the vacuum pumping head and the vacuum assembly.
As shown in fig. 3, in the present invention, the film covering device includes a placing platform and a receiving groove 6 vertically placed below the placing platform. In the present invention, the receiving groove is a circular groove in the adsorption component, and will not be described herein.
In the invention, the film covering device comprises a placing platform, wherein the placing platform comprises a stent 10 and a hollow connecting device 3 horizontally placed on the stent. In the present invention, the hollow connection means is a hollow connection means in the adsorption module. In the present invention, the bracket functions to support the hollow connecting means; the hollow connecting device is capable of supporting a self-healing material.
When the film covering device is used for covering films, the gauze can support the self-healing materials and can also enable redundant film covering materials to seep downwards, and then the films of the self-healing materials can be covered. The aperture of the gauze is not specially limited, and the gauze can be adjusted according to the size of the particle size of the selected self-healing material and can achieve the particle size larger than that of the supporting self-healing material.
In one embodiment of the invention, as shown in fig. 3, the film coating device comprises a base 11 for supporting 10 a support. The invention has no special limitation on the type and the source of the base and can play a role of a support bracket.
The device for preparing the film-covered self-healing material comprises the detachable adsorption device and the film covering device, can be used for preparing the self-healing material, can be assembled by utilizing the hollow connecting device and the circular groove in the device for preparing the self-healing material after the device for preparing the self-healing material is detached, is used for covering the prepared self-healing material, is simple and easy to obtain, and can greatly reduce the investment of equipment funds for preparing and covering the self-healing material.
The invention also provides a preparation method of the film-covered self-healing material, the device adopting the technical scheme is prepared, and the preparation method comprises the following steps:
(1) placing the carrier and the self-repairing material solution in a circular groove of an adsorption device;
(2) the round groove and the hollow connecting device are connected through the rotary screw threads, so that the gauze is positioned below the liquid level of the self-repairing material solution;
(3) coating sealing materials on contact surfaces of the vacuum air pumping head, the top cover with the opening convex groove and the hollow connecting device for sealing, and performing air pumping by using a vacuum assembly for adsorption to obtain a self-healing material;
(4) disassembling the hollow connecting device of the adsorption device and assembling the circular groove into a laminating device, and flatly paving the self-healing material prepared in the step (3) on the gauze in the laminating device;
(5) and pouring the film coating material on the self-healing material for film coating to obtain the film coating self-healing material.
The invention places the carrier and the self-repairing material solution in the circular groove of the adsorption device.
In the present invention, the carrier preferably comprises one or more of ceramsite, pumice, expanded perlite and zeolite, more preferably ceramsite. In the invention, the carrier is porous when being the type, has excellent adsorption capacity on the self-repairing material, and can adsorb more self-repairing materials. The source of the carrier in the present invention is not particularly limited, and commercially available products known to those skilled in the art may be used.
In the invention, the particle size of the carrier is preferably 3-8 mm, and more preferably 5-7 mm. In the invention, the carrier has too small a particle size to adsorb the repairing solution, and too large a particle size affects the macroscopic performance of the concrete, and when the particle size of the carrier is in the above range, the self-healing material with excellent performance can be obtained.
In the present invention, the self-healing material solution preferably includes one or more of a potassium carbonate solution, an ammonium carbonate solution, and a potassium silicate solution, and more preferably a sodium carbonate solution. In the invention, when the self-repairing material solution is of the above type, carbonate or silicate reacts with free calcium ions in the matrix to generate precipitates, so that cracks are filled.
In the present invention, the mass concentration of the self-repairing material solution is preferably 10% to 20%, and more preferably 15% to 20%. In the invention, when the mass concentration of the self-repairing material solution is in the range, the adsorption quantity of the self-repairing material in the carrier is favorably improved.
In the invention, when the mass concentration of the self-repairing material solution is preferably 10-20%, the volume ratio of the mass of the carrier to the self-repairing material solution is preferably (80-120) g: (20-30) mL, more preferably (90-100) g: (25-30) mL. In the invention, when the ratio of the mass of the carrier to the volume of the self-repairing material solution is in the range, the adsorption of the carrier to the self-repairing material is more favorably controlled.
The present invention preferably dries the carrier before placing the carrier and the solution of self-healing material in the circular trough of the adsorption device. In the invention, the drying temperature is preferably 50-65 ℃, and more preferably 55-60 ℃; the drying time is preferably (20-30) h, and more preferably 24 h. The drying apparatus of the present invention is not particularly limited, and a drying apparatus known to those skilled in the art may be used. In the present invention, the drying means is preferably an air-blast drying oven. In the invention, the drying can remove the moisture in the carrier, which is more beneficial to the subsequent adsorption process. In the present invention, when the drying temperature and time are within the above ranges, the carrier can be sufficiently dried, and the internal structure of the carrier can be prevented from being damaged.
After the carrier and the self-repairing material solution are placed in the circular groove of the adsorption device, the gauze is positioned below the liquid level of the self-repairing material solution by connecting the circular groove and the hollow connecting device through the rotary threads.
In the present invention, the pore size of the gauze is preferably smaller than the diameter of the support. In the invention, when the aperture of the gauze is preferably smaller than the diameter of the carrier, the whole carrier can be soaked in the self-repairing material solution by using the gauze, which is more favorable for the carrier to fully adsorb the self-repairing material. The pore diameter of the gauze is not particularly limited, and can be smaller than the diameter of the carrier. In the present invention, when the diameter of the carrier is preferably 3 to 8mm, the pore size of the mesh is preferably 35 to 60 mesh, and more preferably 40 to 50 mesh.
In the invention, the gauze is positioned below the liquid level of the self-repairing material solution, and the carrier is wholly soaked in the self-repairing material solution by using the pressure of the gauze, so that the carrier is favorable for fully adsorbing the self-repairing material.
After the circular groove is connected with the hollow connecting device, sealing materials are coated on the contact surfaces of the vacuum pumping head, the convex groove top cover with the opening and the hollow connecting device for sealing, and the self-healing material is obtained by utilizing a vacuum component for pumping and absorbing.
The sealing material is not particularly limited, and the sealing of the vacuum pumping head, the top cover with the opening convex groove and the hollow connecting device can be realized. In the present invention, the sealing material is preferably vaseline. In the invention, the vaseline can fill the gap between the vacuum pumping head, the top cover with the opening convex groove and the contact surface of the hollow connecting device, so that the effect of sealing the adsorption assembly is realized.
In the present invention, the vacuum module is preferably a vacuum pump. The vacuum pump is not specially limited in type, and can provide a vacuum environment for the adsorption assembly. In the present invention, the vacuum pump is preferably a circulating water type vacuum pump, and the circulating water type vacuum pump preferably includes a barometer. In the invention, the reading of the barometer of the circulating water type vacuum pump can show the vacuum degree provided by the vacuum pump in use, and the reading of the barometer of the circulating water type vacuum pump is 0-0.1 MPa.
In the present invention, the adsorption is performed under a vacuum environment. The vacuum degree of the vacuum environment is not particularly limited, and is determined according to the type of the used vacuum pump.
The adsorption time is not specially limited, and the carrier can fully adsorb the self-repairing material by adjusting the vacuum pump. In the present invention, when the vacuum pump is preferably a circulating water type vacuum pump having a barometer reading of 0 to-0.1 MPa, the adsorption time is preferably 40 to 45min, and more preferably 40 min. In the invention, when the barometer reading of the vacuum pump is in the range and the adsorption time is in the range, the adsorption capacity of the carrier on the self-repairing material can reach more than 90% of the maximum adsorption capacity.
According to the invention, the adsorbed carrier and the self-repairing material solution are preferably filtered after adsorption is finished, so that the self-repairing material is obtained. In the present invention, the means for filtering is preferably a hollow connecting means, and the means for receiving the self-healing material solution is preferably a circular tank.
After the self-healing material is obtained, the hollow connecting device of the detachable adsorption device is assembled into a film covering device, and the self-healing material is flatly paved on the gauze in the film covering device.
The amount of the self-healing material is not specially limited, and the self-healing material can be flatly spread on the gauze.
After the self-healing material is laid on the gauze in the film covering device, the film covering material is poured on the self-healing material for film covering to obtain the film covering self-healing material.
In the present invention, the coating material preferably includes an epoxy resin or polyvinyl alcohol, and more preferably an epoxy resin. In the present invention, the epoxy resin is preferably an epoxy resin adhesive and an epoxy resin curing agent in a ratio of 1: 1, preparing the mixture. The source of the epoxy resin is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used. In the present invention, the epoxy resin is preferably the epoxy resin AB glue of brother of hannan.
In the present invention, the coating process is accompanied by a curing process of the coating material on the surface of the carrier and a process of flowing excess coating material into the receiving tank through the gauze. The time for coating the film is not particularly limited, and the excessive film material can not flow into the receiving groove any more. In the invention, when the coating material is epoxy resin and the aperture of the gauze is 35-60 meshes, the coating time is preferably 1-2 min.
In the present invention, the amount of the coating material is not particularly limited, and the carrier may be coated.
In the present invention, when the thickness of the primary coating does not satisfy the thickness of the desired coating, the present invention preferably repeats the operation of pouring the coating material onto the self-healing material and coating the coating material to prepare the coated self-healing material having different coating thicknesses. The number of repetition is not particularly limited, and may be adjusted according to the desired thickness of the coating film.
The method for preparing the film-coated self-healing material provided by the invention is simple to operate, and not only can be used for preparing the self-healing material, but also can be used for controlling the thickness of the film.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The device for preparing the film-covered self-healing material comprises a detachable adsorption device and a film covering device; the adsorption device comprises a vacuum component and an adsorption component;
the device for preparing the film-covered self-healing material provided by the invention comprises two using states, namely preparation of the self-healing material and film covering.
When the self-healing material is prepared, as shown in fig. 1, the adsorption component comprises a vacuum pumping head 1, a top cover 2, a hollow connecting device 3, a gauze 4, a rotary thread 5 and a circular groove 6 which are sequentially arranged from top to bottom; the upper end of the vacuum pumping head 1 is connected with a vacuum assembly through a hose 7; the bottom of the hollow connecting device 3 is provided with a gauze 4; the hollow connecting device is connected with the circular groove through a rotary thread 5;
as shown in fig. 2, the apparatus for preparing the film-covered self-healing material includes a vacuum module including a circulation vacuum pump 8 and an air pressure gauge 9.
During film covering, as shown in fig. 3, the hollow connecting device and the circular groove of the adsorption device are disassembled to assemble a film covering device, and the film covering device comprises a placing platform and a circular groove 6 vertically placed below the placing platform; the placing platform comprises a support 10 and a hollow connecting device 3 horizontally placed on the support, and the hollow connecting device is a hollow connecting device in the adsorption component; the base 11 functions to support the stand 10.
Example 2
The apparatus of example 1 was used to prepare self-healing materials. The specific process is as follows:
(1) weighing ceramsite, placing in a forced air drying oven, and drying at 60 deg.C for 24 h.
(2) Pouring 200g of the dried ceramsite obtained in the step (1) into the circular groove 6, adding 60mL of a sodium carbonate solution with the mass concentration of 10%, and connecting the circular groove 6 with the hollow connecting device 3 through rotating threads to enable the gauze to be positioned below the liquid level of the self-repairing material solution.
(3) And (3) coating Vaseline on the contact surfaces of the vacuum pumping head 1, the top cover 2 with the opening convex groove and the hollow connecting device 3 for sealing, connecting an air pumping hose 7, starting a vacuum pump 8 to pump until the numerical value of the barometer 9 reaches-0.1 MPa. Vacuum adsorbing for 40 min; after the adsorption is finished, filtering the ceramsite adsorbing the sodium carbonate solution through the hollow connecting device 3 and the circular water tank 6 to obtain a self-healing material;
(4) assembling the hollow connecting device 3 for disassembling the adsorption device into a film covering device, and flatly paving the self-healing material prepared in the step (3) on a gauze in the film covering device;
(5) pouring epoxy resin (epoxy resin glue and epoxy resin curing agent are prepared in advance according to the proportion of 1: 1) on the self-healing material, and performing a film covering process (seepage is carried out for 1min so that redundant epoxy resin solution flows into the circular groove 6) to obtain a film covered self-healing material;
and (5) taking out the redundant epoxy resin solution in the circular water tank 6, and repeating the step (5) for 2-3 times so as to achieve the proper packaging film thickness.
The SEM image of the coating film of the coated self-healing material prepared in this example is shown in fig. 4 according to the observation of the coated self-healing material prepared in this example by using a depth-of-field stereoscopic scanning electron microscope.
As can be seen from fig. 4, the coating film of the coated self-healing material prepared in this example had an average thickness of 78.5 μm.
Testing the performance of the film-covered self-healing material:
in order to explore the packaging effect of the film-coated self-healing material prepared by the device and the method provided by the invention, the film-coated self-healing material prepared by the invention is subjected to an ion permeation test. The film is used for encapsulating the self-healing material and preventing ions in the self-healing material from being released quickly. Since ion diffusion of the carbonate solution is difficult to capture, and chloride ions and carbonate ions are adsorbed at a similar rate when the self-healing material is prepared, and released at a similar rate when released, the 10% mass concentration sodium carbonate solution in example 2 was replaced with a 10% mass concentration sodium chloride solution in this example, and the permeability of carbonate or silicate ions (such as potassium carbonate solution, ammonium carbonate solution, and potassium silicate solution) in the self-healing material was simulated by the permeation of chloride ions. Performance test the prepared film-coated self-healing material was prepared in the same manner as in example 2, except that a sodium chloride solution having a mass concentration was used in place of the sodium carbonate solution having a mass concentration of 10% in example 2. The average thickness of the obtained coating film of the coating film self-healing material was 78.5 μm.
The method of testing for ion penetration is as follows:
10 parts of the film-coated self-healing material sample with a clean and dry surface are taken, and 30g of the sample is weighed in each part. Then, the samples were placed in respective beakers containing 150g of deionized water, and the openings of the beakers were sealed with wrap films. And (5) according to the design time, labeling the beaker, and recording. And after the soaking time is up, filtering the solution in the cup, taking 50mL of the solution as a sample to be detected, and titrating the concentration of chloride ions diffused into deionized water by using a silver nitrate solution so as to determine the packaging effect of the lightweight aggregate sample. In the test, 10 samples are set in total, the diffusion rules of the samples are respectively measured for 1h, 3h, 5h, 7h, 9h, 21h, 24h, 72h, 168h and 336h (14d), and all the samples naturally diffuse in an environment with the temperature of 25 ℃ and the relative humidity of 60% until the specified test age.
After 336 hours of natural diffusion, the chloride ion diffusion curve of the film covering self-healing material is shown in fig. 5. As can be seen from fig. 5, the chloride ion content in the solution continued to increase during the first 24h of diffusion. After natural diffusion for 3h, the content of chloride ions diffused from the ceramsite in the solution reaches 6.93 multiplied by 10-4And (mol). When the diffusion time reaches 24h, the content of chloride ions in the solution continues to increase to 9.19 multiplied by 10-4And (mol). However, as the diffusion experiment continued, there was a significant decrease in the diffusion rate of chloride ions. The content of chloride ions is only increased by 2.83 multiplied by 10 from 24h to 72h-4mol, the chloride ion in the solution reaches 12.03 multiplied by 10-4And (mol). When the diffusion time reaches 168h and 336h, the chlorine ion content is increased by only 0.90X 10 compared with the chlorine ion content in the solution at 72h-4mol and 1.91X 10-4mol, finally 12.93X 10-4mol and 13.94X 10-4And (mol). According to the encapsulation ceramsiteThe total content of chloride ions in 30g of the ceramsite is about 0.16mol, and after the ceramsite is naturally diffused in a deionized solution for 336 hours, the total content of the chloride ions is only 13.94 multiplied by 10-4The mol chloride ion content was lost to the solution, with a diffusion amount of 0.87% of the initial content. It is considered that substantially no leakage occurred.
According to the experimental results, the film-coated self-healing material prepared by the device and the method provided by the invention has a good packaging effect, and when the film-coated self-healing material is used as the self-healing material, the self-healing material can be better kept until cracks are spread.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. A device for preparing a film-covered self-healing material comprises a detachable adsorption device and a film covering device;
the adsorption device comprises a vacuum component and an adsorption component;
the adsorption component comprises a vacuum gas-pumping head, a top cover, a hollow connecting device and a circular groove which are sequentially arranged from top to bottom;
the upper end of the vacuum pumping head is connected with the vacuum assembly through a hose;
the bottom of the hollow connecting device is provided with a gauze;
the hollow connecting device is connected with the circular groove through a rotary thread;
the film covering device comprises a placing platform and a receiving groove vertically placed below the placing platform; the receiving groove is a circular groove in the adsorption component;
the placing platform comprises a support and a hollow connecting device horizontally placed on the support, and the hollow connecting device is a hollow connecting device in the adsorption component.
2. The apparatus according to claim 1, wherein the top cap has a mouth groove at its upper end, and the top cap is connected to the vacuum pumping head via the mouth groove.
3. A self-healing material preparation apparatus according to claim 1, wherein the outer wall of the hollow connection means and the inner wall of the circular groove are provided with mutually engaging rotary threads.
4. A preparation method of a film-covered self-healing material, which is prepared by the device of any one of claims 1 to 3, comprises the following steps:
(1) placing the carrier and the self-repairing material solution in a circular groove of an adsorption device;
(2) the round groove and the hollow connecting device are connected through the rotary screw threads, so that the gauze is positioned below the liquid level of the self-repairing material solution;
(3) coating sealing materials on contact surfaces of the vacuum air pumping head, the top cover with the opening convex groove and the hollow connecting device for sealing, and performing air pumping by using a vacuum assembly for adsorption to obtain a self-healing material;
(4) disassembling the hollow connecting device of the adsorption device and assembling the circular groove into a laminating device, and flatly paving the self-healing material prepared in the step (3) on the gauze in the laminating device;
(5) and pouring the film coating material on the self-healing material for film coating to obtain the film coating self-healing material.
5. The method according to claim 4, wherein the carrier in step (1) comprises one or more of ceramsite, pumice, expanded perlite and zeolite.
6. The method for preparing the self-healing material of claim 4, wherein the self-healing material solution of step (1) includes one or more of a potassium carbonate solution, an ammonium carbonate solution, and a potassium silicate solution.
7. The preparation method of claim 6, wherein the mass concentration of the self-repairing material solution is 10-20%.
8. The method according to claim 4, wherein the mesh in the step (2) has a pore size smaller than the particle size of the carrier in the step (1).
9. The preparation method according to claim 4, wherein the step (5) is repeated to pour the coating material on the self-healing material to perform the coating operation, thereby preparing the coating self-healing material with different coating thicknesses.
10. A method for coating a self-healing material according to claim 4, wherein the coating material in step (5) includes epoxy resin or polyvinyl alcohol.
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