CN116330436A - Porous hydraulic cementing film and preparation method and application thereof - Google Patents
Porous hydraulic cementing film and preparation method and application thereof Download PDFInfo
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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
- C04B28/02—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 hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
-
- 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
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/14—Producing shaped prefabricated articles from the material by simple casting, the material being neither forcibly fed nor positively compacted
-
- 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
- B28B11/243—Setting, e.g. drying, dehydrating or firing ceramic articles
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28C—PREPARING CLAY; PRODUCING MIXTURES CONTAINING CLAY OR CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28C5/00—Apparatus or methods for producing mixtures of cement with other substances, e.g. slurries, mortars, porous or fibrous compositions
- B28C5/003—Methods for mixing
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
-
- 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
- C04B28/02—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 hydraulic cements other than calcium sulfates
- C04B28/06—Aluminous cements
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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
- C04B28/02—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 hydraulic cements other than calcium sulfates
- C04B28/06—Aluminous cements
- C04B28/065—Calcium aluminosulfate cements, e.g. cements hydrating into ettringite
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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
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/02—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/02—Selection of the hardening environment
- C04B40/0263—Hardening promoted by a rise in temperature
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/10—Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
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Abstract
The invention discloses a porous hydraulic cementing film, a preparation method and application thereof, and belongs to the technical field of porous separation film material preparation. Firstly, stirring hydraulic gel powder, deionized water, a binder and a dispersing agent to obtain uniformly mixed hydraulic gel slurry, and sequentially performing freeze molding, dry heat curing and hydration curing to obtain the directional porous hydraulic gel film. The method combines the freeze molding and the dry heat curing process for the first time, not only can keep the lamellar pore structure by promoting the evaporation of water, but also can accelerate the early hydration reaction of the hydraulic cementing material, thereby effectively improving the early strength of the porous hydraulic cementing film and avoiding collapse and damage after contacting with water during hydration curing. Compared with the prior art, the method does not need to use special equipment such as a vacuum freeze dryer, a constant temperature and humidity box and the like, simplifies the process flow and shortens the preparation period while obtaining the directional ordered continuous pore structure, and has remarkable economic benefit and wide application prospect.
Description
Technical Field
The invention belongs to the technical field of porous separation membrane material preparation, and particularly relates to a porous hydraulic cementing membrane and a preparation method thereof.
Background
The freeze molding technology is a method for preparing a bionic material, the water-based ceramic slurry is directionally solidified under the action of a temperature gradient, and the directional porous ceramic material with large specific surface area, high porosity and controllable pore structure can be obtained through freeze drying and high-temperature sintering. However, the porous ceramic material prepared by the freeze molding technology has poor toughness, and in addition, high-temperature sintering causes huge energy consumption and limits the expansion of application of the porous ceramic material. Therefore, the development of novel bionic materials with the characteristics of high strength and light weight is an effective way for reducing energy consumption.
The hydraulic cementing material and water are mixed to form slurry, and the slurry is gradually hardened in air or water, so that the hardness of the hydraulic cementing material can be maintained and continuously developed, and the hydraulic cementing material has excellent plasticity, but pores formed in the hardening process are disordered and discontinuous, and cannot be applied to the field of filtration. The patent CN103739306A discloses a method for preparing directional porous cement by mechanical stirring, ball milling, casting, directional freezing, freeze drying and constant temperature and humidity curing. The patent CN107619226A discloses a porous cement membrane, a preparation method and application thereof, wherein the porous cement membrane is prepared by adopting mechanical stirring, ball milling, directional freezing molding, freeze drying, constant temperature and humidity curing and hydration curing. In the preparation process, freeze drying and constant temperature and humidity curing are carried out on the directional frozen cement membrane to achieve the expected pore structure and hardness, and although the problem of high energy consumption caused by high-temperature sintering is avoided, specific equipment is needed in the freeze drying and constant temperature and humidity curing process, the equipment cost is high, the equipment energy consumption is high, the process is complex, and the preparation period is long.
The dry heat curing is a curing method which does not use steam as a heat transfer medium and does not directly contact the hydraulic material with the heat medium, and can accelerate curing of the hydraulic material. Pang Jiangte in the discussion about the mechanism of concrete dry heat curing, it is proposed that the damage to concrete by dry heat curing is small and the later strength can be recovered by a water immersion method. However, the hydraulic material slurry which is uniformly stirred is directly subjected to dry heat curing, the pore structure is in a disordered state, and the pores are discontinuous, so that directional pore channels cannot be formed, and the hydraulic material slurry cannot be effectively used as a separation material. The directional freezing plasticity can solidify the aqueous solution, and under the conditions of high temperature and low humidity, the ice crystals are quickly melted and evaporated or participate in hydration reaction, so that the pore channels are reserved.
Disclosure of Invention
Aiming at the problems that freeze drying, constant temperature and humidity maintenance special treatment and the like are needed in the preparation of the porous hydraulic cementing film by the traditional freeze molding technology, the invention provides a preparation method which is simple in preparation process, short in preparation period and lower in energy consumption, and the directional porous hydraulic cementing film is prepared by the method of directly carrying out dry heat maintenance process after directional freezing pore-forming, so that the problems of complex process, long preparation period and high energy consumption caused by the traditional method are solved.
In order to achieve the above object, the present invention relates to a method for preparing a porous hydraulic cementing film, comprising the following steps:
1) Mixing a hydraulic cementing material, a dispersing agent, a binding agent and deionized water to obtain uniformly mixed hydraulic cementing slurry, wherein the mass percentages of the dispersing agent, the binding agent, the hydraulic cementing material and the deionized water are respectively (1-2 wt%): (0-1 wt%): (38-58 wt%): (40-60 wt%);
2) The method comprises the steps of 1) degassing the hydraulic cementing slurry, quickly injecting the degassed hydraulic cementing slurry into a forming die, immediately placing the bottom of the forming die in a low-temperature freezing source, and directionally freezing to obtain a solid hydraulic cementing frozen body, wherein the forming die comprises a cylinder with two ends open and a bottom cover, the bottom cover is detachably arranged at the opening of the bottom of the cylinder, the heat conduction rate of the side wall of the cylinder is far less than that of the bottom cover, and the temperature gradually rises from the bottom of the forming die to the top to form a temperature gradient during directional freezing;
3) Putting the forming die with the hydraulic cementing frozen body in the step 2) into an electrothermal constant-temperature blast drying oven, carrying out dry heat curing at the temperature of 40-300 ℃, demoulding after curing to obtain a hydraulic cementing film precursor with certain hardness, and dividing the dry heat curing process into two stages, wherein the first stage is in a closed state, namely, the top opening of the forming die is sealed by using a preservative film, and the sealing time is 8-70 h; the second stage is in a semi-sealing state, namely the preservative film at the top opening is partially opened for 2-30 h;
4) And (3) placing the hydraulic cementing film precursor obtained in the step (3) into a curing pool with deionized water for curing, and flushing and cleaning with the deionized water after curing is finished to finally obtain the directional ordered porous hydraulic cementing film.
Specifically, in the step 1), the mass percentages of the dispersant, the binder, the hydraulic cementing material and the deionized water are respectively (1-2 wt%): (0-1 wt%): (38-58 wt%): (40-60 wt%) and the solid content of the obtained hydraulic cementing slurry is 40-60%.
Specifically, the porous hydraulic cementing material in the step 1) is any one of silicate cement, aluminate cement and sulphoaluminate cement, and the hydraulic cementing material is hydrated in the preparation process to form a three-dimensional network cementing material so as to increase the strength, preferably silicate cement; the binder is at least one of sodium carboxymethyl cellulose, polyvinyl alcohol, carboxymethyl cellulose, ethylene-ethyl acrylate and polyvinylpyrrolidone, and the binder increases slurry suspension viscosity through adsorption and electrostatic action, reduces movement speed of particles, wherein sodium carboxymethyl cellulose is preferred; the dispersing agent is at least one of sodium dodecyl sulfate, sodium polyacrylate, polyethylene glycol and polyacrylamide, and the dispersing agent enables solid particles to be uniformly dispersed in the solution through charge repulsion or steric effect, preferably sodium polyacrylate.
Specifically, in the step 1), the raw materials are uniformly mixed by mechanical stirring, the stirring time is 0.5-2 h, and the rotating speed is 100-400 r/min; preferably, the stirring time is 1-2 h, and the rotating speed is 300-350 r/min.
Specifically, in the forming mold in the step 2), the cylinder can be made of polytetrafluoroethylene, expanded polystyrene, polyphenyl ether, polycarbonate and other materials, and the bottom cover can be made of silver, copper, aluminum, iron, alloy thereof and other materials.
Specifically, the directional freezing temperature in the step 2) is-10 to-196 ℃, and the directional freezing time is 5min to 12h; preferably, the directional freezing temperature is-60 to-80 ℃, the directional freezing time is 0.1 to 12 hours, more preferably the directional freezing time is 0.5 to 1 hour, and the freezing temperature and the freezing time are selected, so that the manufacturing difficulty can be reduced, the preparation time can be shortened, and the solid hydraulic gel frozen body with excellent structure can be obtained.
Specifically, in the step 3), the dry heat curing temperature is 50-100 ℃, the dry heat curing time is 17-50h, correspondingly, the first-stage curing time is 12-35 h, and the second-stage curing time is 5-15 h. The second stage is to partially open the preservative film at the top opening, and the area (area) of the opened part is 1/4-1/2 of that of the top opening of the die, so that the preferential area can promote early hydration of the precursor and prevent fracture.
Specifically, the hydraulic cementing film precursor in the step 4) is further cured for 20-28 d in a curing pool, so as to obtain the directional porous hydraulic cementing film.
The porous hydraulic cementing film prepared by the method has a compact structure on one side and an obvious lamellar pore structure on the other side, the lamellar spacing is 16-25 mu m, the mesoporous pore diameter is 3.8-12 nm, the compressive strength is 2.54-5.32 MPa, and the pure water flux is 92-110 L.m under 0.1MPa -2 ·h -1 Can be used as an ultrafiltration membrane and applied to pretreatment of mariculture water, industrial wastewater and municipal wastewater and oilfield produced water treatment.
During directional freezing (temperature gradually increasing from bottom to top of the mould to form a temperature gradient), the ice crystals begin to nucleate and grow gradually from bottom to top along the temperature gradient, eventually forming a lamellar structure due to the anisotropic growth kinetics of hexagonal ice crystals, during which the hydraulic binder particles are displaced around the ice crystals.
In the dry heat curing process, ice crystals are melted, temperature difference and humidity difference exist in the inside of the refrigerating body, and moisture migrates to the inside under the driving force of temperature gradient when the temperature is raised (the ice outside the hydraulic cementing film precursor is melted into water firstly and then becomes water vapor, and the water vapor outside contacts with the ice inside and then is converted into liquid drops, so that the moisture migrates to the inside); under the action of humidity gradient, the water is transported outwards due to the pushing action of the partial pressure difference of water vapor on the surface of the refrigerating body. The humidity gradient in this process dominates the migration of moisture in the frozen body, thus representing an out-diffusion process, leaving pore channels in the body after evaporation of the moisture. The first stage is that the mold has covering, so that the water vapor partial pressure difference on the surface of the test piece is greatly reduced, water is prevented from escaping from the surface outwards, the water losing process is greatly slowed down, the test piece is prevented from being cracked, and meanwhile, the hydraulic cementing material can be ensured to fully contact with the water to generate hydration reaction. In the second stage, the surface of the die is in a semi-sealing state, the humidity is obviously reduced, the partial pressure difference of water vapor on the surface of the frozen body is increased, so that unreacted moisture in the inner part of the frozen body escapes from the surface, and the strength is high for resisting the damage of the surface tension of the moisture in the subsequent maintenance. This process forms a hydraulically setting gel film precursor having an initial strength and an oriented ordered lamellar pore structure; after hydration curing, the hydraulic cementing film with certain mechanical strength and oriented ordered lamellar pore structure can be obtained.
Compared with the prior art, the application has the following beneficial effects: (1) The dry heat curing technology is used for replacing freeze drying and constant temperature and humidity curing, the preparation method is simple, the preparation period is shortened, and special equipment such as a vacuum freeze dryer, a constant temperature and humidity test box and the like is not needed; (2) On the basis of the prior art, hydraulic cementing films with different aperture ranges can be prepared by adjusting the technological parameters such as solid content, freezing temperature, freezing time, dry heat curing temperature, dry heat curing time and the like; (3) The prepared hydraulic cementing film can obtain hydration products with different forms at different dry heat curing temperatures, and can load target functional substances according to the different forms of the hydration products, so that the application range of the hydraulic cementing film is expanded; (4) According to the method, after freeze molding, dry heat curing is used for promoting ice crystals to be evaporated after melting, lamellar pore channels can be effectively reserved, and meanwhile, the initial strength of the biscuit can be obtained through dry heat curing, so that hydration curing can be prevented from collapsing.
Drawings
FIG. 1 is a sectional scanning electron micrograph of the porous hydraulic gel membrane prepared in example 1;
FIG. 2 is a graph showing the distribution of the adsorption and desorption of nitrogen and the pore diameters of mesopores of the porous hydraulic gel membrane prepared in example 1.
Figure 3 shows a picture of the phenomenon of dry cracking when the frozen body is directly placed into an electrothermal constant temperature blast drying oven.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The following describes the technical scheme of the present application with reference to specific embodiments and drawings.
Example 1
Dissolving 0.5g of sodium carboxymethyl cellulose and 1.5g of sodium polyacrylate in 74g of deionized water, mechanically stirring at a rotating speed of 300r/min for 0.5h until the sodium carboxymethyl cellulose and the sodium polyacrylate are completely dissolved to obtain a clear and transparent mixed solution, adding 73.5g of silicate cement into the mixed solution, continuously mechanically stirring for 0.5h at a rotating speed of 300r/min to obtain a uniformly mixed silicate cement slurry, rapidly injecting the uniformly mixed silicate cement slurry into self-made forming dies after degassing treatment for directional freezing casting, injecting 25g of each die at a freezing temperature of-60 ℃ for 0.5h to obtain a solid silicate cement film frozen body, sealing the top of the dies by a preservative film, then moving the dies into an electrothermal constant-temperature blast drying oven for 25h, continuously preserving for 15h at a constant temperature of 80 ℃, demoulding to obtain a silicate cement film precursor, putting the silicate cement film precursor into a curing pool with deionized water, curing for 20d at room temperature, and then taking out and flushing to obtain the silicate cement film.
FIG. 1 is a microstructure picture of a porous hydraulic gel membrane prepared in this example, the prepared silicate cement membrane has obvious delamination, the top part of the silicate cement membrane presents a lamellar pore structure, a red frame is shown, FIG. 2 is a pore diameter distribution diagram of the porous hydraulic gel membrane prepared in this example, the spacing between sheets is 23 μm, the average pore diameter of mesopores is 3.79nm, the compressive strength is 2.54MPa, more needle-like ettringite appears, the platy calcium hydroxide content is less, and the pure water flux is 105 L.m under 0.1MPa -2 ·h -1 。
In the early stage of the experiment, the dry heat curing is not carried out in two stages. Initially, a forming die filled with a solid Portland cement film frozen body is directly moved into an electrothermal constant-temperature blast drying oven at 50 ℃ for preservation for 25 hours, and the obtained Portland cement film precursor shows dry cracking (shown in figure 3). And in the later experiment, the dry heat curing condition is regulated, the top of a forming die filled with a solid Portland cement film frozen body is sealed by adopting a preservative film, and the sealing die is placed in an electrothermal constant-temperature blast drying oven at 50 ℃ for 25 hours to be stored, so that the Portland cement film precursor is easy to collapse in the later hydration process. Finally, the dry heat curing is adjusted to two stages in the invention.
Example 2
Dissolving 0.34g of polyvinylpyrrolidone and 1.33g of ammonium polyacrylate in 49.3g of deionized water, mechanically stirring at a rotating speed of 350r/min for 1h until the mixture is completely dissolved to obtain a clear and transparent mixed solution, adding 49g of silicate cement into the mixed solution, continuously mechanically stirring for 0.5h at the rotating speed of 350r/min to obtain a uniformly mixed silicate cement slurry, injecting the uniformly mixed silicate cement slurry into self-made forming dies after degassing treatment for directional freezing casting, injecting 20g of each die at a freezing temperature of-60 ℃ for 1h, obtaining a solid silicate cement film frozen body, sealing the top of the dies by a preservative film, then moving the dies into an electrothermal constant temperature blast drying oven for 20h, changing the dies into a semi-sealing state (the opening of the forming dies is 1/4), continuously preserving at the temperature of 80 ℃, demoulding to obtain a silicate cement film precursor, putting the silicate cement film precursor into a curing pool with deionized water, taking out after 20d at room temperature, and flushing to obtain the silicate cement film.
The prepared silicate cement membrane is compact at the side close to the freezing source, has obvious lamellar pore structure at the side far away from the freezing source, has lamellar spacing of 25 μm, mesoporous pore diameter distribution concentrated at 3.84nm and 8nm, compressive strength of 5.32MPa, relatively less needle-like ettringite content, more platy calcium hydroxide and pure water flux of 110 L.m under 0.1MPa -2 ·h -1 。
Example 3
Dissolving 0.34g of ethylene-ethyl acrylate and 1.33g of sodium dodecyl sulfate in 49.3g of deionized water, mechanically stirring at a rotating speed of 300r/min for 1h until the mixture is completely dissolved to obtain a clear and transparent mixed solution, adding 49g of aluminate cement into the mixed solution, continuously mechanically stirring for 1h at a rotating speed of 320r/min to obtain uniformly mixed aluminate cement slurry, injecting the uniformly mixed aluminate cement slurry into self-made forming dies after degassing treatment for directional freezing casting, injecting 25g of each die, freezing at a temperature of minus 196 ℃ for 5min, obtaining a solid aluminate cement film frozen body, sealing the top of the dies by a preservative film, then moving into an electrothermal constant temperature blast drying oven for 20h, changing the die into a semi-sealing state (the opening of the forming die is 1/4), continuously preserving for 10h, maintaining at a constant temperature of 100 ℃, demoulding, taking out the aluminate cement film precursor, and flushing to obtain the aluminate cement film.
The prepared aluminate cement membrane has obvious layered structure, the side close to the freezing source is compact, the side far away from the freezing source is lamellar pore structure, the lamellar spacing is 16 mu m, the mesoporous pore diameter distribution is concentrated at 4nm,8nm and 12nm, the compressive strength is 3.00MPa, more needle-shaped ettringite appears, and the pure water flux is 92 L.m under 0.1MPa -2 ·h -1 。
Example 4
Dissolving 0.5g of polyvinylpyrrolidone and 1.5g of ammonium polyacrylate in 74g of deionized water, mechanically stirring at a rotating speed of 350r/min for 1h until the ammonium polyacrylate is completely dissolved to obtain a clear and transparent mixed solution, adding 73.5g of silicate cement into the mixed solution, continuously mechanically stirring for 0.5h at a rotating speed of 300r/min to obtain a uniformly mixed silicate cement slurry, injecting the uniformly mixed silicate cement slurry into self-made forming dies for directional freezing casting after degassing treatment, injecting 25g of each die, freezing at-80 ℃ for 0.5h to obtain solid silicate cement film frozen bodies, sealing the top of the dies by using a preservative film, then moving the dies into an electrothermal constant-temperature blasting drying oven for 25h, changing the dies into a semi-sealing state (the opening of the forming die is 1/4), continuously preserving at a constant temperature of 100 ℃, demoulding to obtain a silicate cement film precursor, putting the silicate cement film precursor into a curing pool with deionized water, curing at room temperature for 20d, and then taking out the silicate cement film after flushing.
The prepared silicate cement membrane is compact at the side close to the freezing source, has obvious lamellar pore structure at the side far away from the freezing source, has lamellar spacing of 18 μm, mesoporous pore diameter distribution concentrated by 4nm,8nm and 11nm, compressive strength of 3.41MPa, more needle-shaped ettringite appears, and pure water flux of 107 L.m under 0.1MPa -2 ·h -1 。
Example 5
Dissolving 0.5g of polyvinylpyrrolidone and 1.5g of ammonium polyacrylate in 74g of deionized water, mechanically stirring at a rotating speed of 350r/min for 1h until the ammonium polyacrylate is completely dissolved to obtain a clear and transparent mixed solution, adding 73.5g of silicate cement into the mixed solution, continuously mechanically stirring for 0.5h at a rotating speed of 300r/min to obtain a uniformly mixed silicate cement slurry, injecting the uniformly mixed silicate cement slurry into self-made forming dies for directional freezing casting after degassing treatment, injecting 25g of each die, freezing at-80 ℃ for 0.5h to obtain solid silicate cement film frozen bodies, sealing the top of the dies by using a preservative film, then moving the dies into an electrothermal constant-temperature blasting drying oven for 12h, changing the dies into a semi-sealing state (the opening of the forming die is 1/4), continuously preserving at the temperature of 80 ℃, demoulding to obtain a silicate cement film precursor, putting the silicate cement film precursor into a curing pool with deionized water, curing at room temperature for 20d, and then taking out the silicate cement film after flushing.
The prepared silicate cement membrane is compact at the side close to the freezing source, has obvious lamellar pore structure at the side far away from the freezing source, has lamellar spacing of 20 μm, mesoporous pore diameter distribution concentrated at 3.8nm and 8nm, compressive strength of 3.70MPa, more needle-shaped ettringite, less platy calcium hydroxide content and pure water flux of 108 L.m under 0.1MPa -2 ·h -1 。
Example 6
Dissolving 2g of sodium dodecyl sulfate in 60g of deionized water, mechanically stirring at a rotating speed of 400r/min for 0.25h until the sodium dodecyl sulfate is completely dissolved to obtain a clear and transparent mixed solution, adding 38g of sulfoaluminate cement into the mixed solution, continuously mechanically stirring for 0.25h at a rotating speed of 320r/min to obtain uniformly mixed sulfoaluminate cement slurry, injecting the uniformly mixed sulfoaluminate cement slurry into self-made forming dies after degassing treatment for directional freezing casting, injecting 25g of each die, freezing at the temperature of-40 ℃ for 10h, obtaining solid sulfoaluminate cement film frozen bodies, sealing the top of the dies by using a preservative film, then moving the dies into an electrothermal constant-temperature blasting drying box for 35h, changing the dies into a semi-sealing state (the opening of the forming die is 1/2), continuously preserving for 10h, demoulding at the constant temperature of 40 ℃ to obtain a sulfoaluminate cement film precursor, putting the sulfoaluminate cement film precursor into a curing pool with deionized water, curing at room temperature for 20d, and then taking out the sulfoaluminate cement film after flushing.
Example 7
Dissolving 1g of polyvinyl alcohol and 1g of polyethylene glycol in 40g of deionized water, mechanically stirring at a rotating speed of 100r/min for 1h until the polyvinyl alcohol and the polyethylene glycol are completely dissolved to obtain a clear and transparent mixed solution, adding 58g of aluminate cement into the mixed solution, continuously mechanically stirring for 1h at the rotating speed of 100r/min to obtain uniformly mixed aluminate cement slurry, injecting the uniformly mixed aluminate cement slurry into self-made forming dies after degassing treatment for directional freezing casting, injecting 25g of each die, sealing the top of the die by using a preservative film, then moving the die into an electrothermal constant-temperature blasting drying oven for 12h, changing the die into a semi-sealing state (the opening of the forming die is 1/2), continuously preserving for 5h, maintaining at the constant temperature of 300 ℃, demoulding to obtain an aluminate cement film precursor, putting the aluminate cement film precursor into a curing pool with deionized water, curing at the room temperature for 28d, and then taking out and washing to obtain the aluminate cement film.
Comparative example 1
Dissolving 0.5g of sodium carboxymethyl cellulose and 1.33g of sodium polyacrylate in 74g of deionized water, mechanically stirring at a rotating speed of 300r/min for 0.5h until the sodium carboxymethyl cellulose and the sodium polyacrylate are completely dissolved to obtain a clear and transparent mixed solution, adding 73.5g of silicate cement into the mixed solution, continuously mechanically stirring for 0.5h at a rotating speed of 300r/min to obtain a uniformly mixed silicate cement slurry, rapidly injecting the uniformly mixed silicate cement slurry into self-made forming dies after degassing treatment for directional freezing casting, injecting 25g of the silicate cement slurry into each die at a freezing temperature of-60 ℃ for 0.5h to obtain a solid silicate cement film frozen body, immediately putting a frozen blank taken out of the freezing dies into a freeze dryer for 36h, maintaining the vacuum degree in the freeze dryer at 0.15mbar, removing ice crystals in the frozen blank, putting the cement-based porous blank after the freeze drying into a constant-humidity box for curing at a temperature of 30 ℃, taking out after curing for 2d, putting the silicate cement film precursor into a silicate cement pool for curing at a constant temperature of 20d, and taking out the silicate cement film precursor after curing.
The prepared silicate cement membrane has an interlayer spacing of about 30 mu m, mesoporous pore diameter distribution concentrated at 3.97nm and 0.1MPa, and pure water flux of 108 L.m -2 ·h -1 。
Application example
The Portland cement membrane prepared in example 1 was used for oil-water separation, and specifically:
0.90g of HFV-high vacuum oil and 0.2g of sodium dodecyl sulfate are added into deionized water, the mixture is stirred for 36 hours at a high speed after the constant volume is 1.0L, and the mixture is kept stand for 8 hours to obtain a uniformly mixed milky oil-water solution. The ultrafiltration device prepared by the Portland cement membrane of the embodiment 1 is used for oil-water separation test, the operation mode adopts cross-flow filtration, the operation pressure is adjusted to the value required by experiments, the concentration of the stock solution and the filtrate is tested and calculated by an ultraviolet-visible light spectrophotometer, and the oil-water separation performance is calculated. When the operating pressure was adjusted to 0.05,0.10 and 0.15MPa, the oil-water separation performance was 78.05%,77.18% and 75.99%, respectively.
The above description is only for the purpose of illustrating the preferred embodiments of the present method, and is not intended to limit the present method, and the parameters may be modified or changed equally by those skilled in the art based on the above embodiments, and all modifications or changes in the principle of the present method are included in the scope of protection of the present method.
Claims (10)
1. A method for preparing a porous hydraulic gel film, which is characterized by combining a freeze molding process and a dry heat curing process, and specifically comprises the following steps:
1) Mixing a hydraulic cementing material, a dispersing agent, a binding agent and deionized water to obtain uniformly mixed hydraulic cementing slurry, wherein the mass percentages of the dispersing agent, the binding agent, the hydraulic cementing material and the deionized water are respectively (1-2 wt%): (0-1 wt%): (38-58 wt%): (40-60 wt%);
2) The method comprises the steps of 1) degassing the hydraulic cementing slurry, quickly injecting the degassed hydraulic cementing slurry into a forming die, immediately placing the bottom of the forming die in a low-temperature freezing source, and directionally freezing to obtain a solid hydraulic cementing frozen body, wherein the forming die comprises a cylinder with two ends open and a bottom cover, the bottom cover is detachably arranged at the opening of the bottom of the cylinder, the heat conduction rate of the side wall of the cylinder is far less than that of the bottom cover, and the temperature gradually rises from the bottom of the forming die to the top to form a temperature gradient during directional freezing;
3) Putting the forming die with the hydraulic cementing frozen body in the step 2) into an electrothermal constant-temperature blast drying oven, carrying out dry heat curing at the temperature of 40-300 ℃, demoulding after curing to obtain a hydraulic cementing film precursor with certain hardness, and dividing the dry heat curing process into two stages, wherein the first stage is in a closed state, namely, the top opening of the forming die is sealed by using a preservative film, and the sealing time is 8-70 h; the second stage is in a semi-sealing state, namely the preservative film at the top opening is partially opened for 2-30 h;
4) And (3) placing the hydraulic cementing film precursor obtained in the step (3) into a curing pool with deionized water for curing, and flushing and cleaning with the deionized water after curing is finished to finally obtain the directional ordered porous hydraulic cementing film.
2. The method for preparing a porous hydraulic cementing film according to claim 1, wherein the hydraulic cementing material in step 1) is any one of silicate cement, aluminate cement and thioaluminate cement; the binder is one or more of sodium carboxymethyl cellulose, polyvinyl alcohol, ethylene-ethyl acrylate and polyvinylpyrrolidone; the dispersing agent is one or more of sodium dodecyl sulfate, sodium polyacrylate, polyethylene glycol and polyacrylamide.
3. The method for preparing a porous hydraulic gel film according to claim 1, wherein the raw materials are uniformly mixed by mechanical stirring in the step 1), the stirring time is 0.5-2 h, and the rotating speed is 100-400 r/min.
4. The method for preparing a porous hydraulic gel film according to claim 1, wherein in the forming mold in the step 2), the cylinder is made of polytetrafluoroethylene, expanded polystyrene, polyphenylene oxide or polycarbonate, and the bottom cover is made of any one of silver, copper, aluminum, iron and alloys thereof.
5. The method for producing a porous hydraulic gel film according to claim 1, wherein the directional freezing temperature in step 2) is-10 to-196 ℃ and the directional freezing time is 5min to 12h.
6. The method for producing a porous hydraulic gel film according to claim 1, wherein the dry heat curing temperature in step 3) is 50 to 100 ℃, the dry heat curing time is 17 to 50 hours, and correspondingly, the first stage curing time is 12 to 35 hours, and the second stage curing time is 5 to 15 hours.
7. The method for producing a porous hydraulic gel film according to claim 1, wherein the second stage is to partially open the preservative film at the top opening, and the area of the opened portion is 1/4 to 1/2 of the top opening of the mold.
8. A porous hydraulic gel membrane prepared by the method of any one of claims 1-8.
9. The porous hydraulic gel membrane according to claim 8, wherein one side of the porous hydraulic gel membrane has a dense structure and the other side has a distinct lamellar pore structure, the lamellar spacing is 16-25 μm, the mesoporous pore diameter is 3.8-12 nm, the compressive strength is 2.54-5.32 mpa, and the pure water flux is 92-110 l.m at 0.1mpa -2 ·h -1 Can be used as ultrafiltration membrane.
10. The porous hydraulic gel membrane of claim 8, which is applied to pretreatment of mariculture water, industrial wastewater and municipal wastewater and oilfield produced water treatment.
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