CN109293263B - Oriented porous geopolymer inorganic membrane and preparation method thereof - Google Patents
Oriented porous geopolymer inorganic membrane and preparation method thereof Download PDFInfo
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- CN109293263B CN109293263B CN201811224116.8A CN201811224116A CN109293263B CN 109293263 B CN109293263 B CN 109293263B CN 201811224116 A CN201811224116 A CN 201811224116A CN 109293263 B CN109293263 B CN 109293263B
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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
- C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
- C04B12/005—Geopolymer cements, e.g. reaction products of aluminosilicates with alkali metal hydroxides or silicates
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
Abstract
The invention discloses a directional porous geopolymer inorganic membrane, belonging to the technical field of porous inorganic material preparation, which takes active powder and an exciting agent as membrane forming materials, adopts a freezing molding process, takes water as a template agent, and prepares the inorganic membrane which takes geopolymer as a framework and has an oriented macroporous structure and a mesoporous structure distributed on the wall of a macroporous channel by adjusting factors such as freezing temperature, water content and the like. The inorganic membrane prepared by the method has the characteristics of quick film forming, short curing time, high mechanical strength, compressive strength of 4.0-50.0MPa, porosity of 5-75 percent, pore size distribution range of 2nm-800 mu m, high temperature resistance, acid and alkali resistance, low-temperature curing and the like.
Description
Technical Field
The invention relates to a directional porous geopolymer inorganic membrane material and a preparation method thereof, belonging to the technical field of porous inorganic material preparation.
Background
The membrane separation technology is a new separation technology which rises rapidly after the 60's of the 20 th century. There are two main types of separation membranes currently in use: polymeric organic films and inorganic films. Inorganic membranes based on inorganic material science have incomparable advantages over polymeric organic membranes: high mechanical strength, stable chemical property, strong pollution resistance, acid resistance, alkali resistance, organic solvent resistance, high temperature resistance and the like. However, inorganic membrane elements and equipment represented by ceramic membranes have high manufacturing cost, the membrane materials have high brittleness and high energy consumption in high-temperature sintering, the defects of difficult recovery and reutilization and the like limit the wide application of the inorganic membrane elements, and the relatively cheap raw materials for preparing the inorganic membrane are still to be excavated, so that the development of novel inorganic membrane materials with low cost and high performance has important significance for large-scale popularization of the inorganic membrane.
Geopolymers (geopolymers) are a concept proposed by french famous scientist j. Davidovits in 1978, and refer to a three-dimensional network gel material consisting of silicon-oxygen tetrahedrons and aluminum-oxygen tetrahedrons formed from natural aluminosilicate minerals or solid wastes as main raw materials and by depolymerization-polycondensation-gel networking in a strong alkali solution. The geopolymer has the advantages of early strength, quick hardening, corrosion resistance, high temperature resistance, good chemical stability and the like, the raw materials are cheap and easy to obtain, the curing temperature is low, sintering is avoided, pollution is almost avoided, and the geopolymer belongs to a low-carbon green environment-friendly material for sustainable development.
The preparation of inorganic membrane materials is the basis of inorganic membrane science, and the currently common preparation methods with industrial application prospects mainly comprise a solid particle sintering method, a sol-gel method, a thin film deposition method, an anodic oxidation method, a phase separation-leaching method, a thermal decomposition method, a hydrothermal method and the like. The ideal preparation method not only requires the preparation of the membrane material with the structure capable of being accurately regulated and controlled, the shape and the size of the hole are excellent, and the membrane material has certain mechanical property, but also requires low cost and simple process. The freezing molding technology is a new process for preparing porous materials, which not only can 'customize' the shape of microscopic pores, but also can make the pore channels directionally arranged, so that the materials have controllable open porosity, excellent mechanical property and permeability. The materials such as porous ceramics and porous organic foams prepared by the technology are successfully applied in the fields of biology, chemical industry, buildings and the like. And portland cement films (CN 107619226A, CN106892674A, and CN 103739306B) have been successfully prepared using a freeze molding process. Until now, no research on the preparation of oriented porous geopolymer inorganic membrane materials by a freeze molding process has been reported.
In the traditional portland cement forming process, firstly C3S、C3A、C4F reacts with water to form hydration products (hydrated gel and calcium hydroxide) with certain fluidity and plasticity, then the hydration products are coagulated to finally form solidified cement, and the cement is a three-dimensional sealed entity. The freezing molding process forms directional pore canals in the cement stone to prepare the cement film. In the process of preparing the cement film by the frozen molding process, because the hydration and hardening processes of cement are slow at low temperature, the blank formed by frozen molding and freeze drying is only formed by simply stacking cement powder together through a binder, and the cement powder falls off by slight touch, so that the later-period curing time is long and about one month in order to obtain the cement film with certain strength.
Disclosure of Invention
The invention aims to solve the defects of the existing inorganic membrane material and the preparation technology, utilizes cheap chemical raw materials, provides a directional porous geopolymer inorganic membrane which has simple process and low cost and can be widely applied and a preparation method thereof, solves the problems of too long curing time, low strength of a cement membrane and poor strong acid and alkali resistance when a cement membrane is prepared by adopting a freeze molding process, and simultaneously further enriches an inorganic membrane material system.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
an oriented porous geopolymer inorganic membrane takes geopolymer as a framework, and oriented pore channels are uniformly distributed on the geopolymer framework.
A preparation method of an oriented porous geopolymer inorganic membrane specifically comprises the following steps:
(1) preparation of film-forming slurry: 60-100 parts of active powder, 140 parts of exciting agent 100 and 30-80 parts of water are mixed according to the mass part ratio, mechanically stirred uniformly and then placed at 20-50 ℃ for 1-4h for standby.
(2) Preparation of a frozen blank: and adding 10-100 parts of water into the film-forming slurry, quickly and mechanically stirring uniformly, immediately injecting into a self-made freezing mold for directional freezing at the freezing temperature of-20 to-80 ℃, and obtaining a frozen blank after the slurry is solidified.
(3) Preparing a directional porous blank: freeze drying the frozen blank at vacuum degree of 10-50Pa, freezing temperature of-50 deg.C to-80 deg.C for 8-12h to obtain directional porous blank.
(4) Curing the oriented porous inorganic membrane: and (3) putting the oriented porous blank into a constant-temperature constant-humidity curing box for curing at the temperature of more than or equal to 10 ℃ and the humidity of more than or equal to 60 percent for 24-96 hours to finally obtain the oriented porous geopolymer inorganic membrane.
Wherein the compressive strength of the oriented porous geopolymer inorganic membrane is 4.0-50.0MPa, the porosity is 5% -75%, and the pore size distribution range is 2nm-800 μm.
The active powder is one or more of natural silicate powder, clay, kaolin, red mud, volcanic ash, lava, industrial waste and artificial powder. The artificially synthesized powder is specifically Al prepared by a chemical synthesis method2O3-SiO2And (3) powder.
The waste produced by the industry comprises fly ash, slag, furnace slag and tailings.
The excitant is one or more of industrial sodium water glass, potassium water glass, hydroxide of alkali metal, fluoride, carbonate, phosphoric acid, phosphate, sulfate, silicate and aluminosilicate solution.
The water in the step (1) is used as a solvent to participate in geological polymerization reaction, the water in the step (2) is used as a template agent, and the water is added in two times, so that the problems that the concentration of an exciting agent is reduced by adding once to influence the depolymerization process of the active powder, the time for performing freeze molding is difficult to control are avoided, and the problem that the water amount in the step (1) is difficult to play a role of the template agent is solved.
The ice template grows directionally under the action of temperature gradient to form crystals with different forms, and the crystals are removed in the freeze drying process to leave pore channels arranged directionally; and curing the biscuit to obtain the directional porous inorganic separation membrane with controllable porosity and pore size.
Compared with the prior art, the invention has the following advantages:
(1) the preparation method perfectly combines the freezing molding technology with the preparation of geopolymer, not only forms the inorganic membrane which takes geopolymer as a framework and has an oriented macroporous structure and a mesoporous structure distributed on the wall of a macroporous channel, but also the formed inorganic membrane has the characteristics of high temperature resistance, acid and alkali resistance, low-temperature curing and the like, simultaneously avoids the defects that the traditional inorganic porous material such as ceramic needs high-temperature sintering and the like, and provides the inorganic membrane which has simple process, low cost, environmental protection and the preparation method thereof.
(2) The preparation process simultaneously considers the strength and the crystal growth, and realizes the good aperture distribution of the material while ensuring the strength. The geopolymer inorganic membrane prepared by the invention is tightly combined together through chemical bonds after being frozen and molded and frozen and dried, has certain strength, can greatly improve the strength through short-time maintenance, and meets the requirements of industrial application.
(3) The pore morphology and related performance of the oriented porous geopolymer inorganic membrane can be regulated and controlled by changing preparation conditions (water addition amount, freezing temperature, freezing time and the like), the pore size distribution range is 2nm-800 mu m, and the porosity range is 5% -75%.
(4) The internal structure of the oriented porous geopolymer inorganic membrane prepared by the invention consists of an oriented porous supporting layer, a conversion layer and a compact functional layer, the oriented porous supporting layer, the conversion layer and the compact functional layer are molded in one step in the preparation process, post-treatment is not needed, the process flow is simplified, and the compact functional layer with a proper size can achieve the effect of accurate separation.
Drawings
FIG. 1 is a scanning electron microscope cross-sectional view of an oriented porous geopolymer inorganic film prepared in example 1 of the present invention.
FIG. 2 is a scanning electron microscope cross-sectional view of an oriented porous geopolymer inorganic film prepared in example 2 of the present invention.
FIG. 3 is a scanning electron microscope cross-sectional view of an oriented porous geopolymer inorganic film prepared in example 3 of the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and the embodiments.
Example 1
A method for preparing an oriented porous geopolymer inorganic membrane, comprising the steps of:
(1) preparation of film-forming slurry: according to the mass portion, 20g of metakaolin, 24g of industrial sodium silicate (purchased from Shandong Yousio chemical engineering Co., Ltd.) with the modulus of 1.3 and 10g of water are mixed, mechanically stirred for 10min at the speed of 800r/min, and the obtained mixed slurry is kept stand for 2h in an environment with the temperature of 25 ℃ for standby.
(2) Preparation of a frozen blank: and adding 10g of water into the film-forming slurry, mechanically stirring uniformly, injecting into a self-made freezing mold for directional freezing, wherein the freezing temperature is-80 ℃, and obtaining a frozen blank after the slurry is solidified.
(3) Preparing a directional porous blank: and (3) freeze-drying the frozen blank body at the vacuum degree of 15pa at the freezing temperature of-80 ℃ for 8h to form the directional porous blank body.
(4) Curing the oriented porous inorganic membrane: and (3) putting the oriented porous blank into a constant-temperature constant-humidity curing box for curing at the temperature of 30 ℃ and the humidity of 100% for 48 hours to finally obtain the wafer-shaped oriented porous geopolymer inorganic membrane.
FIG. 1 is a scanning electron microscope cross-sectional view of the oriented porous geopolymer inorganic film prepared in this example, from which it can be seen that the interior of the sample shows an oriented porous structure.The pure water flux is 550L m under the operation pressure of 0.2MPa when the pure water flux is tested under the normal temperature condition-2*h-1。
Example 2
A method for preparing an oriented porous geopolymer inorganic membrane, comprising the steps of:
(1) preparation of film-forming slurry: mixing 20g of fly ash, 20g of 10M sodium hydroxide solution and 15g of water according to the mass portion ratio, mechanically stirring for 15min at the speed of 600r/min, and standing the obtained mixed slurry for 3h at the temperature of 20 ℃ for later use.
(2) Preparation of a frozen blank: and adding 10g of water into the film-forming slurry, mechanically stirring uniformly, injecting into a self-made freezing mold for directional freezing at the freezing temperature of-50 ℃, and obtaining a frozen blank after the slurry is solidified.
(3) Preparing a directional porous blank: and (3) freeze-drying the frozen blank at the vacuum degree of 20pa at the freezing temperature of-50 ℃ for 10h to form the directional porous blank.
(4) Curing the oriented porous inorganic membrane: and (3) putting the oriented porous blank into a constant-temperature constant-humidity curing box for curing at the temperature of 25 ℃ and the humidity of 80% for 36 hours to finally obtain the wafer-shaped oriented porous geopolymer inorganic membrane.
FIG. 2 is a scanning electron microscope cross-sectional view of the oriented porous geopolymer inorganic film prepared in this example. It can be seen from the figure that the interior of the sample presents an oriented dendritic porous structure, the porosity is 5% -75%, and the pore size distribution range is 2nm-800 μm. The pure water flux is 640L m under the operation pressure of 0.2MPa when the pure water flux is tested under the normal temperature condition-2*h-1。
Example 3
A method for preparing an oriented porous geopolymer inorganic membrane, comprising the steps of:
(1) preparation of film-forming slurry: taking 25g of slag (specifically granulated blast furnace slag), 30g of industrial sodium silicate with the modulus of 1.3 and 15g of water according to the mass portion ratio, mixing, mechanically stirring for 10min at 700r/min, and standing the obtained mixed slurry for 2h in an environment of 30 ℃ for later use.
(2) Preparation of a frozen blank: and adding 15g of water into the film-forming slurry, mechanically stirring uniformly, injecting into a self-made freezing mold for directional freezing at the freezing temperature of-20 ℃, and obtaining a frozen blank after the slurry is solidified.
(3) Preparing a directional porous blank: and (3) freeze-drying the frozen blank at the vacuum degree of 25pa at the freezing temperature of-50 ℃ for 12h to form the directional porous blank.
(4) Curing the oriented porous inorganic membrane: and (3) putting the oriented porous blank into a constant-temperature constant-humidity curing box for curing at the temperature of 35 ℃ and the humidity of 95% for 72 hours to finally obtain the wafer-shaped oriented porous geopolymer inorganic membrane.
FIG. 3 is a scanning electron microscope cross-sectional view of the oriented porous geopolymer inorganic film prepared in this example. It can be seen from the figure that the interior of the sample exhibits an oriented three-dimensional network-like pore structure. Tested under normal temperature conditions, the pure water flux is 810L m under the operation pressure of 0.2MPa-2*h-1。
Example 4
A method for preparing an oriented porous geopolymer inorganic membrane, comprising the steps of:
(1) preparation of film-forming slurry: mixing 20g of metakaolin, 20g of phosphoric acid solution with the mass fraction of 75% and 10g of water according to the mass part ratio, mechanically stirring for 20min at the speed of 500r/min, and standing the obtained mixed slurry for 1h in an environment at the temperature of 50 ℃ for later use.
(2) Preparation of a frozen blank: and adding 5g of water into the film-forming slurry, mechanically stirring uniformly, injecting into a self-made freezing mold for directional freezing at the freezing temperature of-80 ℃, and obtaining a frozen blank after the slurry is solidified.
(3) Preparing a directional porous blank: and (3) freeze-drying the frozen blank at the vacuum degree of 30pa at the freezing temperature of-60 ℃ for 10h to form the directional porous blank.
(4) Curing the oriented porous inorganic membrane: and (3) putting the oriented porous blank into a constant-temperature constant-humidity curing box for curing at the temperature of 10 ℃ and the humidity of 70% for 24 hours to finally obtain the wafer-shaped oriented porous geopolymer inorganic membrane. 0.2MPa at room temperaturePure water flux at operating pressure of 360L m-2*h-1。
Example 5
A method for preparing an oriented porous geopolymer inorganic membrane, comprising the steps of:
(1) preparation of film-forming slurry: mixing 20g of fly ash, 25g of phosphoric acid solution with the mass fraction of 75% and 15g of water according to the mass part ratio, mechanically stirring for 15min at the speed of 600r/min, and standing the obtained mixed slurry for 2h at the temperature of 40 ℃ for later use.
(2) Preparation of a frozen blank: and adding 20g of water into the film-forming slurry, mechanically stirring uniformly, injecting into a self-made freezing mold for directional freezing at the freezing temperature of-80 ℃, and obtaining a frozen blank after the slurry is solidified.
(3) Preparing a directional porous blank: and (3) freeze-drying the frozen blank at the vacuum degree of 35pa at the freezing temperature of-70 ℃ for 8h to form the directional porous blank.
(4) Curing the oriented porous inorganic membrane: and (3) putting the oriented porous blank into a constant-temperature constant-humidity curing box for curing at the temperature of 35 ℃ and the humidity of 100% for 48 hours to finally obtain the wafer-shaped oriented porous geopolymer inorganic membrane. When tested under normal temperature conditions, the pure water flux is 860L m under the operation pressure of 0.2MPa-2*h-1。
Example 6
A method for preparing an oriented porous geopolymer inorganic membrane, comprising the steps of:
(1) preparation of film-forming slurry: mixing 90g of fly ash, 140g of 55% sodium phosphate solution and 30g of water according to the mass portion ratio, mechanically stirring for 15min at the speed of 600r/min, and standing the obtained mixed slurry for 2h at the temperature of 40 ℃ for later use.
(2) Preparation of a frozen blank: and adding 10g of water into the film-forming slurry, mechanically stirring uniformly, injecting into a self-made freezing mold for directional freezing, wherein the freezing temperature is-80 ℃, and obtaining a frozen blank after the slurry is solidified.
(3) Preparing a directional porous blank: and (3) freeze-drying the frozen blank at the vacuum degree of 50pa at the freezing temperature of-70 ℃ for 8h to form the directional porous blank.
(4) Curing the oriented porous inorganic membrane: and (3) putting the oriented porous blank into a constant-temperature constant-humidity curing box for curing at the temperature of 35 ℃ and the humidity of 100% for 48 hours to finally obtain the wafer-shaped oriented porous geopolymer inorganic membrane. Tested under normal temperature conditions, the pure water flux is 780L m under the operation pressure of 0.2MPa-2*h-1。
Claims (4)
1. A method for preparing an oriented porous geopolymer inorganic membrane, comprising the steps of:
(1) preparation of film-forming slurry: mixing 20g of fly ash, 20g of 10M sodium hydroxide solution and 15g of water according to the mass part ratio, mechanically stirring for 15min at the speed of 600r/min, and standing the obtained mixed slurry for 3h at the temperature of 20 ℃ for later use;
(2) preparation of a frozen blank: adding 10g of water into the film-forming slurry, mechanically stirring uniformly, injecting into a self-made freezing mold for directional freezing, wherein the freezing temperature is-50 ℃, and obtaining a frozen blank after the slurry is solidified;
(3) preparing a directional porous blank: freeze-drying the frozen blank body at the vacuum degree of 20pa at the freezing temperature of-50 ℃ for 10h to form an oriented porous blank body;
(4) curing the oriented porous inorganic membrane: and (3) putting the oriented porous blank into a constant-temperature constant-humidity curing box for curing at the temperature of 25 ℃ and the humidity of 80% for 36 hours to finally obtain the wafer-shaped oriented porous geopolymer inorganic membrane.
2. A method for preparing an oriented porous geopolymer inorganic membrane, comprising the steps of:
(1) preparation of film-forming slurry: taking 25g of slag, 30g of industrial sodium silicate with the modulus of 1.3 and 15g of water according to the mass part ratio, mixing, mechanically stirring for 10min at 700r/min, and standing the obtained mixed slurry for 2h in an environment at 30 ℃ for later use;
(2) preparation of a frozen blank: adding 15g of water into the film-forming slurry, mechanically stirring uniformly, injecting into a self-made freezing mold for directional freezing, wherein the freezing temperature is-20 ℃, and obtaining a frozen blank after the slurry is solidified;
(3) preparing a directional porous blank: freeze-drying the frozen blank body at the vacuum degree of 25pa at the freezing temperature of-50 ℃ for 12h to form an oriented porous blank body;
(4) curing the oriented porous inorganic membrane: and (3) putting the oriented porous blank into a constant-temperature constant-humidity curing box for curing at the temperature of 35 ℃ and the humidity of 95% for 72 hours to finally obtain the wafer-shaped oriented porous geopolymer inorganic membrane.
3. A method for preparing an oriented porous geopolymer inorganic membrane, comprising the steps of:
(1) preparation of film-forming slurry: mixing 20g of fly ash, 25g of phosphoric acid solution with the mass fraction of 75% and 15g of water according to the mass part ratio, mechanically stirring for 15min at the speed of 600r/min, and standing the obtained mixed slurry for 2h at the temperature of 40 ℃ for later use;
(2) preparation of a frozen blank: adding 20g of water into the film-forming slurry, mechanically stirring uniformly, injecting into a self-made freezing mold for directional freezing, wherein the freezing temperature is-80 ℃, and obtaining a frozen blank after the slurry is solidified;
(3) preparing a directional porous blank: freeze-drying the frozen blank body at a vacuum degree of 35pa at a freezing temperature of-70 ℃ for 8h to form an oriented porous blank body;
(4) curing the oriented porous inorganic membrane: and (3) putting the oriented porous blank into a constant-temperature constant-humidity curing box for curing at the temperature of 35 ℃ and the humidity of 100% for 48 hours to finally obtain the wafer-shaped oriented porous geopolymer inorganic membrane.
4. A method for preparing an oriented porous geopolymer inorganic membrane, comprising the steps of:
(1) preparation of film-forming slurry: mixing 90g of fly ash, 140g of 55% sodium phosphate solution and 30g of water according to the mass part ratio, mechanically stirring for 15min at the speed of 600r/min, and standing the obtained mixed slurry for 2h at the temperature of 40 ℃ for later use;
(2) preparation of a frozen blank: adding 10g of water into the film-forming slurry, mechanically stirring uniformly, injecting into a self-made freezing mold for directional freezing, wherein the freezing temperature is-80 ℃, and obtaining a frozen blank after the slurry is solidified;
(3) preparing a directional porous blank: freeze-drying the frozen blank body at the vacuum degree of 50pa at the freezing temperature of-70 ℃ for 8h to form an oriented porous blank body;
(4) curing the oriented porous inorganic membrane: and (3) putting the oriented porous blank into a constant-temperature constant-humidity curing box for curing at the temperature of 35 ℃ and the humidity of 100% for 48 hours to finally obtain the wafer-shaped oriented porous geopolymer inorganic membrane.
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CN107619226A (en) * | 2017-10-23 | 2018-01-23 | 中国海洋大学 | A kind of honeycombed cement film and its production and use |
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