CN113083244A - Chitosan/geopolymer composite membrane for removing Cr (VI) and preparation method thereof - Google Patents
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- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
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Abstract
The invention provides a chitosan/geopolymer composite film for removing Cr (VI) and a preparation method thereof, wherein the preparation method comprises the following steps: adding NaOH solid into industrial water glass, sealing after dissolving, placing in a constant-temperature oven at 25 ℃, cooling and standing for later use; adding metakaolin, an alkali activator and deionized water into a dispersion machine for uniform dispersion to obtain geopolymer slurry, then grouting the slurry into a circular plastic mold, sealing and maintaining the mold, demolding to obtain a geopolymer film, soaking the geopolymer film in water, cleaning the geopolymer film until the pH value of the water is neutral, taking out the geopolymer film and drying the geopolymer film; preparing a chitosan acetic acid solution with the concentration of 1-4%, uniformly coating the chitosan acetic acid solution on the surface of the geopolymer film, drying, and washing with deionized water to obtain a finished product. The polymer composite membrane has a good treatment effect on Cr (VI) in an aqueous solution, and has the advantages of low raw material cost and simple preparation process compared with the traditional ceramic membrane and organic membrane.
Description
Technical Field
The invention relates to the field of inorganic polymer composite materials, in particular to a chitosan/geopolymer composite film for removing Cr (VI) and a preparation method thereof.
Background
With the development of industry, the pollution of heavy metal ions is increasingly serious, and the waste water containing the heavy metal ions is discharged in large quantity, so that the soil and water bodies are seriously polluted. Among the heavy metal ions, chromium is considered to be one of the most toxic heavy metals, and the main sources thereof are electroplating, tanning, dyeing, mining, textile industry, and metallurgical industry. Chromium is usually present in the form of chromium Cr (III) or chromium Cr (VI), which is more dangerous than Cr (III), and can be present as CrO4 2-Or HCrO4 -The morphology diffuses through the cell membrane and infiltrates into the cell, can cause cancer and teratogenesis, and poses serious threats to the ecological environment and human health. Therefore, attention is being paid to the treatment of Cr (VI) wastewater. The pollution of heavy metal is reduced, on one hand, a production process with lower heavy metal discharge is required, and on the other hand, the research of a more appropriate heavy metal wastewater treatment method is also important.
The treatment method for the wastewater containing Cr (VI) mainly comprises a chemical precipitation method, an electrochemical precipitation method, an adsorption method, electrodialysis, membrane filtration, reverse osmosis, an ion exchange method and the like[1]. The membrane filtration method has the characteristics of high treatment efficiency, low energy consumption, simple operation and large treatment capacity, and is widely applied to the industrial fields of chemical industry, food, medicine, environment, smelting and the like. In the water treatment by the membrane filtration method, the type and the property of the membrane material play a key role in the treatment effect of the wastewater. Currently in membranesThe membrane materials used in the filtration water treatment industry mainly include cellulose acetate, polyamide, polyvinylidene fluoride, silicon carbide, Pb membrane, zirconia membrane, etc., and can be divided into organic membrane and inorganic membrane according to their chemical compositions[2-3]. The organic polymer film has simple film-making process, good film-forming property and high flexibility, but has poor pollution resistance and mechanical strength and is not easy to clean. The inorganic membrane material has the advantages of high temperature resistance, high mechanical strength, good chemical stability, microbial corrosion resistance and the like, and occupies a certain proportion in the water treatment industry[4]。
From the current research, the preparation of the inorganic membrane mainly takes metal, metal oxide, zeolite and ceramic as raw materials, and the inorganic membrane is obtained by sintering at the high temperature of more than 1000 ℃, the energy consumption of the preparation process is huge, and the requirement on sintering equipment is higher[5]. The sintering-free inorganic film material can solve the problems, and simultaneously has the advantages of good chemical stability, microbial corrosion resistance and high mechanical strength of the inorganic film material.
Geopolymer (Geopolymer) is a three-dimensional network gel with amorphous and quasicrystal characteristics, which is polymerized from silicon-oxygen tetrahedron and aluminum-oxygen tetrahedron, and has the advantages of simple preparation process, no sintering, low cost, low carbon, environmental protection, realization of large-scale resource recycling of solid waste and the like[6]. The material has been widely used in many fields from the invention up to now, and mainly comprises building materials, automobiles, aviation, electricians, casting, metallurgy, roads, plastics, refractory materials and the like.
Due to their molecular sieve-like structure and their porous properties, geopolymers are used by many researchers as adsorbents for water treatment. Cheng[7]Study of metakaolin geopolymer on Pb2+、Cu2+、Cd2+、Cr3+The adsorption capacity of the four heavy metal ions is respectively 100.00mg/g, 54.54mg/g, 75.74mg/g and 10.15 mg/g. The dynamic and thermodynamic researches on the adsorption process find that the adsorption process is chemical adsorption and monolayer adsorption. Lin[8]Sodium hydroxide and fly ash are used as raw materials and synthesized by an alkali fusion methodA geopolymer adsorbent is provided, the adsorption performance of the geopolymer on methylene blue and crystal violet is researched, and the research finds that the geopolymer has adsorption capacity of different degrees on the two substances. It follows that geopolymer materials have certain feasibility for use in the field of water treatment.
However, from the current research, the water treatment is mainly carried out by utilizing the size exclusion effect of geopolymer materials on suspended matters and the adsorption effect on metal ions, and the research objects are that the metal ions such as Ni exist in the form of cations in aqueous solution2+,Pb2+Or organic macromolecules, mainly because the geopolymer material is in aqueous solution and because of the large amount of Na in the geopolymer material+Elution is a little studied on small-sized anionic contaminants because the adsorption end of geopolymers is negatively charged and more easily adsorbs positively charged ions. A significant portion of the contaminants are present in the aqueous solution as anions. The invention mainly provides a preparation method of a geopolymer film material for removing pollutants such as Cr (VI) existing in an anion form.
The single geopolymer material has limited adsorption performance, and if the single geopolymer material can be compounded with other materials with higher adsorption capacity to prepare the efficient and environment-friendly composite adsorbent, the adsorption capacity can be greatly improved, and the defects of various materials can be overcome. In the Cr (VI) adsorbent, chitosan has wide sources, is green and environment-friendly, has higher adsorption capacity, and is easy to perform complex reaction with heavy metal ions and organic molecules of an aqueous solution due to a large amount of hydroxyl and amino in the molecules, so that the high adsorption capacity is shown. The invention provides a chitosan/geopolymer composite membrane and a preparation method thereof, and the membrane material fills up the gap of geopolymer in the aspect of aiming at anionic pollutants on one hand and also provides an effective removing method aiming at Cr (VI) in water on the other hand.
Disclosure of Invention
The technical problem to be solved is as follows: aiming at the defects in the prior art, the invention provides the chitosan/geopolymer composite membrane for removing Cr (VI) and the preparation method thereof.
The technical scheme is as follows: a preparation method of a chitosan/geopolymer composite membrane for removing Cr (VI) comprises the following steps:
(1) preparing an alkali activator: adding NaOH solid into industrial water glass, stirring by a glass rod and carrying out ultrasonic treatment to dissolve the NaOH solid, sealing by a preservative film, placing in a constant-temperature oven at 25 ℃, cooling and standing for 24 hours for later use, wherein the mass ratio of the NaOH solid to the industrial water glass is (0.07-0.2): 1;
(2) preparation of geopolymer films: adding metakaolin, an alkali activator and deionized water into a dispersion machine for uniform dispersion to obtain geopolymer slurry, then grouting into a circular plastic mould with the diameter of 50mm, sealing, maintaining at 25-80 ℃ for 12-36 h, demoulding to obtain a geopolymer film, soaking the geopolymer film in water, continuously changing the water until the pH value of the solution is neutral, taking out the geopolymer film and drying, wherein the mass ratio of the metakaolin, the alkali activator and the deionized water is (10-30): (10-21): 5-16);
(3) preparation of chitosan/geopolymer composite membrane: preparing a 1-4% chitosan acetic acid solution, uniformly coating the chitosan acetic acid solution on the surface of the geopolymer film obtained in the step (2) for 1-5 times, drying the geopolymer film for 12-36 hours at the temperature of 20-30 ℃, and washing the geopolymer film with deionized water to obtain the chitosan/geopolymer composite film.
The specific condition of the dispersion of the disperser in the step (2) is that the mechanical stirring is carried out for 5-20 min under the condition that the rotating speed is 1000-3000 r/min.
The chitosan/geopolymer composite membrane prepared by the preparation method can be used for removing Cr (VI).
The chitosan in the invention has wide sources, is green and environment-friendly, has higher adsorption capacity, and is easy to perform complex reaction with heavy metal ions and organic molecules in aqueous solution due to a large amount of hydroxyl and amino in the molecules, thereby showing higher adsorption capacity.
Compared with the traditional ceramic membrane, the chitosan/geopolymer composite membrane has the advantages of simple preparation process, no sintering and low energy consumption; compared with the adsorption treatment of chitosan on wastewater, the chitosan can be loaded on a functional layer as a geopolymer is used as a supporting layer, so that the problems of poor mechanical property and limited application form of the chitosan material are solved. Meanwhile, in the invention, the geopolymer material not only plays a supporting role, but also has a certain removing role on Cr (VI). In conclusion, the chitosan/geopolymer composite membrane has the advantages of both inorganic membranes and organic membranes, has the advantages of high removal efficiency, strong mechanical property, low raw material cost, simple preparation process and the like, and provides a new material for the treatment of Cr (VI) wastewater.
Has the advantages that: the chitosan/geopolymer composite film for removing Cr (VI) and the preparation method thereof provided by the invention have the following beneficial effects:
1. the chitosan/geopolymer composite membrane has a good treatment effect on Cr (VI) in an aqueous solution, is synthesized by adopting an injection molding method by taking metakaolin and industrial-grade water glass as main raw materials, and can be obtained by a simple coating method;
2. the invention provides a chitosan/geopolymer composite membrane, which not only fills up the gap of geopolymer in the aspect of aiming at anionic pollutants, but also provides an effective method for removing Cr (VI) in water.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto, and may be carried out with reference to conventional techniques for process parameters not particularly noted.
NaOH solids in the following examples were purchased from Shanghai Aladdin Biotechnology Ltd; industrial grade water glass was purchased from Guangdong force Nature chemical, Inc.; metakaolin was purchased from Shanxi Dajinyuan Kaolin GmbH; chitosan was purchased from shanghai mclin biochemical technologies, ltd.
Example 1
A preparation method of a chitosan/geopolymer composite membrane for removing Cr (VI) comprises the following steps:
(1) preparation of alkali activator: adding 13.05g of NaOH solid into 100g of industrial water glass, stirring by a glass rod and carrying out ultrasonic treatment to dissolve the NaOH solid, sealing by a preservative film, placing in a constant-temperature oven at 25 ℃, cooling and standing for 24 hours for later use;
(2) preparation of geopolymer films: adding 30.21g of metakaolin, 16.56g of alkali activator and 7.44g of deionized water into a dispersion machine for uniform dispersion to obtain geopolymer slurry, then grouting the slurry into a circular plastic mould with the diameter of 50mm, sealing, maintaining at 40 ℃ for 36 hours, demolding to obtain a geopolymer film, soaking the geopolymer film in water, continuously changing the water until the pH value of the solution is neutral, taking out the geopolymer film and drying;
(3) preparation of chitosan/geopolymer composite membrane: and (3) preparing a chitosan acetic acid solution with the concentration of 3%, uniformly coating the chitosan acetic acid solution on the surface of the geopolymer film obtained in the step (2) for 2 times, drying the geopolymer film at the temperature of 20 ℃ for 36 hours, and washing the geopolymer film with deionized water to obtain the chitosan/geopolymer composite film.
The chitosan/geopolymer composite membrane prepared in the embodiment is placed in a suction filtration device, the chitosan layer faces upwards, and suction filtration is carried out by using a circulating water type multi-purpose vacuum pump under the negative pressure of 0.2 MPa. The upper layer of the diaphragm is connected with a potassium dichromate aqueous solution, the initial concentration of a chromium ion solution in the potassium dichromate aqueous solution is 800mg/L, the pH value is 6, the solution passes through the diaphragm under the action of negative pressure, and meanwhile, chromium ions in the solution are intercepted and removed, and the purified solution is finally obtained. According to the technical scheme, the removal rate of chromium ions can reach 86%.
Example 2
A preparation method of a chitosan/geopolymer composite membrane for removing Cr (VI) comprises the following steps:
(1) preparation of alkali activator: adding 17.04g of NaOH solid into 100g of industrial water glass, stirring by a glass rod and carrying out ultrasonic treatment to dissolve the NaOH solid, sealing by a preservative film, placing in a constant-temperature oven at 25 ℃, cooling and standing for 24 hours for later use;
(2) preparation of geopolymer films: adding 25.22g of metakaolin, 14.98g of alkali activator and 5.25g of deionized water into a dispersion machine for uniform dispersion to obtain geopolymer slurry, then grouting into a circular plastic mould with the diameter of 50mm, sealing, maintaining at 60 ℃ for 24 hours, demolding to obtain a geopolymer film, soaking the geopolymer film in water, and continuously changing water until the pH value of the solution is neutral;
(3) preparation of chitosan/geopolymer composite membrane: and (3) preparing a chitosan acetic acid solution with the concentration of 2%, uniformly coating the chitosan acetic acid solution on the surface of the geopolymer film obtained in the step (2) for 2 times, drying the geopolymer film at the temperature of 20 ℃ for 36 hours, and washing the geopolymer film with deionized water to obtain the chitosan/geopolymer composite film.
The chitosan/geopolymer composite membrane prepared in the embodiment is placed in a suction filtration device, the chitosan layer faces upwards, and suction filtration is carried out by using a circulating water type multi-purpose vacuum pump under the negative pressure of 0.2 MPa. The upper layer of the diaphragm is connected with a potassium dichromate aqueous solution, the initial concentration of a chromium ion solution in the potassium dichromate aqueous solution is 1000mg/L, the pH value is 7, the solution passes through the diaphragm under the action of negative pressure, and meanwhile, chromium ions in the solution are intercepted and removed, and the purified solution is finally obtained. According to the technical scheme, the removal rate of the chromium ions can reach 90%.
Example 3
A preparation method of a chitosan/geopolymer composite membrane for removing Cr (VI) comprises the following steps:
(1) preparation of alkali activator: adding 20.21g of NaOH solid into 100g of industrial water glass, stirring by a glass rod and carrying out ultrasonic treatment, dissolving, sealing by a preservative film, placing in a constant-temperature oven at 25 ℃, cooling and standing for 24h for later use, wherein the mass of the NaOH solid and the mass of the industrial water glass are respectively 20.21g and 100 g;
(2) preparation of geopolymer films: adding 30.05g of metakaolin, 17.84g of alkali activator and 3.09g of deionized water into a dispersion machine for uniform dispersion to obtain geopolymer slurry, then grouting the slurry into a circular plastic mould with the diameter of 50mm, sealing, maintaining at 25 ℃ for 36 hours, demolding to obtain a geopolymer film, soaking the geopolymer film in water, continuously changing the water until the pH value of the solution is neutral, taking out the geopolymer film and drying;
(3) preparation of chitosan/geopolymer composite membrane: and (3) preparing a 1% chitosan acetic acid solution, uniformly coating the chitosan acetic acid solution on the surface of the geopolymer film obtained in the step (2) for 3 times, drying the geopolymer film at the temperature of 20 ℃ for 36 hours, and washing the geopolymer film with deionized water to obtain the chitosan/geopolymer composite film.
The chitosan/geopolymer composite membrane prepared in the embodiment is placed in a suction filtration device, the chitosan layer faces upwards, and suction filtration is carried out by using a circulating water type multi-purpose vacuum pump under the negative pressure of 0.1 MPa. The upper layer of the diaphragm is connected with a potassium dichromate aqueous solution, the initial concentration of a chromium ion solution in the potassium dichromate aqueous solution is 700mg/L, the pH value is 5, the solution passes through the diaphragm under the action of negative pressure, and meanwhile, chromium ions in the solution are intercepted and removed, and the purified solution is finally obtained. According to the technical scheme, the removal rate of the chromium ions can reach 82%.
In conclusion, the chitosan/geopolymer composite membrane prepared by the method has the advantages that the removal rate of Cr (VI) can reach more than 82%, the preparation method is simple, and the cost is low.
The above examples of the present invention are merely examples for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (3)
1. A preparation method of a chitosan/geopolymer composite film for removing Cr (VI) is characterized by comprising the following steps:
(1) preparing an alkali activator: adding NaOH solid into industrial water glass, stirring by a glass rod and carrying out ultrasonic treatment to dissolve the NaOH solid, sealing by a preservative film, placing in a constant-temperature oven at 25 ℃, cooling and standing for 24 hours for later use, wherein the mass ratio of the NaOH solid to the industrial water glass is (0.07-0.2): 1;
(2) preparation of geopolymer films: adding metakaolin, an alkali activator and deionized water into a dispersion machine for uniform dispersion to obtain geopolymer slurry, then grouting into a circular plastic mould with the diameter of 50mm, sealing, maintaining at 25-80 ℃ for 12-36 h, demoulding to obtain a geopolymer film, soaking the geopolymer film in water, continuously changing the water until the pH value of the solution is neutral, taking out the geopolymer film and drying, wherein the mass ratio of the metakaolin, the alkali activator and the deionized water is (10-30): (10-21): 5-16);
(3) preparation of chitosan/geopolymer composite membrane: preparing a 1-4% chitosan acetic acid solution, uniformly coating the chitosan acetic acid solution on the surface of the geopolymer film obtained in the step (2) for 1-5 times, drying the geopolymer film for 12-36 hours at the temperature of 20-30 ℃, and washing the geopolymer film with deionized water to obtain the chitosan/geopolymer composite film.
2. The method for preparing the chitosan/geopolymer composite film for removing Cr (VI) as claimed in claim 1, wherein: the specific condition of the dispersion of the disperser in the step (2) is that the mechanical stirring is carried out for 5-20 min under the condition that the rotating speed is 1000-3000 r/min.
3. A chitosan/geopolymer composite film for removing Cr (vi) prepared by the preparation method of any one of claims 1 to 2.
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