CN107812509B - Filtering membrane material and preparation method and application thereof - Google Patents
Filtering membrane material and preparation method and application thereof Download PDFInfo
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- CN107812509B CN107812509B CN201710828587.9A CN201710828587A CN107812509B CN 107812509 B CN107812509 B CN 107812509B CN 201710828587 A CN201710828587 A CN 201710828587A CN 107812509 B CN107812509 B CN 107812509B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- 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
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
- B01J20/3234—Inorganic material layers
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
- C02F1/705—Reduction by metals
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention relates to the technical field of filter materials, and discloses a preparation method of a filter membrane material, which comprises the following steps: dissolving transition metal salt in solvent to form solution, adding carbon film, mixing, adding into high pressure reactor for reaction, vacuumizing, and introducing CO2Heating to 35-60 ℃ until the internal absolute pressure is 80-150 bar, starting the reaction, and releasing CO after the reaction is carried out for 0.5-24 h2Cooling to room temperature to normal pressure to obtain reaction kettle liquid, drying to obtain a precursor carbon film, reacting the precursor carbon film at 700-1000 ℃ for 2-8 h under the atmosphere of protective gas to obtain a transition metal/carbon composite film, and immersing the transition metal/carbon composite film into CS (sulfur)2Soaking the solution for 1-12 h, filtering and drying to obtain a filter membrane material; the filter membrane material prepared by the invention has the characteristics of uniform transition metal load, good consistency, high adsorption efficiency, high adsorption capacity and the like, is easy to separate from water, is simple to recover, and is suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of filter materials, in particular to a filter membrane material and a preparation method and application thereof.
Background
The total mercury consumption of China is about 1000 tons, which accounts for about 50% of the total consumption of the world, and is the largest consumer country and producer country in the world. However, mercury is highly neurotoxic, can enter the organism through various routes, and is difficult to metabolize, thus causing cumulative effects in the organism, constituting a great threat to human health. Therefore, the control of mercury pollution is not slow.
Heretofore, the technologies for treating mercury-containing wastewater mainly include chemical methods, electrolytic methods, ion exchange methods, adsorption methods, and the like. Among them, the adsorption method is the most common technical means in the demercuration technology. The demercuration adsorbent mainly comprises a carbon-based adsorbent, an oxide-based adsorbent, an ore adsorbent, a precious metal-based adsorbent and the like. From the actual demercuration effect, the carbon-based adsorbent is the most mature, efficient and cheap demercuration adsorbent due to the developed pore structure, the huge surface area and the abundant surface functional groups. However, most of the untreated carbon-based adsorbents belong to physical adsorption, and can provide less active sites for mercury, so that the mercury removal efficiency is low. Therefore, the current adsorbents for removing mercury ions from water mainly have the following problems: (1) limited adsorbent capacity; (2) the selectivity is poor; (3) most of the adsorbent is powder, which is not easy to separate from water and difficult to recycle. Therefore, it is necessary to develop a highly efficient adsorbent having a high adsorption capacity, a high selectivity and an easy recovery.
Disclosure of Invention
In order to solve the problems, the invention provides a filtering membrane material and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of a filter membrane material is characterized by comprising the following steps:
(1) dissolving transition metal salt in a solvent to form a solution after uniform dissolution;
(2) adding a carbon film into the 10-60ml solution obtained in the step (1), uniformly mixing, adding into a 100ml high-pressure reaction kettle for reaction, pumping the high-pressure reaction kettle to a vacuum degree of 0.01-0.1 MPa, and filling CO2Heating to the inside absolute pressure of 8-15 MPa of the high-pressure reaction kettle to 35-60 MPaoC, starting reaction, and releasing CO in the high-pressure reaction kettle after the reaction is carried out for 0.5-24 h2Cooling to room temperature under normal pressure to obtain reaction kettle liquid;
(3) evaporating the reaction kettle liquid, evaporating the solvent, and drying the remaining solid to obtain a precursor carbon film;
(4) reacting the precursor carbon film for 2-8 h at the reaction temperature of 700-1000 ℃ under the atmosphere of protective gas to obtain a transition metal/carbon composite film;
(5) immersing the transition metal/carbon composite membrane in 10ml of sulfur CS2And soaking the solution for 1-12 h, filtering and drying to obtain the filter membrane material.
Preferably, the transition metal salt is one or more of sulfate, nitrate or chloride of iron, cobalt, nickel, manganese, copper and zinc, and the transition metal salt is changed into a transition metal simple substance through the steps of the preparation method, has strong reducibility, and can reduce mercury ions into the mercury simple substance.
Preferably, the solvent is at least one of water, ethanol and isopropanol, the solvent can well dissolve the transition metal salt to form a uniform solution, and the transition metal salt can be hydrolyzed in the solvent.
Preferably, in the step (1), the molar concentration of the transition metal salt in the solution is 0.01-1 mol/L.
Preferably, in the step (2), the carbon film is at least one of carbon paper, carbon cloth and carbon fiber, the added mass of the carbon film is 0.5-10 g, the carbon film has a size of several millimeters to several centimeters, can be in a block shape or a sheet shape, can be in a spherical shape, a rectangular shape, a circular shape, an irregular polygonal shape and the like, and the carbon film serves as a carrier and provides active sites for the transition metal simple substance and the sulfur simple substance.
Preferably, in the step (4), the protective gas is Ar or H2、N2At least one of the transition metals exists in the precursor carbon film in the form of hydroxide, the transition metal exists in the precursor carbon film and is reduced into a transition metal simple substance by the carbon film under the high-temperature condition, and the protective gas is used for preventing the reduced transition metal simple substance from being oxidized.
Preferably, in the step (4), the reaction temperature is preferably 750 to 900%oAnd C, the reaction time is preferably 2-4 h.
Preferably, in the step (5), CS of sulfur is2In solution, sulfur and CS2The mass-to-volume ratio of (A) is 1-50: 100g/mL, sulfur has the function of adsorbing mercury simple substances.
The invention also provides the filter membrane material prepared by the method.
The invention also provides application of the filter membrane material in removing mercury ions in liquid.
When the high-pressure reaction kettle is used for reaction, CO2The function of the method is to provide a medium in a supercritical state, and under the supercritical state, the transition metal salt solution is contacted with the carbon film more uniformly.
The invention has the following beneficial effects: (1) the invention reduces mercury ions by loading transition metal simple substances on the carbon film and utilizing the strong reducibility of the transition metals, and then fixes the mercury ions in the water solution on the carbon film by the chemical adsorption of sulfur, thereby realizing the purification of mercury sewage; (2) the obtained filter membrane material has uniform transition metal load and good consistency, and the filter membrane material is provided with adjustable mercury adsorption sites, so that the filter membrane material has high adsorption efficiency and high adsorption capacity; (3) the filter membrane material is easy to separate from water and is easy to recover.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention without limiting the invention. In the drawings:
FIG. 1 is an XRD photograph of the product obtained in example 1.
Figure 2 is a graph of the mercury sorption capacity of the product obtained in example 1.
FIG. 3 is an XRD photograph of the product obtained in example 2.
Detailed Description
The technical solution of the present invention is further specifically described below by way of specific examples in conjunction with the accompanying drawings.
Example 1
0.98g of NiCl is taken2·6H2And dissolving O in 30mL of absolute ethyl alcohol, uniformly dissolving to form a solution, adding 3g of carbon cloth into the solution, uniformly mixing, and putting into a 100mL high-pressure reaction kettle for reaction. After the high-pressure reaction kettle is pumped to a vacuum degree of 0.1MPa, CO is filled in2Gas, the absolute pressure in the high-pressure reaction kettle reaches 9 MPa, and CO in the high-pressure reaction kettle is released after the reaction is carried out for 0.5 h at the temperature of 40 DEG C2Cooling to room temperature under normal pressure to obtain reaction kettle liquid; and volatilizing the solvent from the reaction kettle liquid in vacuum, drying the remaining solid, placing the dried solid in an argon protective gas atmosphere, raising the temperature to 800 ℃ at the heating rate of 5 ℃/min, calcining for 2h, and cooling to obtain the nickel/carbon composite membrane material. Weighing 0.3g of sulfur, dissolving the sulfur in 10ml of carbon disulfide to form a sulfur carbon disulfide solution, soaking the nickel/carbon composite membrane material in the sulfur carbon disulfide solution for 6 hours, evaporating the carbon disulfide, and drying to obtain the filter membrane material, wherein the XRD (X-ray diffraction) pattern of the filter membrane material is shown in figure 1.
The filter membrane material obtained in example 1 was used to carry out a mercury adsorption experiment under the following conditions: with HgCl2Preparing mercury ion with concentration of 50mg L for mercury source-120ml of mercury solution as simulated mercury sewage.
The prepared filter membrane material is used for mercury adsorption experiments, the test conditions are that the prepared filter membrane material is immersed into the prepared mercury sewage solution at normal temperature, the adsorption efficiency of mercury ions in 5min of the adsorption material reaches 83%, the adsorption efficiency of the mercury ions after 30min reaches 98%, and the mercury adsorption capacity curve of the filter membrane material is shown in figure 2.
Example 2
0.02g of NiCl is taken2·6H2Dissolving O in 10mL of water, dissolving uniformly to form a solution, adding 0.5g of carbon paper into the solution, mixing uniformly, putting the solution into a 100mL high-pressure reaction kettle for reaction, and introducing CO when the high-pressure reaction kettle is pumped to a vacuum degree of-0.05 MPa2Gas, the absolute pressure in the high-pressure reaction kettle reaches 8 MPa, and CO in the high-pressure reaction kettle is released after the reaction is carried out for 24 hours at the temperature of 60 DEG C2Cooling to room temperature under normal pressure to obtain reaction kettle liquid; and fully drying the reaction kettle liquid, placing the reaction kettle liquid in an argon protective gas atmosphere, raising the temperature to 900 ℃ at the heating rate of 5 ℃/min, calcining for 3h, and cooling to obtain the nickel/carbon composite membrane material. Weighing 0.1g of sulfur, dissolving the sulfur in 10ml of carbon disulfide to form a sulfur carbon disulfide solution, soaking the nickel/carbon composite membrane material in the sulfur carbon disulfide solution for 1 hour, evaporating the carbon disulfide, and drying to obtain the filter membrane material, wherein the XRD (X-ray diffraction) pattern of the filter membrane material is shown in figure 3.
The prepared filter membrane material is used for mercury adsorption experiments, and the test conditions are that the prepared filter membrane material is immersed into the prepared mercury sewage solution at normal temperature, the adsorption efficiency of mercury ions of the adsorption material reaches 80% within 5min, and the adsorption efficiency of mercury ions reaches 97% after 40 min.
Example 3
6.48g of FeCl was taken3Dissolving the carbon fiber into 40mL of absolute ethyl alcohol, forming a solution after uniform dissolution, adding 10g of carbon fiber into the solution, uniformly mixing, adding the mixture into a 100mL high-pressure reaction kettle for reaction, and introducing CO after the high-pressure reaction kettle is pumped to a vacuum degree of 0.1MPa2Gas, the absolute pressure in the high-pressure reaction kettle reaches 15MPa, and CO in the high-pressure reaction kettle is released after the reaction is carried out for 6 hours at the temperature of 50 DEG C2Cooling to room temperature under normal pressure to obtain reaction kettle liquid; and fully drying the reaction kettle liquid, placing the reaction kettle liquid in an argon protective gas atmosphere, raising the temperature to 1000 ℃ at the heating rate of 5 ℃/min, calcining for 4h, and cooling to obtain the iron/carbon composite membrane material. WeighingDissolving 5g of sulfur in 10ml of carbon disulfide to form a carbon disulfide solution of sulfur, soaking the iron/carbon composite membrane material in the carbon disulfide solution of sulfur for 8 hours, volatilizing the carbon disulfide, and drying to obtain the filter membrane material.
The prepared filter membrane material is used for mercury adsorption experiments, and the test conditions are that the prepared filter membrane material is immersed into the prepared mercury sewage solution at normal temperature, the adsorption efficiency of mercury ions of the adsorption material reaches 90% within 3min, and the adsorption efficiency of mercury ions reaches 99% after 20 min.
Example 4
3.25g of Fe (NO) are taken3)3·9H2Dissolving O in 35mL of water, dissolving uniformly to form a solution, adding 2.5g of carbon fiber into the solution, mixing uniformly, putting the solution into a 100mL high-pressure reaction kettle for reaction, and introducing CO after the high-pressure reaction kettle is pumped to a vacuum degree of 0.01MPa2The absolute pressure in the autoclave was adjusted to 10 MPa by the gas. After reacting for 12 hours at the temperature of 35 ℃, releasing CO in the high-pressure reaction kettle2Cooling to room temperature under normal pressure to obtain reaction kettle liquid; and fully drying the reaction kettle liquid, placing the reaction kettle liquid in a nitrogen protective gas atmosphere, raising the temperature to 750 ℃ at the heating rate of 5 ℃/min, calcining for 8h, and cooling to obtain the iron/carbon composite membrane material. Weighing 2.0g of sulfur, dissolving the sulfur in 10ml of carbon disulfide to form a sulfur carbon disulfide solution, soaking the iron/carbon composite membrane material in the sulfur carbon disulfide solution for 12 hours, volatilizing the carbon disulfide, and drying to obtain the filter membrane material.
The prepared filter membrane material is used for mercury adsorption experiments, and the test conditions are that the prepared filter membrane material is immersed into the prepared mercury sewage solution at normal temperature, the adsorption efficiency of mercury ions of the adsorption material reaches 92% within 3min, and the adsorption efficiency of mercury ions reaches 99% after 15 min.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (8)
1. A preparation method of a filter membrane material is characterized by comprising the following steps: (1) dissolving transition metal salt in a solvent to form a solution after uniform dissolution; (2) taking 10-60mL of the solution obtained in the step (1), adding a carbon film, uniformly mixing, adding into a 100mL high-pressure reaction kettle for reaction, pumping the high-pressure reaction kettle to a vacuum degree of 0.01-0.1 MPa, and introducing CO2Heating to 35-60 ℃ until the absolute pressure in the high-pressure reaction kettle is 8-15 MPa, starting the reaction, and releasing CO in the high-pressure reaction kettle after the reaction is carried out for 0.5-24 h2Cooling to room temperature under normal pressure to obtain reaction kettle liquid; (3) evaporating the reaction kettle liquid, evaporating the solvent, and drying the remaining solid to obtain a precursor carbon film; (4) reacting the precursor carbon film for 2-8 h at the reaction temperature of 700-1000 ℃ under the atmosphere of protective gas to obtain a transition metal/carbon composite film; (5) immersing the transition metal/carbon composite membrane in 10mL of sulfur CS2Soaking the solution for 1-12 h, filtering and drying to obtain a filter membrane material;
the transition metal salt is one or more of sulfate, nitrate or chloride of iron, cobalt, nickel, manganese, copper and zinc; in the step (2), the carbon film is at least one of carbon paper, carbon cloth and carbon fiber, and the adding mass of the carbon film is 0.5-10 g.
2. The method for preparing a filter membrane material as claimed in claim 1, wherein the solvent is at least one of water, ethanol and isopropanol.
3. The preparation method of the filter membrane material as claimed in claim 1, wherein in the step (1), the molar concentration of the transition metal salt in the solution is 0.01-1 mol/L.
4. The method for preparing a filter membrane material as claimed in claim 1, wherein in the step (4), the protective gas is Ar and N2At least one of (1).
5. The preparation method of the filter membrane material as claimed in claim 1, wherein in the step (4), the reaction temperature is 750-900 ℃ and the reaction time is 2-5 h.
6. The method for preparing a filter membrane material as claimed in claim 1, wherein in the step (5), CS of the sulfur is2In solution, sulfur and CS2The mass-to-volume ratio of (A) is 1-50: 100 g/mL.
7. A filter membrane material prepared by the preparation method of any one of claims 1 to 6.
8. Use of the filtration membrane material of claim 7 for removing mercury ions from a liquid.
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