CN107362768B - Copper foam ferrite, preparation method thereof and application thereof in adsorption removal of arsenic in water body - Google Patents
Copper foam ferrite, preparation method thereof and application thereof in adsorption removal of arsenic in water body Download PDFInfo
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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0233—Compounds of Cu, Ag, Au
- B01J20/0237—Compounds of Cu
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
- B01J20/28042—Shaped bodies; Monolithic structures
- B01J20/28045—Honeycomb or cellular structures; Solid foams or sponges
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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
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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Abstract
The invention discloses a copper ferrite foam, a preparation method thereof and application thereof in adsorption removal of arsenic in a water body. The foamed copper ferrite takes foamed iron as a matrix, the foamed iron matrix is composed of a smooth framework, the framework forms three-dimensional communication holes, and micro-nano copper ferrite grows on the framework of the matrix to roughen the surface of the framework; the foamed copper ferrite replicates the framework structure of the foamed iron matrix. The preparation method of the copper ferrite foam comprises the following steps: (1) removing an oxide film on the surface of the foamed iron; (2) pouring ferric nitrate and cupric nitrate into distilled water, stirring and dissolving, adding urea, and continuously stirring for 10-60 min; then putting the mixture and the processed foam iron into a reaction kettle, sealing and then carrying out heat preservation reaction; (3) and after the reaction is finished, taking out the foamed iron with the copper ferrite growing on the surface, washing with distilled water, and drying to obtain the foamed copper ferrite. The copper ferrite foam has very strong adsorption capacity on arsenic in water and better recycling performance.
Description
(I) technical field
The invention relates to copper ferrite foam, a preparation method thereof and application thereof in adsorption removal of arsenic in a water body, and belongs to the technical field of heavy metal water treatment.
(II) background of the invention
Arsenic is semi-metallic and often used as an alloying additive to improve alloying properties, for example, adding small amounts of arsenic to copper to make arsenic copper alloys can significantly reduce the thermal and electrical conductivity of copper. In addition, arsenic is also often used as a dopant material for the preparation of some semiconductor materials. Natural arsenic or metallic compounds of arsenic are very rare in nature and are mostly incorporated as sulfides in other metal ores such as copper, lead, zinc and cobalt ores. With the mining and smelting of arsenic-containing minerals by human beings and the wide utilization of arsenide, the migration and conversion process of arsenic in the environment are directly or indirectly influenced. On the other hand, arsenic and compounds thereof are recognized carcinogens by various authorities in the world, and excessive intake of arsenic can cause great harm to human bodies. After arsenic is absorbed by human body, trivalent arsenic can interfere the reaction of phosphorus in human body, such as blocking the synthesis of adenosine triphosphate, etc., arsenic can also react with sulfhydryl of enzyme protein in the body, so that enzyme loses activity, normal metabolism of cells is affected, tissue damage and body disorder are caused, and poisoning and even death are directly caused. Chronic drinking arsenic poisoning can cause damage to multiple system functions of the human body, resulting in diseases such as hypertension, cardiovascular and cerebrovascular diseases, diabetes, skin pigment metabolism disorder and the like, and finally developing into skin cancer. In recent years, along with the acceleration of the industrialization process, arsenic pollution caused by industrial production is continuously expanded, and the toxicity of arsenic in water bodies is reported at home and abroad.
The world health organization and other international research institutions agree that arsenic is a highly toxic element and is one of the pollutants preferentially controlled in water. Arsenic in different forms is also toxic, inorganic arsenic is generally more toxic than organic arsenic, trivalent arsenic is more toxic than pentavalent arsenic, and compounds of arsenic have far greater toxicity of hydrogen arsenide than other arsenates and arsenites. In the world, various diseases such as cancer and even death frequently occur due to acute or chronic arsenic poisoning caused by arsenic pollution of drinking water, and the amazing data of the diseases cause high attention to arsenic in drinking water. In 1993, the limit of the arsenic content in a new drinking water standard established by the world health organization is 10 mug/L, and countries around the world adopt the standard one by one, so that the maximum allowable arsenic content standard in the drinking water is improved from 50 mug/L to 10 mug/L.
At present, the common methods for removing arsenic from water bodies include a coagulation method, an ion exchange method, an adsorption method, an oxidation precipitation method, a biological method and the like. The adsorption method is the first choice method for removing arsenic from drinking water, common adsorbents comprise activated alumina, titanium oxide, zeolite, iron-manganese compounds and the like, the method is simple and convenient to operate, the price of the adsorbent is low, and the method is suitable for treating arsenic pollution of water bodies of factories. However, the powder adsorbent is difficult to recover and reuse, and even the powder can cause secondary pollution to water bodies, so the powder adsorbent is not suitable for arsenic pollution treatment of large-area water bodies such as lakes, rivers and the like.
Therefore, the research on the high-efficiency recyclable adsorbent has very important significance for treating the arsenic pollution of the water body.
Disclosure of the invention
The invention aims to provide copper ferrite foam, a preparation method thereof and application thereof in adsorption removal of arsenic in water aiming at the defects of arsenic pollution treatment in the prior art.
The technical solution adopted by the present invention to achieve the above object is specifically described below.
The invention provides a foamed copper ferrite, which takes foamed iron as a matrix, the foamed iron matrix is composed of a smooth frame, the frame forms a three-dimensional communicating hole, the pore size of the foamed iron matrix is 30-120 ppi, and micro-nano copper ferrite grows on the frame of the matrix to roughen the surface of the frame; the foamed copper ferrite replicates the framework structure of the foamed iron matrix.
The foamed copper ferrite is in a black porous block foam shape, and the main component of the surface of the foamed copper ferrite is CuFe2O4。
The invention also provides a preparation method of the copper ferrite foam, which comprises the following steps:
(1) taking a foam iron matrix, and soaking the foam iron matrix in a hydrochloric acid solution to remove an oxide film on the surface;
(2) weighing ferric nitrate and cupric nitrate with the molar ratio of copper to iron being 1: 1-1: 5, adding the ferric nitrate and cupric nitrate into distilled water, stirring to dissolve, adding urea to enable the molar ratio of nitrate (namely ferric nitrate and cupric nitrate) to urea to be 20: 1-5: 1, and continuously stirring for 10-60 min; then putting the processed foamed iron substrate and the processed foamed iron substrate into a reaction kettle, sealing completely, and transferring the reaction kettle into an oven for heat preservation reaction, wherein the reaction temperature is 50-200 ℃, and the heat preservation time is 3-12 hours;
(3) and after the reaction is finished, taking out the foamed iron with the copper ferrite growing on the surface, repeatedly washing the foamed iron with distilled water, and drying the foamed iron in a drying oven at the temperature of 50-100 ℃ to obtain the foamed copper ferrite.
Further, in the step (1), the concentration of the hydrochloric acid solution is preferably 1-3M. The soaking time is preferably 2-10 min.
The invention further provides an application of the copper ferrite foam in adsorption removal of arsenic in a water body, and the application specifically comprises the following steps:
(a) adjusting the pH value of the arsenic-containing wastewater to 2-12, adding foamed copper ferrite into a constant-temperature water bath oscillator, and oscillating and adsorbing at the temperature of 10-60 ℃ at the speed of 100-400 r/min;
(b) after oscillation adsorption, the foamed copper ferrite is sucked out by a magnet, and the wastewater is filtered to obtain the treated water body. The adsorbed copper ferrite foam can be washed and desorbed by NaOH solution with a certain concentration, and can be reused.
Further, the arsenic is preferably as (v).
The water body (namely the arsenic-containing wastewater) is industrial heavy metal metallurgical wastewater, surface water or domestic sewage.
In the application range, the pH value is reduced, the adsorption temperature is increased, or the adsorption time is prolonged, so that the adsorption rate is improved.
The invention has the beneficial effects that:
(1) compared with the nano CuFe reported in the existing literature, the copper ferrite foam provided by the invention2O4And higher adsorption capacity for As (V).
(2) The invention adopts the method of removing arsenic by the copper ferrite foam adsorption, the adsorbent can easily separate the arsenic from the water body by using the magnet while efficiently removing the arsenic in the water body, and secondary pollution is not generated, thereby successfully solving the aeipathia that the adsorbent is difficult to recycle and reuse and easily causes secondary pollution in the existing treatment process of arsenic pollution in the water body.
(3) The preparation process of the foamed copper ferrite is simple, convenient to operate, high in efficiency, easy to realize, free of secondary pollution, economical and environment-friendly, and realizes renewable utilization of resources.
(IV) description of the drawings
FIG. 1 is an SEM topography of a foamed iron matrix and a prepared foamed copper ferrite in example 1, wherein FIGS. a and b are SEM images of the foamed iron matrix, and FIGS. c and d are SEM images of the foamed copper ferrite; as can be seen from the figure a, a large number of three-dimensional communicating holes exist on the foam iron matrix, and the frame is smooth (figure b); the copper ferrite foam basically replicates the framework structure of the iron foam matrix, and micro-nano particles grow on the framework (fig. c and d).
FIG. 2: 50mL of arsenic-containing raw solution with 10mg/L of As (V), adjusting the pH value of the solution to 3 by hydrochloric acid, adding 1 block of prepared copper ferrite foam, transferring the solution to a constant-temperature water bath oscillator, stirring at 200r/min for 180min, and obtaining a relation curve between the removal efficiency of arsenic in a water body and the reaction temperature.
(V) detailed description of the preferred embodiments
The present invention is further illustrated by the following specific examples, but the scope of the present invention is not limited thereto.
Example 1
Soaking a foamed iron substrate with the pore size of 30ppi and the size of 3cm multiplied by 0.5cm in 1M hydrochloric acid solution for 2min to remove an oxide film on the surface; weighing 16.1g of ferric nitrate nonahydrate and 9.6g of cupric nitrate trihydrate (the molar ratio of copper to iron is 1:1), pouring into a beaker containing 100mL of distilled water, stirring to completely dissolve, adding 0.6g of urea, and continuing stirring for 10 min; after the reaction is completed, putting the reaction product and the processed foam iron matrix into a reaction kettle, sealing the reaction kettle completely, and transferring the reaction kettle into an oven for heat preservation, wherein the reaction temperature is 50 ℃, and the heat preservation time is 3 hours; and after the reaction is finished, taking out the foamed iron with the copper ferrite growing on the surface, repeatedly washing the foamed iron with distilled water, and drying the foamed iron in a drying oven at 50 ℃ to obtain the foamed copper ferrite.
50mL of arsenic-containing raw solution with 10mg/L of As (V) content is put into a 250mL conical flask, the pH value of the solution is adjusted to 3 by hydrochloric acid, a piece of prepared copper ferrite foam is added, the mixture is transferred to a constant-temperature water bath oscillator, the stirring speed is 200r/min, the reaction temperature is 50 ℃, and the adsorption time is 5-180 min.
And evaluating the adsorption removal effect of the copper ferrate foam on arsenic in the water body by adopting the adsorption rate.
TABLE 1 results of experiments with different adsorption times
| Time/min | Adsorption rate of arsenic/%) |
| 5 | 11.3 |
| 15 | 32.1 |
| 30 | 41.4 |
| 60 | 60.3 |
| 120 | 86.1 |
| 180 | 97.9 |
Example 2
Taking a foamed iron substrate with the pore size of 30ppi and the size of 3cm multiplied by 0.5cm, and soaking in 3M hydrochloric acid solution for 10min to remove an oxide film on the surface; weighing 16.1g of ferric nitrate nonahydrate and 9.6g of cupric nitrate trihydrate (the molar ratio of copper to iron is 1:1), pouring into a beaker containing 100mL of distilled water, stirring to completely dissolve, adding 0.6g of urea, and continuing stirring for 60 min; after the reaction is completed, putting the reaction product and the processed foam iron matrix into a reaction kettle, sealing the reaction kettle completely, and transferring the reaction kettle into an oven for heat preservation, wherein the reaction temperature is 200 ℃, and the heat preservation time is 12 hours; and after the reaction is finished, taking out the foamed iron with the copper ferrite growing on the surface, repeatedly washing the foamed iron with distilled water, and drying the foamed iron in a drying oven at the temperature of 100 ℃ to obtain the foamed copper ferrite.
50mL of arsenic-containing raw solution with 10mg/L of As (V) content is put into a 250mL conical flask, the pH value of the solution is adjusted to 3 by hydrochloric acid, a piece of prepared copper ferrite foam is added, the mixture is transferred to a constant-temperature water bath oscillator, the stirring speed is 200r/min, the reaction temperature is 50 ℃, and the adsorption time is 5-180 min.
And evaluating the adsorption removal effect of the copper ferrate foam on arsenic in the water body by adopting the adsorption rate.
TABLE 2 results of experiments with different adsorption times
Example 3
The preparation method of the copper ferrite foam is the same as that of example 1.
50mL of arsenic-containing raw solution with 10mg/L of As (V) content is put into a 250mL conical flask, the pH value of the solution is adjusted to 3 by hydrochloric acid, a piece of prepared copper ferrite foam is added, the mixture is transferred to a constant-temperature water bath oscillator, the stirring speed is 200r/min, the reaction temperature is 15-60 ℃, and the adsorption time is 180 min.
And evaluating the adsorption removal effect of the copper ferrate foam on arsenic in the water body by adopting the adsorption rate.
TABLE 3 results of experiments with different adsorption temperatures
| Temperature/. degree.C | Adsorption rate of arsenic/%) |
| 15 | 52.6 |
| 20 | 60.1 |
| 30 | 64.4 |
| 40 | 95.2 |
| 50 | 97.9 |
| 60 | 98.9 |
Example 4
The preparation method of the copper ferrite foam is the same as that of example 1.
50mL of arsenic-containing raw solution with 10mg/L of As (V) content is put into a 250mL conical flask, the pH value is adjusted to 2-12 by hydrochloric acid, a piece of prepared copper ferrite foam is added, the mixture is transferred to a constant-temperature water bath oscillator, the stirring speed is 200r/min, the reaction temperature is 50 ℃, and the adsorption time is 180 min.
And evaluating the replacement and removal effect of the copper ferrite foam on arsenic in the water body by adopting the adsorption rate.
TABLE 4 adsorption test results at different pH
Example 5
The preparation method of the copper ferrite foam is the same as that of example 1.
50mL of arsenic-containing raw solution is put into a 250mL conical flask, hydrochloric acid is used for adjusting the pH value to 3, a piece of prepared copper ferrite foam is added, the mixture is transferred to a constant-temperature water bath oscillator, the stirring speed is 200r/min, the reaction temperature is 50 ℃, and the adsorption time is 180 min.
And evaluating the replacement and removal effect of the copper ferrite foam on arsenic in the water body by adopting the adsorption rate.
TABLE 5 adsorption experiment results for different arsenic concentrations
| As (V) concentration/mgL-1 | Adsorption rate/%) |
| 10 | 97.9 |
| 20 | 49.5 |
| 40 | 25.9 |
| 60 | 24.7 |
| 80 | 16.1 |
| 100 | 14.3 |
Example 6
Three kinds of copper ferrite foams were prepared in the same manner as in example 1 except that the iron foam substrate of example 1 having a pore size of 30ppi and a size of 3 cm. times.3 cm. times.0.5 cm was replaced with the iron foam substrate of example 1 having a pore size of 60ppi, 90ppi, or 120 ppi.
50mL of arsenic-containing raw solution with 10mg/L of As (V) content is put into a 250mL conical flask, hydrochloric acid is used for adjusting the pH value to 3, a piece of foamy copper ferrite with different pore sizes is respectively added, the mixture is transferred to a constant-temperature water bath oscillator, the stirring speed is 200r/min, the reaction temperature is 50 ℃, and the adsorption time is 180 min.
And evaluating the replacement and removal effect of the copper ferrite foam on arsenic in the water body by adopting the adsorption rate.
TABLE 6 adsorption experiment results for different pore sizes
Example 7: experiment of adsorption Capacity
The preparation method of the foamy copper ferrite is the same as that in example 1, preparing arsenic (V) containing raw solution with initial concentration of 5, 10, 20, 40, 60, 80 and 100mg/L and adjusting pH to 7, respectively taking 50mL of the arsenic containing raw solution to 7 conical flasks of 250mL, respectively adding a piece of adsorbing material with the same mass, transferring to a constant temperature water bath oscillator, stirring at the speed of 200r/min, reacting at the temperature of 50 ℃ and adsorbing for 180 min. Comparing the results of the 7 flasks, it was found that the arsenic (V) adsorbed by the adsorbent of a certain mass had a saturation value, and that the adsorption amount did not increase beyond the certain value, which is the saturation adsorption amount, and the saturation adsorption amount per unit mass is the adsorption capacity of the adsorbent. Table 7 compares the adsorption capacities of three adsorbents:
TABLE 7 comparison of adsorption capacities
[a]:Y.-J.Tu,C.-F.You,C.-K.Chang,S.-L.Wang,T.-S.Chan,Adsorptionbehavior of As(III)onto a copper ferrite generated from printed circuit boardindustry,ChemEng J,225(2013)433-439。
Claims (4)
1. A copper ferrite foam is characterized in that: the foamed copper ferrite takes foamed iron as a matrix, the foamed iron matrix is composed of a smooth framework, the framework forms three-dimensional communicating holes, the pore size of the foamed iron matrix is 30-120 ppi, and micro-nano copper ferrite grows on the framework of the matrix to roughen the surface of the framework; the foamed copper ferrite replicates the framework structure of the foamed iron matrix;
the preparation method of the foamed copper ferrite comprises the following steps:
(1) taking a foam iron matrix, and soaking the foam iron matrix in a hydrochloric acid solution to remove an oxide film on the surface;
(2) weighing ferric nitrate and cupric nitrate with the molar ratio of copper to iron being 1: 1-1: 5, adding into distilled water, stirring to dissolve, adding urea to enable the molar ratio of nitrate to urea to be 20: 1-5: 1, and continuously stirring for 10-60 min; then putting the processed foamed iron substrate and the processed foamed iron substrate into a reaction kettle, sealing completely, and transferring the reaction kettle into an oven for heat preservation reaction, wherein the reaction temperature is 50-200 ℃, and the heat preservation time is 3-12 hours;
(3) and after the reaction is finished, taking out the foamed iron with the copper ferrite growing on the surface, repeatedly washing the foamed iron with distilled water, and drying the foamed iron in a drying oven at the temperature of 50-100 ℃ to obtain the foamed copper ferrite.
2. The copper foam ferrite of claim 1 wherein: in the step (1), the concentration of the hydrochloric acid solution is 1-3M, and the soaking time is 2-10 min.
3. The application of the copper ferrite foam in removing arsenic in a water body by adsorption according to claim 1, which is specifically as follows:
(a) adjusting the pH value of the arsenic-containing wastewater to 2-12, adding foamed copper ferrite into a constant-temperature water bath oscillator, and oscillating and adsorbing at the temperature of 10-60 ℃ at the speed of 100-400 r/min;
(b) after oscillation adsorption, the foamed copper ferrite is sucked out by a magnet, and the wastewater is filtered to obtain the treated water body.
4. Use according to claim 3, characterized in that: the arsenic is As (V).
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102527319A (en) * | 2012-01-09 | 2012-07-04 | 中国科学院金属研究所 | High-efficiency superparamagnetic ferrite nano arsenic adsorbent and preparation process thereof |
| CN103831108A (en) * | 2014-03-18 | 2014-06-04 | 南京大学 | Copper ferrite-loaded activated carbon fiber, preparation method and application of fiber, and method for degrading activated azo dye wastewater |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102527319A (en) * | 2012-01-09 | 2012-07-04 | 中国科学院金属研究所 | High-efficiency superparamagnetic ferrite nano arsenic adsorbent and preparation process thereof |
| CN103831108A (en) * | 2014-03-18 | 2014-06-04 | 南京大学 | Copper ferrite-loaded activated carbon fiber, preparation method and application of fiber, and method for degrading activated azo dye wastewater |
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| Nanostructured iron(III)-copper(II) binary oxide: A novel adsorbent for enhanced arsenic removal from aqueous solutions;Gaosheng Zhang et al.;《Water Research》;20130322;第47卷;说明书第4023页第2.2节、第4024页第2.4节 * |
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